#------------------------------------------------------------------------------ #$Date: 2009-11-16 01:43:51 +0000 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: svn://www.crystallography.net/cod/cif/1/1100883.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_1100883 _publ_requested_journal 'Organometallics' _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _[local]_cod_cif_authors_sg_H-M P2(1)/n loop_ _publ_author_name 'Roesky, Peter W.' 'Panda, Tarun K.; Zulys, A.; Gamer, Michael T. ' _chemical_formula_sum 'C39 H47 N2 P2 Si2 Sm' _chemical_formula_weight 812.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0015 0.0009 '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' 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0522 0.0431 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.0667 0.0580 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sm' 'Sm' -0.4287 2.2815 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic 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 12.3050(8) _cell_length_b 19.6230(13) _cell_length_c 15.6500(10) _cell_angle_alpha 90.00 _cell_angle_beta 99.364(8) _cell_angle_gamma 90.00 _cell_volume 3728.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plates _exptl_crystal_colour red _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1660 _exptl_absorpt_coefficient_mu 0.938 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.56087 _diffrn_radiation_type AgK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe-IPDS' _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 24303 _diffrn_reflns_av_R_equivalents 0.1285 _diffrn_reflns_av_sigmaI/netI 0.0876 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 20.81 _reflns_number_total 7714 _reflns_number_gt 5976 _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^)+(0.1000P)^2^+0.0000P] 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 7714 _refine_ls_number_parameters 421 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0721 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.1742 _refine_ls_wR_factor_gt 0.1619 _refine_ls_goodness_of_fit_ref 1.120 _refine_ls_restrained_S_all 1.120 _refine_ls_shift/su_max 0.002 _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 C1 C -0.1097(5) 0.1802(3) 0.4317(4) 0.0440(14) Uani 1 1 d . . . H1 H -0.1167 0.1451 0.3902 0.053 Uiso 1 1 calc R . . C2 C -0.0991(5) 0.1551(3) 0.5176(5) 0.0438(15) Uani 1 1 d . . . H2A H -0.1012 0.1073 0.5204 0.053 Uiso 1 1 calc R . . C3 C -0.0859(4) 0.1865(3) 0.6003(4) 0.0372(13) Uani 1 1 d . . . H3A H -0.0763 0.1546 0.6458 0.045 Uiso 1 1 calc R . . C4 C -0.0839(5) 0.2534(2) 0.6298(4) 0.0347(14) Uani 1 1 d . . . H4A H -0.0762 0.2562 0.6904 0.042 Uiso 1 1 calc R . . C5 C -0.0907(4) 0.3176(3) 0.5904(4) 0.0347(12) Uani 1 1 d . . . H5A H -0.0863 0.3531 0.6311 0.042 Uiso 1 1 calc R . . C6 C -0.1025(5) 0.3420(3) 0.5052(4) 0.0369(12) Uani 1 1 d . . . H6A H -0.1054 0.3898 0.5020 0.044 Uiso 1 1 calc R . . C7 C -0.1111(5) 0.3109(3) 0.4232(4) 0.0381(12) Uani 1 1 d . . . H7A H -0.1174 0.3425 0.3776 0.046 Uiso 1 1 calc R . . C8 C -0.1122(5) 0.2440(3) 0.3951(4) 0.0425(15) Uani 1 1 d . . . H8A H -0.1155 0.2415 0.3347 0.051 Uiso 1 1 calc R . . C9 C 0.1872(5) 0.25479(18) 0.3926(3) 0.0206(10) Uani 1 1 d . . . H9A H 0.1484 0.2568 0.3321 0.025 Uiso 1 1 calc R . . C10 C 0.1588(4) 0.3960(2) 0.3716(3) 0.0246(9) Uani 1 1 d . . . C11 C 0.1576(4) 0.3979(3) 0.2836(3) 0.0353(11) Uani 1 1 d . . . H11A H 0.1976 0.3656 0.2570 0.042 Uiso 1 1 calc R . . C12 C 0.0980(5) 0.4470(3) 0.2349(4) 0.0484(14) Uani 1 1 d . . . H12A H 0.0981 0.4484 0.1749 0.058 Uiso 1 1 calc R . . C13 C 0.0379(5) 0.4945(3) 0.2717(4) 0.0495(15) Uani 1 1 d . . . H13A H -0.0046 0.5271 0.2371 0.059 Uiso 1 1 calc R . . C14 C 0.0409(4) 0.4937(3) 0.3589(4) 0.0425(13) Uani 1 1 d . . . H14A H 0.0018 0.5269 0.3849 0.051 Uiso 1 1 calc R . . C15 C 0.1009(4) 0.4443(2) 0.4103(4) 0.0342(11) Uani 1 1 d . . . H15A H 0.1021 0.4439 0.4706 0.041 Uiso 1 1 calc R . . C16 C 0.3770(4) 0.3497(2) 0.4236(3) 0.0219(9) Uani 1 1 d . . . C17 C 0.4401(3) 0.3980(2) 0.4737(3) 0.0236(9) Uani 1 1 d . . . H17A H 0.4099 0.4224 0.5160 0.028 Uiso 1 1 calc R . . C18 C 0.5476(4) 0.4107(2) 0.4618(3) 0.0310(10) Uani 1 1 d . . . H18A H 0.5904 0.4431 0.4966 0.037 Uiso 1 1 calc R . . C19 C 0.5914(4) 0.3762(3) 0.3995(3) 0.0333(11) Uani 1 1 d . . . H19A H 0.6646 0.3842 0.3921 0.040 Uiso 1 1 calc R . . C20 C 0.5285(4) 0.3298(3) 0.3478(3) 0.0374(12) Uani 1 1 d . . . H20A H 0.5584 0.3068 0.3043 0.045 Uiso 1 1 calc R . . C21 C 0.4211(4) 0.3167(2) 0.3594(3) 0.0308(10) Uani 1 1 d . . . H21A H 0.3783 0.2851 0.3233 0.037 Uiso 1 1 calc R . . C22 C 0.1997(4) 0.1194(2) 0.3375(3) 0.0238(9) Uani 1 1 d . . . C23 C 0.1438(4) 0.0594(2) 0.3476(3) 0.0331(11) Uani 1 1 d . . . H23A H 0.1242 0.0485 0.4015 0.040 Uiso 1 1 calc R . . C24 C 0.1170(5) 0.0159(3) 0.2782(4) 0.0428(13) Uani 1 1 d . . . H24A H 0.0807 -0.0253 0.2857 0.051 Uiso 1 1 calc R . . C25 C 0.1425(4) 0.0317(3) 0.1986(3) 0.0395(12) Uani 1 1 d . . . H25A H 0.1240 0.0016 0.1517 0.047 Uiso 1 1 calc R . . C26 C 0.1955(4) 0.0919(3) 0.1878(3) 0.0337(11) Uani 1 1 d . . . H26A H 0.2124 0.1035 0.1331 0.040 Uiso 1 1 calc R . . C27 C 0.2241(4) 0.1357(2) 0.2570(3) 0.0287(10) Uani 1 1 d . . . H27A H 0.2603 0.1768 0.2492 0.034 Uiso 1 1 calc R . . C28 C 0.3869(4) 0.1745(2) 0.4527(3) 0.0253(9) Uani 1 1 d . . . C29 C 0.4556(4) 0.1447(2) 0.4010(3) 0.0361(11) Uani 1 1 d . . . H29A H 0.4251 0.1209 0.3507 0.043 Uiso 1 1 calc R . . C30 C 0.5683(5) 0.1499(3) 0.4237(4) 0.0461(14) Uani 1 1 d . . . H30A H 0.6143 0.1299 0.3882 0.055 Uiso 1 1 calc R . . C31 C 0.6140(5) 0.1838(3) 0.4971(5) 0.0556(17) Uani 1 1 d . . . H31A H 0.6910 0.1873 0.5117 0.067 Uiso 1 1 calc R . . C32 C 0.5473(4) 0.2130(3) 0.5498(4) 0.0479(14) Uani 1 1 d . . . H32A H 0.5784 0.2361 0.6006 0.057 Uiso 1 1 calc R . . C33 C 0.4345(4) 0.2079(2) 0.5274(3) 0.0343(11) Uani 1 1 d . . . H33A H 0.3891 0.2275 0.5636 0.041 Uiso 1 1 calc R . . C34 C 0.2675(5) 0.4626(3) 0.6351(4) 0.0470(14) Uani 1 1 d . . . H34C H 0.2939 0.4797 0.5841 0.056 Uiso 1 1 calc R . . H34B H 0.3150 0.4789 0.6866 0.056 Uiso 1 1 calc R . . H34A H 0.1930 0.4786 0.6353 0.056 Uiso 1 1 calc R . . C35 C 0.4106(4) 0.3376(3) 0.6764(3) 0.0340(11) Uani 1 1 d . . . H35C H 0.4092 0.2897 0.6914 0.041 Uiso 1 1 calc R . . H35B H 0.4398 0.3639 0.7275 0.041 Uiso 1 1 calc R . . H35A H 0.4570 0.3441 0.6325 0.041 Uiso 1 1 calc R . . C36 C 0.1815(4) 0.3373(3) 0.7118(3) 0.0439(14) Uani 1 1 d . . . H36C H 0.1733 0.2882 0.7077 0.053 Uiso 1 1 calc R . . H36B H 0.1096 0.3586 0.6985 0.053 Uiso 1 1 calc R . . H36A H 0.2156 0.3496 0.7700 0.053 Uiso 1 1 calc R . . C37 C 0.1156(5) 0.0355(3) 0.6034(4) 0.0526(16) Uani 1 1 d . . . H37C H 0.0843 0.0148 0.5486 0.063 Uiso 1 1 calc R . . H37B H 0.0597 0.0624 0.6249 0.063 Uiso 1 1 calc R . . H37A H 0.1417 0.0001 0.6449 0.063 Uiso 1 1 calc R . . C38 C 0.2860(6) 0.1302(3) 0.6938(4) 0.0542(16) Uani 1 1 d . . . H38C H 0.3548 0.1534 0.6907 0.065 Uiso 1 1 calc R . . H38B H 0.2984 0.0949 0.7376 0.065 Uiso 1 1 calc R . . H38A H 0.2328 0.1627 0.7089 0.065 Uiso 1 1 calc R . . C39 C 0.3392(5) 0.0341(3) 0.5560(4) 0.0513(15) Uani 1 1 d . . . H39C H 0.3166 0.0191 0.4968 0.062 Uiso 1 1 calc R . . H39B H 0.3483 -0.0051 0.5942 0.062 Uiso 1 1 calc R . . H39A H 0.4085 0.0585 0.5606 0.062 Uiso 1 1 calc R . . N1 N 0.2155(3) 0.33235(19) 0.5364(2) 0.0225(8) Uani 1 1 d . . . N2 N 0.1887(3) 0.15457(18) 0.5132(3) 0.0226(8) Uani 1 1 d . . . Si1 Si 0.26894(11) 0.36673(6) 0.63387(8) 0.0267(3) Uani 1 1 d . . . Si2 Si 0.23247(11) 0.09143(6) 0.58749(8) 0.0274(3) Uani 1 1 d . . . P1 P 0.23608(10) 0.33103(5) 0.43812(7) 0.0191(2) Uani 1 1 d . . . P2 P 0.23821(9) 0.17538(5) 0.42901(7) 0.0189(2) Uani 1 1 d . . . Sm1 Sm 0.057188(18) 0.248290(9) 0.517652(14) 0.02030(13) Uani 1 1 d . . . 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 C1 0.038(3) 0.048(3) 0.047(3) -0.023(3) 0.009(3) -0.015(2) C2 0.030(3) 0.027(3) 0.076(4) -0.004(3) 0.015(3) -0.007(2) C3 0.028(3) 0.035(3) 0.051(3) 0.004(2) 0.016(3) -0.003(2) C4 0.028(3) 0.049(4) 0.031(3) 0.006(2) 0.017(3) 0.0064(19) C5 0.033(3) 0.037(3) 0.038(3) -0.004(2) 0.017(2) 0.008(2) C6 0.033(3) 0.033(3) 0.046(3) 0.006(2) 0.012(3) 0.012(2) C7 0.037(3) 0.045(3) 0.031(3) 0.007(2) 0.002(2) 0.014(2) C8 0.035(3) 0.059(4) 0.032(3) -0.006(2) 0.001(3) 0.006(2) C9 0.024(3) 0.017(2) 0.024(2) -0.0031(14) 0.012(2) -0.0012(14) C10 0.025(2) 0.019(2) 0.030(2) 0.0055(17) 0.0065(19) -0.0014(17) C11 0.041(3) 0.033(3) 0.032(3) 0.004(2) 0.006(2) 0.006(2) C12 0.056(4) 0.052(3) 0.036(3) 0.018(3) 0.002(3) -0.005(3) C13 0.044(3) 0.030(3) 0.071(4) 0.018(3) -0.002(3) 0.003(2) C14 0.040(3) 0.027(2) 0.058(4) 0.001(2) 0.000(3) 0.007(2) C15 0.036(3) 0.024(2) 0.043(3) 0.002(2) 0.008(2) 0.0038(19) C16 0.025(2) 0.021(2) 0.021(2) 0.0046(16) 0.0102(18) -0.0034(16) C17 0.031(2) 0.022(2) 0.017(2) 0.0026(15) 0.0035(18) -0.0037(16) C18 0.030(2) 0.028(2) 0.036(3) 0.0010(19) 0.008(2) -0.0113(18) C19 0.022(2) 0.039(3) 0.040(3) 0.002(2) 0.008(2) -0.006(2) C20 0.030(3) 0.045(3) 0.042(3) -0.011(2) 0.022(2) -0.006(2) C21 0.031(2) 0.030(2) 0.035(3) -0.0068(19) 0.015(2) -0.0103(19) C22 0.024(2) 0.022(2) 0.027(2) -0.0058(17) 0.0068(19) -0.0022(16) C23 0.044(3) 0.023(2) 0.034(3) -0.0034(19) 0.011(2) -0.006(2) C24 0.052(3) 0.025(2) 0.051(3) -0.007(2) 0.007(3) -0.011(2) C25 0.045(3) 0.033(3) 0.039(3) -0.020(2) 0.006(2) -0.007(2) C26 0.029(2) 0.043(3) 0.031(3) -0.013(2) 0.009(2) -0.001(2) C27 0.031(2) 0.030(2) 0.028(2) -0.0070(19) 0.012(2) -0.0062(19) C28 0.023(2) 0.018(2) 0.036(2) -0.0008(18) 0.011(2) 0.0030(16) C29 0.036(3) 0.033(3) 0.042(3) -0.001(2) 0.017(2) 0.010(2) C30 0.033(3) 0.051(3) 0.057(4) 0.001(3) 0.018(3) 0.012(2) C31 0.023(3) 0.062(4) 0.084(5) 0.010(4) 0.016(3) 0.011(3) C32 0.030(3) 0.057(4) 0.056(4) -0.012(3) 0.004(3) -0.002(2) C33 0.031(3) 0.032(2) 0.042(3) -0.001(2) 0.013(2) 0.003(2) C34 0.053(3) 0.033(3) 0.057(4) -0.021(2) 0.016(3) -0.004(2) C35 0.032(3) 0.044(3) 0.026(2) -0.001(2) 0.005(2) -0.008(2) C36 0.034(3) 0.075(4) 0.023(2) -0.006(3) 0.006(2) -0.013(3) C37 0.055(4) 0.043(3) 0.059(4) 0.027(3) 0.007(3) -0.008(3) C38 0.092(5) 0.036(3) 0.032(3) 0.001(2) 0.001(3) -0.013(3) C39 0.063(4) 0.037(3) 0.055(4) 0.014(3) 0.013(3) 0.027(3) N1 0.028(2) 0.0194(17) 0.0222(18) -0.0025(14) 0.0107(16) -0.0020(15) N2 0.0242(19) 0.0179(17) 0.028(2) 0.0005(14) 0.0115(16) 0.0006(14) Si1 0.0306(7) 0.0288(6) 0.0230(6) -0.0070(5) 0.0113(5) -0.0061(5) Si2 0.0351(7) 0.0197(6) 0.0272(6) 0.0029(5) 0.0049(6) 0.0010(5) P1 0.0233(6) 0.0156(5) 0.0208(5) -0.0007(4) 0.0107(5) -0.0024(4) P2 0.0200(6) 0.0158(5) 0.0229(6) -0.0032(4) 0.0093(5) 0.0003(4) Sm1 0.0189(2) 0.02117(18) 0.02323(19) -0.00092(7) 0.01054(13) 0.00054(7)