#------------------------------------------------------------------------------ #$Date: 2009-09-25 14:53:10 +0300 (Fri, 25 Sep 2009) $ #$Revision: 823 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/7104063.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_7104063 loop_ _publ_author_name 'Hans-Wolfram Lerner' 'Michael Bolte' 'Matthias Wagner' _publ_section_title ; A Novel Type of Phosphide: Synthesis and X-ray Crystal Structure Analysis of (tBu3Si)3P4Li3 ; _journal_name_full 'Chemical communications (Cambridge, England)' _journal_year 2003 _chemical_formula_sum 'C72 H162 Li6 P8 Si6' _chemical_formula_weight 1485.96 _chemical_name_systematic ; ? ; _space_group_IT_number 163 _symmetry_cell_setting Trigonal _symmetry_space_group_name_Hall '-P 3 2c' _symmetry_space_group_name_H-M 'P -3 1 c' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_formula_units_Z 2 _cell_length_a 14.2685(10) _cell_length_b 14.2685(10) _cell_length_c 26.965(2) _cell_measurement_reflns_used 6043 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 25.1 _cell_measurement_theta_min 2.6 _cell_volume 4754.3(6) _computing_cell_refinement 'X-Area (Stoe & Cie, 2001)' _computing_data_collection 'X-Area (Stoe & Cie, 2001)' _computing_data_reduction 'X-Area (Stoe & Cie, 2001)' _computing_molecular_graphics 'XP in SHELXTL-Plus (Sheldrick, 1991)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997) ' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990) ' _database_code_CSD 202252 _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full 0.973 _diffrn_measured_fraction_theta_max 0.973 _diffrn_measurement_device_type 'STOE IPDS II two-circle-diffractometer' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0971 _diffrn_reflns_av_sigmaI/netI 0.0930 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_number 14364 _diffrn_reflns_theta_full 25.34 _diffrn_reflns_theta_max 25.34 _diffrn_reflns_theta_min 2.24 _exptl_absorpt_coefficient_mu 0.256 _exptl_absorpt_correction_T_max 0.9873 _exptl_absorpt_correction_T_min 0.9435 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'MULABS (Spek, 1990; Blessing, 1995)' _exptl_crystal_colour 'light yellow' _exptl_crystal_density_diffrn 1.038 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1632 _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.375 _refine_diff_density_min -0.528 _refine_diff_density_rms 0.048 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.859 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 139 _refine_ls_number_reflns 2835 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.859 _refine_ls_R_factor_all 0.1021 _refine_ls_R_factor_gt 0.0528 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1119 _refine_ls_wR_factor_ref 0.1255 _reflns_number_gt 1583 _reflns_number_total 2835 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file b210984k.txt _[local]_cod_data_source_block wa187 _[local]_cod_cif_authors_sg_H-M P-31c 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' Li Li -0.0003 0.0001 '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_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' 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 Li1 Li 0.1649(5) 0.5000(5) 0.2779(2) 0.0481(14) Uani 1 1 d . . . P1 P 0.32998(8) 0.52243(7) 0.31695(4) 0.0427(2) Uani 1 1 d . . . P2 P 0.3333 0.6667 0.35533(7) 0.0447(4) Uani 1 3 d S . . Si1 Si 0.34554(7) 0.40120(7) 0.36570(4) 0.0424(3) Uani 1 1 d . . . C1 C 0.2902(3) 0.3958(4) 0.43240(17) 0.0618(12) Uani 1 1 d . . . C2 C 0.4965(3) 0.4356(3) 0.36868(17) 0.0563(11) Uani 1 1 d . . . C3 C 0.2600(3) 0.2657(3) 0.33003(18) 0.0590(11) Uani 1 1 d . . . C11 C 0.3688(4) 0.4920(4) 0.46312(19) 0.0787(14) Uani 1 1 d . . . H11A H 0.4373 0.4922 0.4661 0.118 Uiso 1 1 calc R . . H11B H 0.3383 0.4872 0.4962 0.118 Uiso 1 1 calc R . . H11C H 0.3816 0.5589 0.4470 0.118 Uiso 1 1 calc R . . C12 C 0.1858(3) 0.4023(4) 0.43003(18) 0.0726(14) Uani 1 1 d . . . H12A H 0.1314 0.3417 0.4104 0.109 Uiso 1 1 calc R . . H12B H 0.2014 0.4707 0.4145 0.109 Uiso 1 1 calc R . . H12C H 0.1582 0.3986 0.4637 0.109 Uiso 1 1 calc R . . C13 C 0.2631(5) 0.2902(4) 0.4608(2) 0.0909(17) Uani 1 1 d . . . H13A H 0.2122 0.2273 0.4412 0.136 Uiso 1 1 calc R . . H13B H 0.2305 0.2892 0.4929 0.136 Uiso 1 1 calc R . . H13C H 0.3297 0.2875 0.4661 0.136 Uiso 1 1 calc R . . C21 C 0.5352(4) 0.4200(4) 0.3175(2) 0.0801(15) Uani 1 1 d . . . H21A H 0.4908 0.3443 0.3071 0.120 Uiso 1 1 calc R . . H21B H 0.6112 0.4385 0.3197 0.120 Uiso 1 1 calc R . . H21C H 0.5283 0.4671 0.2931 0.120 Uiso 1 1 calc R . . C22 C 0.5715(3) 0.5564(3) 0.3808(2) 0.0695(13) Uani 1 1 d . . . H22A H 0.5608 0.6008 0.3563 0.104 Uiso 1 1 calc R . . H22B H 0.6470 0.5733 0.3800 0.104 Uiso 1 1 calc R . . H22C H 0.5543 0.5718 0.4140 0.104 Uiso 1 1 calc R . . C23 C 0.5166(3) 0.3689(4) 0.4074(2) 0.0729(14) Uani 1 1 d . . . H23A H 0.4705 0.2916 0.4002 0.109 Uiso 1 1 calc R . . H23B H 0.4995 0.3845 0.4405 0.109 Uiso 1 1 calc R . . H23C H 0.5928 0.3878 0.4063 0.109 Uiso 1 1 calc R . . C31 C 0.2851(4) 0.1768(3) 0.3462(2) 0.0806(16) Uani 1 1 d . . . H31A H 0.2747 0.1656 0.3821 0.121 Uiso 1 1 calc R . . H31B H 0.3603 0.1992 0.3378 0.121 Uiso 1 1 calc R . . H31C H 0.2364 0.1091 0.3289 0.121 Uiso 1 1 calc R . . C32 C 0.1381(3) 0.2205(3) 0.3379(2) 0.0804(16) Uani 1 1 d . . . H32A H 0.1215 0.2091 0.3734 0.121 Uiso 1 1 calc R . . H32B H 0.0974 0.1514 0.3203 0.121 Uiso 1 1 calc R . . H32C H 0.1178 0.2720 0.3249 0.121 Uiso 1 1 calc R . . C33 C 0.2765(4) 0.2801(3) 0.27393(19) 0.0714(13) Uani 1 1 d . . . H33A H 0.3531 0.3083 0.2661 0.107 Uiso 1 1 calc R . . H33B H 0.2543 0.3311 0.2622 0.107 Uiso 1 1 calc R . . H33C H 0.2327 0.2100 0.2575 0.107 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 Li1 0.051(3) 0.046(3) 0.051(4) -0.001(3) 0.002(3) 0.028(3) P1 0.0469(5) 0.0382(5) 0.0441(6) 0.0035(4) 0.0038(5) 0.0221(4) P2 0.0421(5) 0.0421(5) 0.0497(11) 0.000 0.000 0.0211(3) Si1 0.0363(5) 0.0428(5) 0.0496(6) 0.0049(4) -0.0048(5) 0.0208(4) C1 0.062(2) 0.083(3) 0.055(3) 0.022(2) 0.007(2) 0.047(2) C2 0.042(2) 0.058(2) 0.075(3) -0.013(2) -0.0079(19) 0.0299(18) C3 0.054(2) 0.041(2) 0.077(3) 0.003(2) -0.019(2) 0.0198(17) C11 0.094(3) 0.114(4) 0.055(3) -0.007(3) -0.009(2) 0.072(3) C12 0.066(3) 0.102(4) 0.066(3) 0.038(3) 0.024(2) 0.055(3) C13 0.108(4) 0.112(4) 0.077(4) 0.045(3) 0.013(3) 0.073(4) C21 0.056(3) 0.086(3) 0.102(4) -0.028(3) 0.001(3) 0.039(2) C22 0.042(2) 0.061(3) 0.103(4) -0.021(2) -0.014(2) 0.0241(19) C23 0.058(2) 0.074(3) 0.105(4) -0.019(3) -0.031(2) 0.047(2) C31 0.083(3) 0.046(2) 0.108(4) -0.004(2) -0.036(3) 0.029(2) C32 0.052(2) 0.054(2) 0.113(4) 0.019(3) -0.025(3) 0.010(2) C33 0.078(3) 0.053(2) 0.082(4) -0.017(2) -0.031(3) 0.032(2) 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 Li1 P1 2.452(6) . ? Li1 P1 2.489(6) 3_565 ? Li1 P1 2.582(6) 5 ? Li1 Li1 2.791(12) 6_565 ? Li1 Li1 2.857(12) 5 ? P1 Si1 2.2700(12) . ? P1 P2 2.2826(12) . ? P1 Li1 2.489(6) 2_665 ? P1 Li1 2.582(6) 5 ? P2 P1 2.2826(12) 2_665 ? P2 P1 2.2826(12) 3_565 ? Si1 C3 1.948(4) . ? Si1 C1 1.950(5) . ? Si1 C2 1.958(4) . ? C1 C11 1.512(7) . ? C1 C12 1.539(5) . ? C1 C13 1.557(6) . ? C2 C23 1.534(6) . ? C2 C22 1.542(5) . ? C2 C21 1.544(6) . ? C3 C33 1.529(7) . ? C3 C32 1.537(6) . ? C3 C31 1.544(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? 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 P1 Li1 P1 91.0(2) . 3_565 ? P1 Li1 P1 109.4(2) . 5 ? P1 Li1 P1 111.0(2) 3_565 5 ? P1 Li1 Li1 121.76(15) . 6_565 ? P1 Li1 Li1 58.2(2) 3_565 6_565 ? P1 Li1 Li1 55.0(2) 5 6_565 ? P1 Li1 Li1 57.6(2) . 5 ? P1 Li1 Li1 120.17(15) 3_565 5 ? P1 Li1 Li1 53.3(2) 5 5 ? Li1 Li1 Li1 94.3(3) 6_565 5 ? Si1 P1 P2 117.29(6) . . ? Si1 P1 Li1 127.11(14) . . ? P2 P1 Li1 84.15(15) . . ? Si1 P1 Li1 116.14(14) . 2_665 ? P2 P1 Li1 83.30(15) . 2_665 ? Li1 P1 Li1 113.9(3) . 2_665 ? Si1 P1 Li1 117.33(13) . 5 ? P2 P1 Li1 124.86(14) . 5 ? Li1 P1 Li1 69.1(2) . 5 ? Li1 P1 Li1 66.8(2) 2_665 5 ? P1 P2 P1 101.05(6) 2_665 3_565 ? P1 P2 P1 101.05(6) 2_665 . ? P1 P2 P1 101.05(6) 3_565 . ? C3 Si1 C1 112.1(2) . . ? C3 Si1 C2 109.52(17) . . ? C1 Si1 C2 110.19(19) . . ? C3 Si1 P1 102.65(13) . . ? C1 Si1 P1 111.84(12) . . ? C2 Si1 P1 110.34(14) . . ? C11 C1 C12 105.6(4) . . ? C11 C1 C13 108.8(4) . . ? C12 C1 C13 107.4(4) . . ? C11 C1 Si1 111.6(3) . . ? C12 C1 Si1 110.1(3) . . ? C13 C1 Si1 113.0(3) . . ? C23 C2 C22 108.0(3) . . ? C23 C2 C21 109.2(3) . . ? C22 C2 C21 104.7(4) . . ? C23 C2 Si1 113.3(3) . . ? C22 C2 Si1 110.5(3) . . ? C21 C2 Si1 110.8(3) . . ? C33 C3 C32 105.0(4) . . ? C33 C3 C31 107.8(4) . . ? C32 C3 C31 107.2(3) . . ? C33 C3 Si1 112.2(3) . . ? C32 C3 Si1 111.4(3) . . ? C31 C3 Si1 112.9(3) . . ? C1 C11 H11A 109.5 . . ? C1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C1 C12 H12A 109.5 . . ? C1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C1 C13 H13A 109.5 . . ? C1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C2 C21 H21A 109.5 . . ? C2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C2 C22 H22A 109.5 . . ? C2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C2 C23 H23A 109.5 . . ? C2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C3 C31 H31A 109.5 . . ? C3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C3 C32 H32A 109.5 . . ? C3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C3 C33 H33A 109.5 . . ? C3 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C3 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Li1 P1 Si1 125.13(13) 3_565 . . . ? P1 Li1 P1 Si1 -122.15(17) 5 . . . ? Li1 Li1 P1 Si1 177.6(3) 6_565 . . . ? Li1 Li1 P1 Si1 -109.11(18) 5 . . . ? P1 Li1 P1 P2 5.09(14) 3_565 . . . ? P1 Li1 P1 P2 117.8(2) 5 . . . ? Li1 Li1 P1 P2 57.6(4) 6_565 . . . ? Li1 Li1 P1 P2 130.85(9) 5 . . . ? P1 Li1 P1 Li1 -74.9(3) 3_565 . . 2_665 ? P1 Li1 P1 Li1 37.8(3) 5 . . 2_665 ? Li1 Li1 P1 Li1 -22.4(5) 6_565 . . 2_665 ? Li1 Li1 P1 Li1 50.86(16) 5 . . 2_665 ? P1 Li1 P1 Li1 -125.76(14) 3_565 . . 5 ? P1 Li1 P1 Li1 -13.0(3) 5 . . 5 ? Li1 Li1 P1 Li1 -73.3(4) 6_565 . . 5 ? Si1 P1 P2 P1 121.60(8) . . . 2_665 ? Li1 P1 P2 P1 -109.38(15) . . . 2_665 ? Li1 P1 P2 P1 5.59(15) 2_665 . . 2_665 ? Li1 P1 P2 P1 -49.94(18) 5 . . 2_665 ? Si1 P1 P2 P1 -134.68(7) . . . 3_565 ? Li1 P1 P2 P1 -5.66(15) . . . 3_565 ? Li1 P1 P2 P1 109.31(14) 2_665 . . 3_565 ? Li1 P1 P2 P1 53.79(18) 5 . . 3_565 ? P2 P1 Si1 C3 148.43(14) . . . . ? Li1 P1 Si1 C3 44.2(2) . . . . ? Li1 P1 Si1 C3 -115.4(2) 2_665 . . . ? Li1 P1 Si1 C3 -39.4(2) 5 . . . ? P2 P1 Si1 C1 28.10(16) . . . . ? Li1 P1 Si1 C1 -76.2(2) . . . . ? Li1 P1 Si1 C1 124.2(2) 2_665 . . . ? Li1 P1 Si1 C1 -159.7(2) 5 . . . ? P2 P1 Si1 C2 -94.94(14) . . . . ? Li1 P1 Si1 C2 160.8(2) . . . . ? Li1 P1 Si1 C2 1.2(2) 2_665 . . . ? Li1 P1 Si1 C2 77.2(2) 5 . . . ? C3 Si1 C1 C11 168.8(3) . . . . ? C2 Si1 C1 C11 46.5(3) . . . . ? P1 Si1 C1 C11 -76.6(3) . . . . ? C3 Si1 C1 C12 -74.3(3) . . . . ? C2 Si1 C1 C12 163.5(3) . . . . ? P1 Si1 C1 C12 40.3(4) . . . . ? C3 Si1 C1 C13 45.8(4) . . . . ? C2 Si1 C1 C13 -76.4(4) . . . . ? P1 Si1 C1 C13 160.5(3) . . . . ? C3 Si1 C2 C23 -77.1(3) . . . . ? C1 Si1 C2 C23 46.6(3) . . . . ? P1 Si1 C2 C23 170.6(3) . . . . ? C3 Si1 C2 C22 161.6(3) . . . . ? C1 Si1 C2 C22 -74.7(4) . . . . ? P1 Si1 C2 C22 49.3(4) . . . . ? C3 Si1 C2 C21 46.0(4) . . . . ? C1 Si1 C2 C21 169.8(3) . . . . ? P1 Si1 C2 C21 -66.3(3) . . . . ? C1 Si1 C3 C33 160.3(3) . . . . ? C2 Si1 C3 C33 -77.1(3) . . . . ? P1 Si1 C3 C33 40.2(3) . . . . ? C1 Si1 C3 C32 43.0(3) . . . . ? C2 Si1 C3 C32 165.6(3) . . . . ? P1 Si1 C3 C32 -77.2(3) . . . . ? C1 Si1 C3 C31 -77.6(4) . . . . ? C2 Si1 C3 C31 45.0(4) . . . . ? P1 Si1 C3 C31 162.2(3) . . . . ?