#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/1/1100882.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100882 _publ_requested_journal 'Organometallics' loop_ _publ_author_name 'Roesky, Peter W.' 'Panda, Tarun K.; Zulys, A.; Gamer, Michael T. ' _chemical_formula_sum 'C41.50 H52 N2 P2 Si2 Y' _chemical_formula_weight 785.88 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' 0.0000 0.0000 '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' 'Si' 'Si' 0.0817 0.0704 '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' 'Y' 'Y' -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4016(17) _cell_length_b 9.5304(16) _cell_length_c 22.771(4) _cell_angle_alpha 93.146(4) _cell_angle_beta 92.938(4) _cell_angle_gamma 98.530(4) _cell_volume 2011.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plates _exptl_crystal_colour colorless _exptl_crystal_size_max .58 _exptl_crystal_size_mid .36 _exptl_crystal_size_min .1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.298 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 1.620 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.795879 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart 1000 CCD' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25111 _diffrn_reflns_av_R_equivalents 0.0183 _diffrn_reflns_av_sigmaI/netI 0.0309 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 0.90 _diffrn_reflns_theta_max 30.52 _reflns_number_total 12116 _reflns_number_gt 10132 _reflns_threshold_expression >2sigma(I) _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^)+(0.0534P)^2^+0.4061P] 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_extinction_coef ? _refine_ls_number_reflns 12116 _refine_ls_number_parameters 437 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0465 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0949 _refine_ls_wR_factor_gt 0.0875 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 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 Y1 Y 0.536698(16) 0.781580(17) 0.743874(7) 0.02018(5) Uani 1 1 d . . . P1 P 0.77196(4) 0.88677(4) 0.659539(18) 0.01845(8) Uani 1 1 d . . . P2 P 0.83060(4) 0.95561(4) 0.794163(18) 0.01820(8) Uani 1 1 d . . . Si1 Si 0.51121(6) 1.04750(6) 0.63883(2) 0.02661(11) Uani 1 1 d . . . Si2 Si 0.61705(5) 1.03727(6) 0.87687(2) 0.02512(10) Uani 1 1 d . . . N1 N 0.61263(15) 0.92362(15) 0.66319(6) 0.0218(3) Uani 1 1 d . . . N2 N 0.66760(14) 0.96187(15) 0.81126(6) 0.0191(3) Uani 1 1 d . . . C1 C 0.5242(2) 0.5109(2) 0.72394(12) 0.0438(6) Uani 1 1 d . . . H1 H 0.5931 0.4543 0.7110 0.053 Uiso 1 1 calc R . . C2 C 0.4397(3) 0.5511(2) 0.67709(10) 0.0428(5) Uani 1 1 d . . . H2 H 0.4598 0.5093 0.6402 0.051 Uiso 1 1 calc R . . C3 C 0.3327(3) 0.6380(2) 0.67174(11) 0.0456(6) Uani 1 1 d . . . H3 H 0.2959 0.6397 0.6322 0.055 Uiso 1 1 calc R . . C4 C 0.2672(2) 0.7230(2) 0.71083(13) 0.0481(6) Uani 1 1 d . . . H4 H 0.2038 0.7767 0.6913 0.058 Uiso 1 1 calc R . . C5 C 0.2739(2) 0.7474(2) 0.77314(14) 0.0501(7) Uani 1 1 d . . . H5 H 0.2129 0.8127 0.7859 0.060 Uiso 1 1 calc R . . C6 C 0.3500(3) 0.6971(3) 0.81973(11) 0.0489(6) Uani 1 1 d . . . H6 H 0.3232 0.7307 0.8570 0.059 Uiso 1 1 calc R . . C7 C 0.4560(3) 0.6091(3) 0.82492(11) 0.0500(6) Uani 1 1 d . . . H7 H 0.4838 0.5971 0.8648 0.060 Uiso 1 1 calc R . . C8 C 0.5311(3) 0.5344(2) 0.78514(12) 0.0459(6) Uani 1 1 d . . . H8 H 0.6029 0.4897 0.8042 0.055 Uiso 1 1 calc R . . C9 C 0.82895(17) 0.84649(17) 0.72960(7) 0.0188(3) Uani 1 1 d . . . H9 H 0.8859 0.7660 0.7317 0.023 Uiso 1 1 calc R . . C10 C 0.78065(18) 0.72718(18) 0.61287(8) 0.0231(3) Uani 1 1 d . . . C11 C 0.8976(2) 0.6535(2) 0.61861(9) 0.0351(4) Uani 1 1 d . . . H11 H 0.9712 0.6841 0.6487 0.042 Uiso 1 1 calc R . . C12 C 0.9083(3) 0.5364(2) 0.58113(11) 0.0480(6) Uani 1 1 d . . . H12 H 0.9877 0.4861 0.5860 0.058 Uiso 1 1 calc R . . C13 C 0.8035(3) 0.4932(2) 0.53680(11) 0.0472(6) Uani 1 1 d . . . H13 H 0.8108 0.4132 0.5110 0.057 Uiso 1 1 calc R . . C14 C 0.6884(3) 0.5653(3) 0.52967(10) 0.0467(6) Uani 1 1 d . . . H14 H 0.6173 0.5359 0.4985 0.056 Uiso 1 1 calc R . . C15 C 0.6753(2) 0.6815(2) 0.56798(9) 0.0352(4) Uani 1 1 d . . . H15 H 0.5942 0.7295 0.5634 0.042 Uiso 1 1 calc R . . C16 C 0.88893(18) 1.01652(18) 0.62080(8) 0.0223(3) Uani 1 1 d . . . C17 C 0.8511(2) 1.0343(2) 0.56191(8) 0.0316(4) Uani 1 1 d . . . H17 H 0.7671 0.9788 0.5432 0.038 Uiso 1 1 calc R . . C18 C 0.9352(2) 1.1326(2) 0.53048(9) 0.0372(5) Uani 1 1 d . . . H18 H 0.9089 1.1438 0.4904 0.045 Uiso 1 1 calc R . . C19 C 1.0566(2) 1.2136(2) 0.55738(10) 0.0368(5) Uani 1 1 d . . . H19 H 1.1132 1.2817 0.5359 0.044 Uiso 1 1 calc R . . C20 C 1.0963(2) 1.1966(2) 0.61517(11) 0.0393(5) Uani 1 1 d . . . H20 H 1.1802 1.2529 0.6336 0.047 Uiso 1 1 calc R . . C21 C 1.01322(19) 1.0962(2) 0.64683(9) 0.0308(4) Uani 1 1 d . . . H21 H 1.0424 1.0828 0.6864 0.037 Uiso 1 1 calc R . . C22 C 0.93096(18) 0.87253(19) 0.84966(8) 0.0236(3) Uani 1 1 d . . . C23 C 0.9143(2) 0.7245(2) 0.84842(9) 0.0313(4) Uani 1 1 d . . . H23 H 0.8600 0.6697 0.8165 0.038 Uiso 1 1 calc R . . C24 C 0.9760(3) 0.6566(3) 0.89315(10) 0.0432(5) Uani 1 1 d . . . H24 H 0.9652 0.5557 0.8915 0.052 Uiso 1 1 calc R . . C25 C 1.0536(3) 0.7353(3) 0.94027(10) 0.0464(6) Uani 1 1 d . . . H25 H 1.0949 0.6886 0.9712 0.056 Uiso 1 1 calc R . . C26 C 1.0707(2) 0.8824(3) 0.94233(10) 0.0443(6) Uani 1 1 d . . . H26 H 1.1244 0.9365 0.9746 0.053 Uiso 1 1 calc R . . C27 C 1.0097(2) 0.9510(2) 0.89750(9) 0.0337(4) Uani 1 1 d . . . H27 H 1.0214 1.0519 0.8993 0.040 Uiso 1 1 calc R . . C28 C 0.92503(18) 1.13421(18) 0.78744(8) 0.0241(3) Uani 1 1 d . . . C29 C 1.0753(2) 1.1695(2) 0.79577(9) 0.0322(4) Uani 1 1 d . . . H29 H 1.1313 1.1016 0.8096 0.039 Uiso 1 1 calc R . . C30 C 1.1423(2) 1.3049(2) 0.78361(11) 0.0430(5) Uani 1 1 d . . . H30 H 1.2438 1.3293 0.7900 0.052 Uiso 1 1 calc R . . C31 C 1.0625(3) 1.4030(2) 0.76241(12) 0.0482(6) Uani 1 1 d . . . H31 H 1.1088 1.4945 0.7539 0.058 Uiso 1 1 calc R . . C32 C 0.9139(3) 1.3679(2) 0.75346(12) 0.0424(5) Uani 1 1 d . . . H32 H 0.8588 1.4354 0.7385 0.051 Uiso 1 1 calc R . . C33 C 0.8453(2) 1.2341(2) 0.76626(9) 0.0314(4) Uani 1 1 d . . . H33 H 0.7435 1.2112 0.7605 0.038 Uiso 1 1 calc R . . C34 C 0.3794(3) 0.9672(3) 0.57754(10) 0.0485(6) Uani 1 1 d . . . H34A H 0.4315 0.9330 0.5448 0.073 Uiso 1 1 calc R . . H34B H 0.3229 1.0390 0.5641 0.073 Uiso 1 1 calc R . . H34C H 0.3148 0.8874 0.5916 0.073 Uiso 1 1 calc R . . C35 C 0.6127(3) 1.2138(2) 0.61272(11) 0.0463(6) Uani 1 1 d . . . H35A H 0.6967 1.2471 0.6398 0.070 Uiso 1 1 calc R . . H35B H 0.5499 1.2871 0.6114 0.070 Uiso 1 1 calc R . . H35C H 0.6447 1.1944 0.5732 0.070 Uiso 1 1 calc R . . C36 C 0.4122(2) 1.1035(2) 0.70309(9) 0.0320(4) Uani 1 1 d . . . H36A H 0.3405 1.0239 0.7128 0.048 Uiso 1 1 calc R . . H36B H 0.3637 1.1840 0.6931 0.048 Uiso 1 1 calc R . . H36C H 0.4806 1.1320 0.7371 0.048 Uiso 1 1 calc R . . C37 C 0.6200(3) 0.9108(3) 0.93664(9) 0.0410(5) Uani 1 1 d . . . H37A H 0.5463 0.8275 0.9270 0.062 Uiso 1 1 calc R . . H37B H 0.6001 0.9580 0.9740 0.062 Uiso 1 1 calc R . . H37C H 0.7150 0.8805 0.9403 0.062 Uiso 1 1 calc R . . C38 C 0.4320(2) 1.0826(2) 0.86641(9) 0.0365(5) Uani 1 1 d . . . H38A H 0.4334 1.1617 0.8406 0.055 Uiso 1 1 calc R . . H38B H 0.3980 1.1102 0.9047 0.055 Uiso 1 1 calc R . . H38C H 0.3672 0.9996 0.8484 0.055 Uiso 1 1 calc R . . C39 C 0.7355(2) 1.2066(2) 0.90452(10) 0.0393(5) Uani 1 1 d . . . H39A H 0.8356 1.1897 0.9090 0.059 Uiso 1 1 calc R . . H39B H 0.7044 1.2391 0.9427 0.059 Uiso 1 1 calc R . . H39C H 0.7281 1.2795 0.8763 0.059 Uiso 1 1 calc R . . C100 C 0.2426(6) 0.3789(6) 0.9495(3) 0.0864(14) Uiso 0.75 1 d P . . C101 C 0.3100(7) 0.4677(7) 0.9807(3) 0.0960(16) Uiso 0.75 1 d P . . C102 C 0.4323(7) 0.4148(7) 0.9684(3) 0.0592(14) Uiso 0.50 1 d P . . C103 C 0.5214(6) 0.5332(6) 1.0069(3) 0.0514(13) Uiso 0.50 1 d P . . 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 Y1 0.01623(7) 0.01943(8) 0.02295(8) 0.00151(6) 0.00188(5) -0.00387(5) P1 0.01750(18) 0.01855(19) 0.01920(19) 0.00177(15) 0.00337(14) 0.00137(14) P2 0.01381(17) 0.01897(19) 0.02080(19) -0.00069(15) 0.00014(14) 0.00019(14) Si1 0.0302(2) 0.0308(3) 0.0220(2) 0.00552(19) 0.00319(19) 0.0128(2) Si2 0.0216(2) 0.0321(3) 0.0216(2) -0.00350(19) 0.00223(17) 0.00542(19) N1 0.0190(6) 0.0241(7) 0.0232(7) 0.0051(5) 0.0032(5) 0.0045(5) N2 0.0146(6) 0.0208(7) 0.0208(6) -0.0005(5) 0.0014(5) -0.0003(5) C1 0.0350(11) 0.0222(10) 0.0725(17) -0.0023(10) 0.0105(11) -0.0022(8) C2 0.0501(13) 0.0288(10) 0.0425(12) -0.0101(9) 0.0093(10) -0.0147(9) C3 0.0451(13) 0.0383(12) 0.0437(12) 0.0037(10) -0.0162(10) -0.0196(10) C4 0.0219(9) 0.0318(11) 0.0859(19) 0.0102(12) -0.0120(10) -0.0081(8) C5 0.0227(9) 0.0291(11) 0.095(2) -0.0084(12) 0.0244(11) -0.0092(8) C6 0.0487(13) 0.0419(13) 0.0494(13) -0.0060(11) 0.0275(11) -0.0198(11) C7 0.0662(16) 0.0395(13) 0.0370(12) 0.0161(10) 0.0037(11) -0.0212(12) C8 0.0431(12) 0.0261(10) 0.0656(16) 0.0155(10) -0.0095(11) -0.0049(9) C9 0.0177(7) 0.0176(7) 0.0210(7) 0.0014(6) 0.0017(6) 0.0023(6) C10 0.0242(8) 0.0210(8) 0.0234(8) -0.0001(6) 0.0075(6) -0.0008(6) C11 0.0420(11) 0.0324(10) 0.0329(10) -0.0020(8) 0.0028(8) 0.0134(9) C12 0.0733(17) 0.0336(12) 0.0432(13) 0.0015(10) 0.0162(12) 0.0242(11) C13 0.0688(16) 0.0255(10) 0.0446(13) -0.0082(9) 0.0283(12) -0.0060(10) C14 0.0423(12) 0.0513(14) 0.0374(11) -0.0176(10) 0.0128(9) -0.0195(10) C15 0.0265(9) 0.0445(12) 0.0315(10) -0.0082(8) 0.0066(7) -0.0026(8) C16 0.0227(8) 0.0209(8) 0.0245(8) 0.0040(6) 0.0081(6) 0.0040(6) C17 0.0371(10) 0.0335(10) 0.0246(9) 0.0051(7) 0.0063(7) 0.0034(8) C18 0.0463(12) 0.0390(11) 0.0310(10) 0.0137(8) 0.0151(9) 0.0130(9) C19 0.0372(10) 0.0298(10) 0.0486(12) 0.0177(9) 0.0234(9) 0.0090(8) C20 0.0269(9) 0.0374(11) 0.0527(13) 0.0122(10) 0.0107(9) -0.0040(8) C21 0.0220(8) 0.0354(10) 0.0344(10) 0.0088(8) 0.0043(7) -0.0004(7) C22 0.0170(7) 0.0302(9) 0.0235(8) -0.0001(7) -0.0004(6) 0.0045(6) C23 0.0356(10) 0.0317(10) 0.0271(9) 0.0034(7) -0.0029(7) 0.0079(8) C24 0.0548(14) 0.0420(12) 0.0361(11) 0.0082(9) -0.0051(10) 0.0183(11) C25 0.0506(13) 0.0649(16) 0.0289(10) 0.0071(10) -0.0067(9) 0.0273(12) C26 0.0388(11) 0.0652(16) 0.0288(10) -0.0067(10) -0.0128(9) 0.0166(11) C27 0.0290(9) 0.0403(11) 0.0307(10) -0.0075(8) -0.0061(7) 0.0082(8) C28 0.0194(7) 0.0197(8) 0.0307(9) -0.0038(7) 0.0030(6) -0.0036(6) C29 0.0195(8) 0.0304(10) 0.0438(11) -0.0041(8) 0.0013(7) -0.0033(7) C30 0.0242(9) 0.0364(11) 0.0624(15) -0.0084(10) 0.0071(9) -0.0126(8) C31 0.0420(12) 0.0238(10) 0.0741(17) -0.0018(10) 0.0133(11) -0.0117(9) C32 0.0405(11) 0.0209(9) 0.0659(15) 0.0049(9) 0.0093(11) 0.0015(8) C33 0.0235(8) 0.0231(9) 0.0462(11) 0.0005(8) 0.0053(8) -0.0014(7) C34 0.0542(14) 0.0636(16) 0.0312(11) -0.0010(10) -0.0125(10) 0.0270(12) C35 0.0660(16) 0.0331(11) 0.0480(13) 0.0164(10) 0.0250(12) 0.0215(11) C36 0.0292(9) 0.0385(11) 0.0315(9) 0.0038(8) 0.0058(7) 0.0134(8) C37 0.0453(12) 0.0555(14) 0.0237(9) 0.0057(9) 0.0059(8) 0.0099(10) C38 0.0268(9) 0.0473(12) 0.0366(11) -0.0065(9) 0.0034(8) 0.0121(8) C39 0.0347(10) 0.0418(12) 0.0387(11) -0.0172(9) -0.0014(8) 0.0056(9)