Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'M. Lappert' 'P. B. Hitchcock' 'Qi-Gu Huang' 'Meisu Zhou' _publ_contact_author_name 'Michael F. Lappert' _publ_contact_author_address ; Department of Chemistry University of Sussex BRIGHTON BN1 9QJ UNITED KINGDOM ; _publ_contact_author_email M.F.LAPPERT@SUSSEX.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; The coordination chemistry of the C1-symmetric bis(silyl)methyl ligand [CH(SiMe3){SiMe(OMe)2}]? revisited: Li/M- (M = Zn, Tl, Ce), Li4- or Ce2- methoxy-bridged alkyls ; _publ_requested_category FM data_(3)-dec1103 _database_code_depnum_ccdc_archive 'CCDC 275749' _audit_creation_date 2003-12-08T11:48:03-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C24 H60 Cl2 Li2 O8 Si4 Zn2' _chemical_formula_sum 'C24 H60 Cl2 Li2 O8 Si4 Zn2' _chemical_formula_weight 804.6 _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 9.6026(3) _cell_length_b 15.4505(3) _cell_length_c 13.7502(4) _cell_angle_alpha 90 _cell_angle_beta 94.667(1) _cell_angle_gamma 90 _cell_volume 2033.28(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10601 _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 colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.465 _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 0.617 _exptl_absorpt_correction_T_max 0.6704 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _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_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.633564E-1 _diffrn_orient_matrix_ub_12 0.259408E-1 _diffrn_orient_matrix_ub_13 -0.463473E-1 _diffrn_orient_matrix_ub_21 0.818389E-1 _diffrn_orient_matrix_ub_22 -0.98406E-2 _diffrn_orient_matrix_ub_23 0.48491E-1 _diffrn_orient_matrix_ub_31 0.143339E-1 _diffrn_orient_matrix_ub_32 -0.584746E-1 _diffrn_orient_matrix_ub_33 -0.287212E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_unetI/netI 0.0265 _diffrn_reflns_number 17527 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.75 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 3584 _reflns_number_gt 3195 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _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^)+(0.0368P)^2^+1.9864P] 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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 3584 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0366 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0781 _refine_ls_wR_factor_gt 0.0749 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.524 _refine_diff_density_min -0.381 _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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' O O 0.0106 0.006 '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 Zn Zn 0.04011(3) 0.437409(17) 0.924628(18) 0.02229(10) Uani 1 1 d . . . Li Li -0.1831(4) 0.5588(3) 0.8527(3) 0.0308(9) Uani 1 1 d . . . Cl Cl -0.17798(7) 0.40258(4) 0.85038(5) 0.03443(17) Uani 1 1 d . . . Si1 Si 0.22897(8) 0.37587(5) 0.75442(5) 0.03465(19) Uani 1 1 d . . . Si2 Si 0.30676(7) 0.33378(4) 0.97630(5) 0.02455(16) Uani 1 1 d . . . O1 O -0.00861(16) 0.56658(10) 0.93082(11) 0.0221(3) Uani 1 1 d . . . O2 O 0.18885(18) 0.26071(11) 0.99639(13) 0.0350(4) Uani 1 1 d . . . O3 O 0.33542(17) 0.38624(12) 1.08269(12) 0.0316(4) Uani 1 1 d . . . O4 O -0.2165(2) 0.59496(12) 0.71833(13) 0.0368(4) Uani 1 1 d . . . C1 C 0.0843(3) 0.63007(16) 0.8968(2) 0.0333(6) Uani 1 1 d . . . H1A H 0.1711 0.6307 0.9395 0.05 Uiso 1 1 calc R . . H1B H 0.0402 0.6872 0.8974 0.05 Uiso 1 1 calc R . . H1C H 0.1054 0.6158 0.8301 0.05 Uiso 1 1 calc R . . C2 C 0.2309(3) 0.40703(16) 0.88396(18) 0.0273(5) Uani 1 1 d . . . H2 H 0.2872 0.4614 0.8909 0.033 Uiso 1 1 calc R . . C3 C 0.1270(5) 0.4547(3) 0.6743(3) 0.0909(17) Uani 1 1 d . . . H3A H 0.1275 0.4364 0.6061 0.136 Uiso 1 1 calc R . . H3B H 0.1694 0.5122 0.6822 0.136 Uiso 1 1 calc R . . H3C H 0.0305 0.4569 0.6926 0.136 Uiso 1 1 calc R . . C4 C 0.4087(3) 0.3711(2) 0.7097(2) 0.0455(7) Uani 1 1 d . . . H4A H 0.4016 0.354 0.6409 0.068 Uiso 1 1 calc R . . H4B H 0.4653 0.3286 0.7483 0.068 Uiso 1 1 calc R . . H4C H 0.4528 0.4282 0.7168 0.068 Uiso 1 1 calc R . . C5 C 0.1488(4) 0.2664(3) 0.7353(3) 0.0680(11) Uani 1 1 d . . . H5A H 0.1484 0.2504 0.6663 0.102 Uiso 1 1 calc R . . H5B H 0.0527 0.2675 0.7544 0.102 Uiso 1 1 calc R . . H5C H 0.2033 0.2239 0.7753 0.102 Uiso 1 1 calc R . . C6 C 0.4725(3) 0.2777(2) 0.9527(2) 0.0405(7) Uani 1 1 d . . . H6A H 0.5439 0.3208 0.9405 0.061 Uiso 1 1 calc R . . H6B H 0.4563 0.2401 0.8956 0.061 Uiso 1 1 calc R . . H6C H 0.5044 0.2428 1.0097 0.061 Uiso 1 1 calc R . . C7 C 0.2174(3) 0.18410(19) 1.0524(2) 0.0470(7) Uani 1 1 d . . . H7A H 0.1313 0.1503 1.0546 0.07 Uiso 1 1 calc R . . H7B H 0.2527 0.1999 1.1189 0.07 Uiso 1 1 calc R . . H7C H 0.2877 0.1494 1.0222 0.07 Uiso 1 1 calc R . . C8 C 0.4638(3) 0.4296(2) 1.1122(2) 0.0427(7) Uani 1 1 d . . . H8A H 0.4575 0.4558 1.1766 0.064 Uiso 1 1 calc R . . H8B H 0.481 0.4749 1.0647 0.064 Uiso 1 1 calc R . . H8C H 0.5408 0.3878 1.1154 0.064 Uiso 1 1 calc R . . C9 C -0.2498(4) 0.5378(2) 0.6373(2) 0.0571(10) Uani 1 1 d . . . H9A H -0.2736 0.4794 0.6604 0.069 Uiso 1 1 calc R . . H9B H -0.17 0.5329 0.5964 0.069 Uiso 1 1 calc R . . C10 C -0.3725(4) 0.57808(19) 0.5811(2) 0.0513(8) Uani 1 1 d . . . H10A H -0.4607 0.5637 0.61 0.062 Uiso 1 1 calc R . . H10B H -0.3793 0.5593 0.512 0.062 Uiso 1 1 calc R . . C11 C -0.3402(3) 0.67348(19) 0.5902(2) 0.0445(7) Uani 1 1 d . . . H11A H -0.4269 0.7084 0.5848 0.053 Uiso 1 1 calc R . . H11B H -0.2793 0.6925 0.5395 0.053 Uiso 1 1 calc R . . C12 C -0.2654(3) 0.68078(16) 0.69130(19) 0.0345(6) Uani 1 1 d . . . H12A H -0.1857 0.7214 0.6907 0.041 Uiso 1 1 calc R . . H12B H -0.3301 0.7023 0.7383 0.041 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 Zn 0.02611(16) 0.02062(16) 0.01991(16) -0.00062(11) 0.00041(11) 0.00324(10) Li 0.034(2) 0.030(2) 0.028(2) -0.0003(18) -0.0026(17) 0.0049(17) Cl 0.0360(3) 0.0255(3) 0.0394(4) 0.0001(3) -0.0113(3) -0.0037(3) Si1 0.0357(4) 0.0476(5) 0.0209(3) -0.0020(3) 0.0041(3) 0.0065(3) Si2 0.0236(3) 0.0261(4) 0.0240(3) 0.0012(3) 0.0023(3) 0.0034(3) O1 0.0251(8) 0.0201(8) 0.0212(8) 0.0017(6) 0.0026(6) -0.0004(6) O2 0.0347(10) 0.0289(10) 0.0412(11) 0.0060(8) 0.0013(8) 0.0002(8) O3 0.0274(9) 0.0385(10) 0.0283(9) -0.0047(8) -0.0004(7) -0.0026(8) O4 0.0547(12) 0.0298(10) 0.0239(9) -0.0014(8) -0.0085(8) 0.0103(8) C1 0.0400(15) 0.0234(13) 0.0373(15) 0.0057(11) 0.0079(12) -0.0065(11) C2 0.0287(13) 0.0287(13) 0.0246(12) 0.0001(11) 0.0025(10) 0.0008(10) C3 0.107(3) 0.134(4) 0.0328(19) 0.022(2) 0.010(2) 0.071(3) C4 0.0476(17) 0.058(2) 0.0325(15) -0.0040(14) 0.0138(13) 0.0001(14) C5 0.060(2) 0.089(3) 0.055(2) -0.034(2) 0.0092(17) -0.023(2) C6 0.0346(15) 0.0493(18) 0.0380(15) 0.0033(13) 0.0046(12) 0.0118(13) C7 0.0535(19) 0.0317(15) 0.0557(19) 0.0138(14) 0.0042(15) -0.0036(13) C8 0.0310(15) 0.0521(19) 0.0441(17) -0.0055(14) -0.0032(12) -0.0101(13) C9 0.102(3) 0.0395(17) 0.0268(15) -0.0083(13) -0.0148(16) 0.0200(18) C10 0.074(2) 0.0426(18) 0.0341(16) 0.0017(14) -0.0162(15) -0.0093(15) C11 0.0552(18) 0.0397(16) 0.0361(16) 0.0081(13) -0.0110(13) 0.0012(14) C12 0.0448(16) 0.0249(13) 0.0331(14) 0.0047(11) -0.0008(12) 0.0008(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 Zn C2 2.014(2) . ? Zn O1 2.0356(16) 3_567 ? Zn O1 2.0532(15) . ? Zn Cl 2.3173(7) . ? Li O1 1.919(4) . ? Li O4 1.933(4) . ? Li O3 1.965(5) 3_567 ? Li Cl 2.414(4) . ? Si1 C2 1.844(2) . ? Si1 C3 1.865(4) . ? Si1 C5 1.868(4) . ? Si1 C4 1.880(3) . ? Si2 O2 1.6382(19) . ? Si2 O3 1.6755(18) . ? Si2 C2 1.809(2) . ? Si2 C6 1.863(3) . ? O1 C1 1.430(3) . ? O2 C7 1.427(3) . ? O3 C8 1.432(3) . ? O3 Li 1.965(5) 3_567 ? O4 C9 1.437(3) . ? O4 C12 1.445(3) . ? C9 C10 1.491(4) . ? C10 C11 1.509(4) . ? C11 C12 1.516(4) . ? 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 Zn O1 118.35(8) . 3_567 ? C2 Zn O1 116.97(9) . . ? O1 Zn O1 86.36(6) 3_567 . ? C2 Zn Cl 129.31(7) . . ? O1 Zn Cl 102.85(5) 3_567 . ? O1 Zn Cl 92.48(5) . . ? O1 Li O4 125.9(2) . . ? O1 Li O3 111.6(2) . 3_567 ? O4 Li O3 103.6(2) . 3_567 ? O1 Li Cl 93.03(16) . . ? O4 Li Cl 106.17(19) . . ? O3 Li Cl 117.1(2) 3_567 . ? Zn Cl Li 77.32(10) . . ? C2 Si1 C3 111.31(15) . . ? C2 Si1 C5 110.11(14) . . ? C3 Si1 C5 108.5(2) . . ? C2 Si1 C4 112.87(13) . . ? C3 Si1 C4 106.52(18) . . ? C5 Si1 C4 107.31(16) . . ? O2 Si2 O3 104.64(10) . . ? O2 Si2 C2 107.76(11) . . ? O3 Si2 C2 109.77(11) . . ? O2 Si2 C6 108.70(12) . . ? O3 Si2 C6 107.15(11) . . ? C2 Si2 C6 118.01(12) . . ? C1 O1 Li 113.56(19) . . ? C1 O1 Zn 119.13(14) . 3_567 ? Li O1 Zn 110.61(15) . 3_567 ? C1 O1 Zn 120.18(15) . . ? Li O1 Zn 96.15(14) . . ? Zn O1 Zn 93.64(6) 3_567 . ? C7 O2 Si2 123.91(17) . . ? C8 O3 Si2 123.34(17) . . ? C8 O3 Li 109.0(2) . 3_567 ? Si2 O3 Li 121.89(15) . 3_567 ? C9 O4 C12 108.47(19) . . ? C9 O4 Li 125.0(2) . . ? C12 O4 Li 122.46(19) . . ? Si2 C2 Si1 119.11(14) . . ? Si2 C2 Zn 105.92(12) . . ? Si1 C2 Zn 113.03(12) . . ? O4 C9 C10 105.2(2) . . ? C9 C10 C11 102.5(3) . . ? C10 C11 C12 103.2(2) . . ? O4 C12 C11 106.7(2) . . ? #===END data_(4)-jun104 _database_code_depnum_ccdc_archive 'CCDC 275750' _audit_creation_date 2004-06-01T14:07:19-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C28 H76 Li2 O8 Si8 Tl2' _chemical_formula_sum 'C28 H76 Li2 O8 Si8 Tl2' _chemical_formula_weight 1188.23 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0468(5) _cell_length_b 10.1659(4) _cell_length_c 12.8293(5) _cell_angle_alpha 95.078(3) _cell_angle_beta 91.045(2) _cell_angle_gamma 103.642(2) _cell_volume 1267.32(9) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10331 _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 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 588 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 6.574 _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 0.3118 _exptl_absorpt_correction_T_max 0.7012 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _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_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.746237E-1 _diffrn_orient_matrix_ub_12 -0.849782E-1 _diffrn_orient_matrix_ub_13 -0.13712E-2 _diffrn_orient_matrix_ub_21 -0.223711E-1 _diffrn_orient_matrix_ub_22 0.273707E-1 _diffrn_orient_matrix_ub_23 0.73166E-1 _diffrn_orient_matrix_ub_31 -0.666231E-1 _diffrn_orient_matrix_ub_32 0.486845E-1 _diffrn_orient_matrix_ub_33 -0.279019E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0599 _diffrn_reflns_av_unetI/netI 0.0524 _diffrn_reflns_number 10669 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 25.01 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.976 _diffrn_measured_fraction_theta_max 0.976 _reflns_number_total 4360 _reflns_number_gt 3939 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _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^)+(0.0487P)^2^+3.4529P] 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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 4360 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0439 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0975 _refine_ls_wR_factor_gt 0.0925 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.196 _refine_diff_density_min -2.006 _refine_diff_density_rms 0.146 #----------------------------------------------------------------------------# # 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' 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' Tl Tl -2.8358 9.6688 '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' 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 Tl Tl 0.46791(2) 0.34782(2) 0.757860(19) 0.03267(11) Uani 1 1 d . . . Li Li 0.6008(11) 0.1222(11) 0.9870(8) 0.032(2) Uani 1 1 d . . . Si1 Si 0.32449(17) 0.00526(17) 0.83694(13) 0.0280(3) Uani 1 1 d . . . Si2 Si 0.28157(17) 0.06834(18) 0.60277(13) 0.0299(4) Uani 1 1 d . . . Si3 Si 0.76422(17) 0.27964(17) 0.84890(13) 0.0275(3) Uani 1 1 d . . . Si4 Si 0.80207(19) 0.48460(18) 0.67079(14) 0.0332(4) Uani 1 1 d . . . O1 O 0.3982(4) 0.0807(4) 0.9550(3) 0.0293(9) Uani 1 1 d . . . O2 O 0.3742(5) -0.1376(4) 0.8560(3) 0.0336(10) Uani 1 1 d . . . O3 O 0.6731(5) 0.3150(4) 0.9521(3) 0.0329(10) Uani 1 1 d . . . O4 O 0.7141(4) 0.1122(4) 0.8595(3) 0.0299(9) Uani 1 1 d . . . C1 C 0.3872(6) 0.0872(6) 0.7251(5) 0.0262(12) Uani 1 1 d . . . H1 H 0.4704 0.054 0.7056 0.031 Uiso 1 1 calc R . . C2 C 0.7102(6) 0.3308(6) 0.7291(4) 0.0250(12) Uani 1 1 d . . . H2 H 0.7049 0.2526 0.6748 0.03 Uiso 1 1 calc R . . C3 C 0.3470(8) 0.1890(7) 1.0055(5) 0.0392(15) Uani 1 1 d . . . H3A H 0.3983 0.2223 1.0721 0.059 Uiso 1 1 calc R . . H3B H 0.2497 0.1557 1.0187 0.059 Uiso 1 1 calc R . . H3C H 0.3581 0.2633 0.9602 0.059 Uiso 1 1 calc R . . C4 C 0.3623(10) -0.2450(8) 0.7751(6) 0.055(2) Uani 1 1 d . . . H4A H 0.396 -0.3191 0.8017 0.082 Uiso 1 1 calc R . . H4B H 0.4167 -0.2114 0.7161 0.082 Uiso 1 1 calc R . . H4C H 0.2659 -0.2786 0.7516 0.082 Uiso 1 1 calc R . . C5 C 0.1367(8) -0.0282(9) 0.8536(7) 0.0513(19) Uani 1 1 d . . . H5A H 0.1052 0.0539 0.8426 0.077 Uiso 1 1 calc R . . H5B H 0.1161 -0.0535 0.9245 0.077 Uiso 1 1 calc R . . H5C H 0.0898 -0.1027 0.8023 0.077 Uiso 1 1 calc R . . C6 C 0.1321(8) 0.1466(9) 0.6213(6) 0.0491(18) Uani 1 1 d . . . H6A H 0.0787 0.1351 0.5551 0.074 Uiso 1 1 calc R . . H6B H 0.1651 0.2438 0.6439 0.074 Uiso 1 1 calc R . . H6C H 0.0741 0.1021 0.6748 0.074 Uiso 1 1 calc R . . C7 C 0.2114(8) -0.1118(8) 0.5447(6) 0.0449(17) Uani 1 1 d . . . H7A H 0.1573 -0.1119 0.4804 0.067 Uiso 1 1 calc R . . H7B H 0.1529 -0.1628 0.5951 0.067 Uiso 1 1 calc R . . H7C H 0.2874 -0.1545 0.5285 0.067 Uiso 1 1 calc R . . C8 C 0.3895(8) 0.1586(8) 0.5003(5) 0.0438(17) Uani 1 1 d . . . H8A H 0.3343 0.1491 0.4351 0.066 Uiso 1 1 calc R . . H8B H 0.4681 0.1185 0.4877 0.066 Uiso 1 1 calc R . . H8C H 0.4223 0.2552 0.5247 0.066 Uiso 1 1 calc R . . C9 C 0.6886(9) 0.4500(7) 1.0010(6) 0.0475(18) Uani 1 1 d . . . H9A H 0.6266 0.4484 1.0592 0.071 Uiso 1 1 calc R . . H9B H 0.6662 0.5082 0.9497 0.071 Uiso 1 1 calc R . . H9C H 0.7834 0.4858 1.0276 0.071 Uiso 1 1 calc R . . C10 C 0.7418(8) 0.0131(7) 0.7823(6) 0.0409(16) Uani 1 1 d . . . H10A H 0.7044 -0.0782 0.8036 0.061 Uiso 1 1 calc R . . H10B H 0.8411 0.0276 0.7756 0.061 Uiso 1 1 calc R . . H10C H 0.699 0.0219 0.7149 0.061 Uiso 1 1 calc R . . C11 C 0.9478(7) 0.3376(8) 0.8932(6) 0.0453(17) Uani 1 1 d . . . H11A H 1.0055 0.3193 0.8355 0.068 Uiso 1 1 calc R . . H11B H 0.965 0.2886 0.9525 0.068 Uiso 1 1 calc R . . H11C H 0.9696 0.4354 0.9148 0.068 Uiso 1 1 calc R . . C12 C 0.8036(10) 0.6416(8) 0.7576(8) 0.060(2) Uani 1 1 d . . . H12A H 0.8534 0.7212 0.7248 0.09 Uiso 1 1 calc R . . H12B H 0.8489 0.6376 0.8252 0.09 Uiso 1 1 calc R . . H12C H 0.7092 0.6487 0.7687 0.09 Uiso 1 1 calc R . . C13 C 0.7132(8) 0.4970(8) 0.5441(6) 0.0485(19) Uani 1 1 d . . . H13A H 0.7616 0.5787 0.513 0.073 Uiso 1 1 calc R . . H13B H 0.6186 0.5023 0.5568 0.073 Uiso 1 1 calc R . . H13C H 0.7128 0.4164 0.496 0.073 Uiso 1 1 calc R . . C14 C 0.9875(8) 0.4912(9) 0.6445(7) 0.052(2) Uani 1 1 d . . . H14A H 1.0285 0.576 0.6143 0.078 Uiso 1 1 calc R . . H14B H 0.9932 0.4136 0.5952 0.078 Uiso 1 1 calc R . . H14C H 1.037 0.4875 0.7102 0.078 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 Tl 0.03447(15) 0.02705(15) 0.03834(16) 0.00303(10) 0.00439(10) 0.01082(10) Li 0.027(5) 0.033(5) 0.037(5) 0.005(4) 0.004(4) 0.006(4) Si1 0.0269(8) 0.0267(8) 0.0303(8) 0.0056(7) -0.0024(6) 0.0052(7) Si2 0.0270(8) 0.0335(9) 0.0307(8) 0.0048(7) -0.0038(6) 0.0097(7) Si3 0.0276(8) 0.0238(8) 0.0300(8) 0.0015(6) 0.0029(6) 0.0040(6) Si4 0.0362(9) 0.0253(8) 0.0382(9) 0.0067(7) 0.0104(7) 0.0053(7) O1 0.032(2) 0.029(2) 0.029(2) 0.0003(17) -0.0016(17) 0.0109(18) O2 0.047(3) 0.024(2) 0.029(2) 0.0007(17) -0.0061(19) 0.0077(19) O3 0.042(2) 0.026(2) 0.030(2) -0.0027(17) 0.0100(19) 0.0077(19) O4 0.036(2) 0.024(2) 0.031(2) 0.0014(17) 0.0059(18) 0.0101(18) C1 0.025(3) 0.025(3) 0.031(3) 0.005(2) 0.000(2) 0.010(2) C2 0.029(3) 0.018(3) 0.028(3) -0.002(2) 0.004(2) 0.006(2) C3 0.047(4) 0.040(4) 0.035(3) -0.003(3) 0.006(3) 0.020(3) C4 0.080(6) 0.039(4) 0.045(4) 0.003(3) -0.011(4) 0.015(4) C5 0.034(4) 0.064(5) 0.054(4) 0.017(4) 0.004(3) 0.004(4) C6 0.038(4) 0.066(5) 0.051(4) 0.011(4) -0.004(3) 0.026(4) C7 0.040(4) 0.047(4) 0.044(4) -0.001(3) -0.010(3) 0.006(3) C8 0.052(4) 0.055(5) 0.030(3) 0.013(3) 0.001(3) 0.018(4) C9 0.056(5) 0.031(4) 0.051(4) -0.009(3) 0.007(4) 0.006(3) C10 0.050(4) 0.034(4) 0.044(4) 0.006(3) 0.011(3) 0.020(3) C11 0.035(4) 0.051(4) 0.046(4) 0.008(3) -0.003(3) 0.002(3) C12 0.074(6) 0.027(4) 0.074(6) 0.001(4) 0.026(5) 0.001(4) C13 0.047(4) 0.047(4) 0.058(5) 0.029(4) 0.010(4) 0.016(4) C14 0.040(4) 0.054(5) 0.061(5) 0.023(4) 0.014(3) 0.001(4) #----------------------------------------------------------------------------# # 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 Tl C2 2.512(6) . ? Tl C1 2.575(6) . ? Li O1 2.006(11) . ? Li O2 2.013(12) 2_657 ? Li O3 2.017(11) . ? Li O4 2.019(11) . ? Li O1 2.256(11) 2_657 ? Si1 O2 1.679(4) . ? Si1 O1 1.708(4) . ? Si1 C1 1.774(6) . ? Si1 C5 1.856(8) . ? Si2 C1 1.848(6) . ? Si2 C6 1.867(7) . ? Si2 C7 1.880(8) . ? Si2 C8 1.882(7) . ? Si3 O4 1.676(4) . ? Si3 O3 1.684(4) . ? Si3 C2 1.781(6) . ? Si3 C11 1.860(7) . ? Si4 C2 1.846(6) . ? Si4 C12 1.861(8) . ? Si4 C13 1.869(8) . ? Si4 C14 1.886(8) . ? O1 C3 1.431(8) . ? O2 C4 1.420(9) . ? O3 C9 1.429(8) . ? O4 C10 1.428(8) . ? 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 Tl C1 89.57(18) . . ? O1 Li O2 106.5(5) . 2_657 ? O1 Li O3 105.3(5) . . ? O2 Li O3 103.1(5) 2_657 . ? O1 Li O4 114.1(5) . . ? O2 Li O4 138.7(6) 2_657 . ? O3 Li O4 73.4(4) . . ? O1 Li O1 95.9(4) . 2_657 ? O2 Li O1 68.7(4) 2_657 2_657 ? O3 Li O1 158.8(6) . 2_657 ? O4 Li O1 99.5(5) . 2_657 ? O2 Si1 O1 91.0(2) . . ? O2 Si1 C1 116.3(3) . . ? O1 Si1 C1 116.3(3) . . ? O2 Si1 C5 108.0(3) . . ? O1 Si1 C5 105.6(3) . . ? C1 Si1 C5 116.5(3) . . ? C1 Si2 C6 111.7(3) . . ? C1 Si2 C7 115.1(3) . . ? C6 Si2 C7 106.9(4) . . ? C1 Si2 C8 108.9(3) . . ? C6 Si2 C8 107.5(4) . . ? C7 Si2 C8 106.4(4) . . ? O4 Si3 O3 91.8(2) . . ? O4 Si3 C2 114.3(3) . . ? O3 Si3 C2 114.0(3) . . ? O4 Si3 C11 108.0(3) . . ? O3 Si3 C11 106.2(3) . . ? C2 Si3 C11 119.0(3) . . ? C2 Si4 C12 111.5(3) . . ? C2 Si4 C13 109.3(3) . . ? C12 Si4 C13 107.6(4) . . ? C2 Si4 C14 114.8(3) . . ? C12 Si4 C14 105.5(4) . . ? C13 Si4 C14 107.9(4) . . ? C3 O1 Si1 118.3(4) . . ? C3 O1 Li 107.8(5) . . ? Si1 O1 Li 123.0(4) . . ? C3 O1 Li 128.2(5) . 2_657 ? Si1 O1 Li 91.9(3) . 2_657 ? Li O1 Li 84.1(4) . 2_657 ? C4 O2 Si1 121.9(4) . . ? C4 O2 Li 134.5(5) . 2_657 ? Si1 O2 Li 101.8(4) . 2_657 ? C9 O3 Si3 122.4(4) . . ? C9 O3 Li 138.3(5) . . ? Si3 O3 Li 97.3(4) . . ? C10 O4 Si3 122.5(4) . . ? C10 O4 Li 139.4(5) . . ? Si3 O4 Li 97.5(4) . . ? Si1 C1 Si2 122.1(3) . . ? Si1 C1 Tl 114.3(3) . . ? Si2 C1 Tl 101.2(2) . . ? Si3 C2 Si4 123.5(3) . . ? Si3 C2 Tl 104.3(3) . . ? Si4 C2 Tl 108.5(3) . . ? #===END data_(4')-dec1604 _database_code_depnum_ccdc_archive 'CCDC 275751' _audit_creation_date 2004-12-09T14:57:09-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C28 H76 Li2 O8 Si8 Tl2' _chemical_formula_sum 'C28 H76 Li2 O8 Si8 Tl2' _chemical_formula_weight 1188.23 _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 13.2498(5) _cell_length_b 9.4096(4) _cell_length_c 20.7365(7) _cell_angle_alpha 90 _cell_angle_beta 93.816(2) _cell_angle_gamma 90 _cell_volume 2579.60(17) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 20862 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.53 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 6.459 _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 0.2828 _exptl_absorpt_correction_T_max 0.462 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.98528E-2 _diffrn_orient_matrix_ub_12 0.7616E-3 _diffrn_orient_matrix_ub_13 0.48231E-1 _diffrn_orient_matrix_ub_21 0.2494E-2 _diffrn_orient_matrix_ub_22 -0.106216 _diffrn_orient_matrix_ub_23 0.2455E-3 _diffrn_orient_matrix_ub_31 0.749546E-1 _diffrn_orient_matrix_ub_32 0.34341E-2 _diffrn_orient_matrix_ub_33 -0.31026E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0845 _diffrn_reflns_av_unetI/netI 0.0733 _diffrn_reflns_number 20344 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 26.03 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 5064 _reflns_number_gt 3675 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _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^)+(0.0322P)^2^+4.9101P] 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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 5064 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0803 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.0956 _refine_ls_wR_factor_gt 0.0855 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.481 _refine_diff_density_min -1.063 _refine_diff_density_rms 0.156 #----------------------------------------------------------------------------# # 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' 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' Tl Tl -2.8358 9.6688 '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' 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 Tl Tl 0.61746(2) 0.92705(3) 0.382278(13) 0.03456(11) Uani 1 1 d . . . Li Li 0.5959(8) 0.5745(12) 0.5125(5) 0.033(3) Uani 1 1 d . . . Si1 Si 0.42454(14) 0.6440(2) 0.39252(9) 0.0283(4) Uani 1 1 d . . . Si2 Si 0.45766(14) 0.8018(2) 0.26029(9) 0.0327(5) Uani 1 1 d . . . Si3 Si 0.76859(15) 0.6800(2) 0.46028(10) 0.0337(5) Uani 1 1 d . . . Si4 Si 0.87861(16) 0.8766(2) 0.36040(11) 0.0405(5) Uani 1 1 d . . . O1 O 0.4646(3) 0.6506(5) 0.47181(19) 0.0275(10) Uani 1 1 d . . . O2 O 0.4208(3) 0.4661(5) 0.3945(2) 0.0326(11) Uani 1 1 d . . . O3 O 0.6878(4) 0.7504(5) 0.5106(2) 0.0397(12) Uani 1 1 d . . . O4 O 0.7044(4) 0.5278(5) 0.4551(2) 0.0354(12) Uani 1 1 d . . . C1 C 0.5053(5) 0.7209(7) 0.3374(3) 0.0309(16) Uani 1 1 d . . . H1 H 0.5527 0.6438 0.3258 0.037 Uiso 1 1 calc R . . C2 C 0.7726(5) 0.7713(8) 0.3846(3) 0.0341(17) Uani 1 1 d . . . H2 H 0.7592 0.698 0.3501 0.041 Uiso 1 1 calc R . . C3 C 0.4469(5) 0.7776(8) 0.5076(3) 0.0371(17) Uani 1 1 d . . . H3A H 0.474 0.7657 0.5524 0.056 Uiso 1 1 calc R . . H3B H 0.374 0.7959 0.5069 0.056 Uiso 1 1 calc R . . H3C H 0.4805 0.858 0.488 0.056 Uiso 1 1 calc R . . C4 C 0.4031(6) 0.3827(8) 0.3372(4) 0.048(2) Uani 1 1 d . . . H4A H 0.4038 0.2816 0.3487 0.072 Uiso 1 1 calc R . . H4B H 0.4562 0.4017 0.3077 0.072 Uiso 1 1 calc R . . H4C H 0.3371 0.4074 0.3161 0.072 Uiso 1 1 calc R . . C5 C 0.2910(5) 0.7099(9) 0.3883(3) 0.0427(19) Uani 1 1 d . . . H5A H 0.2907 0.814 0.3871 0.064 Uiso 1 1 calc R . . H5B H 0.2577 0.6772 0.4265 0.064 Uiso 1 1 calc R . . H5C H 0.2545 0.6729 0.3492 0.064 Uiso 1 1 calc R . . C6 C 0.3783(6) 0.9642(8) 0.2727(4) 0.052(2) Uani 1 1 d . . . H6A H 0.3547 1.0035 0.2306 0.078 Uiso 1 1 calc R . . H6B H 0.419 1.0355 0.2971 0.078 Uiso 1 1 calc R . . H6C H 0.32 0.9381 0.2968 0.078 Uiso 1 1 calc R . . C7 C 0.3786(6) 0.6832(9) 0.2050(3) 0.049(2) Uani 1 1 d . . . H7A H 0.357 0.7354 0.1656 0.073 Uiso 1 1 calc R . . H7B H 0.319 0.6519 0.2267 0.073 Uiso 1 1 calc R . . H7C H 0.4185 0.6002 0.1937 0.073 Uiso 1 1 calc R . . C8 C 0.5671(6) 0.8608(9) 0.2133(4) 0.049(2) Uani 1 1 d . . . H8A H 0.5413 0.9037 0.1724 0.074 Uiso 1 1 calc R . . H8B H 0.6093 0.7785 0.2044 0.074 Uiso 1 1 calc R . . H8C H 0.6075 0.9309 0.2386 0.074 Uiso 1 1 calc R . . C9 C 0.7103(6) 0.8769(8) 0.5475(4) 0.048(2) Uani 1 1 d . . . H9A H 0.6533 0.8995 0.5735 0.072 Uiso 1 1 calc R . . H9B H 0.7217 0.9561 0.5182 0.072 Uiso 1 1 calc R . . H9C H 0.7712 0.8615 0.5761 0.072 Uiso 1 1 calc R . . C10 C 0.7260(7) 0.4194(9) 0.4089(5) 0.068(3) Uani 1 1 d . . . H10A H 0.6804 0.3386 0.4135 0.102 Uiso 1 1 calc R . . H10B H 0.7962 0.3877 0.4168 0.102 Uiso 1 1 calc R . . H10C H 0.7162 0.4581 0.3651 0.102 Uiso 1 1 calc R . . C11 C 0.8899(6) 0.6507(10) 0.5090(4) 0.059(2) Uani 1 1 d . . . H11A H 0.9281 0.7399 0.5123 0.089 Uiso 1 1 calc R . . H11B H 0.9298 0.5785 0.4881 0.089 Uiso 1 1 calc R . . H11C H 0.8758 0.6183 0.5524 0.089 Uiso 1 1 calc R . . C12 C 0.9029(7) 1.0293(9) 0.4177(4) 0.061(3) Uani 1 1 d . . . H12A H 0.9602 1.0853 0.4042 0.092 Uiso 1 1 calc R . . H12B H 0.9186 0.9926 0.4615 0.092 Uiso 1 1 calc R . . H12C H 0.8426 1.0896 0.4174 0.092 Uiso 1 1 calc R . . C13 C 0.8461(7) 0.9491(10) 0.2777(4) 0.067(3) Uani 1 1 d . . . H13A H 0.9027 1.0063 0.2639 0.1 Uiso 1 1 calc R . . H13B H 0.7856 1.0087 0.2784 0.1 Uiso 1 1 calc R . . H13C H 0.8332 0.8704 0.2473 0.1 Uiso 1 1 calc R . . C14 C 1.0016(7) 0.7783(11) 0.3576(5) 0.084(3) Uani 1 1 d . . . H14A H 1.054 0.8434 0.3442 0.126 Uiso 1 1 calc R . . H14B H 0.9935 0.6998 0.3267 0.126 Uiso 1 1 calc R . . H14C H 1.0215 0.7403 0.4006 0.126 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 Tl 0.04037(17) 0.02731(16) 0.03509(17) -0.00243(14) -0.00437(12) 0.00126(14) Li 0.037(6) 0.032(7) 0.030(6) 0.007(6) 0.000(5) -0.001(6) Si1 0.0319(10) 0.0258(11) 0.0269(10) 0.0023(9) -0.0016(8) 0.0006(8) Si2 0.0350(11) 0.0331(12) 0.0290(10) 0.0036(9) -0.0042(9) 0.0006(9) Si3 0.0345(11) 0.0285(11) 0.0376(11) 0.0018(9) 0.0001(9) 0.0008(9) Si4 0.0361(11) 0.0400(13) 0.0455(13) 0.0046(10) 0.0024(10) -0.0065(10) O1 0.042(3) 0.021(3) 0.020(2) 0.000(2) 0.004(2) 0.005(2) O2 0.049(3) 0.024(3) 0.025(2) -0.003(2) 0.003(2) -0.007(2) O3 0.052(3) 0.027(3) 0.039(3) -0.008(2) -0.001(2) 0.001(2) O4 0.046(3) 0.025(3) 0.037(3) -0.003(2) 0.012(2) 0.001(2) C1 0.038(4) 0.024(4) 0.031(4) 0.001(3) -0.002(3) 0.001(3) C2 0.037(4) 0.031(4) 0.033(4) 0.000(3) -0.002(3) -0.003(3) C3 0.039(4) 0.031(4) 0.041(4) -0.009(4) 0.001(3) 0.004(3) C4 0.071(6) 0.035(5) 0.037(4) -0.012(4) 0.001(4) -0.008(4) C5 0.042(4) 0.049(5) 0.037(4) 0.009(4) 0.002(4) -0.004(4) C6 0.069(6) 0.038(5) 0.046(5) 0.007(4) -0.008(4) 0.009(4) C7 0.056(5) 0.053(6) 0.036(4) 0.009(4) -0.009(4) -0.013(4) C8 0.056(5) 0.047(5) 0.045(5) 0.006(4) 0.007(4) -0.002(4) C9 0.074(6) 0.034(4) 0.035(4) -0.003(4) -0.010(4) 0.004(4) C10 0.092(7) 0.038(5) 0.081(7) -0.016(5) 0.054(6) -0.009(5) C11 0.054(5) 0.064(6) 0.058(6) 0.015(5) -0.007(4) 0.010(5) C12 0.066(6) 0.046(5) 0.070(6) 0.005(5) -0.010(5) -0.025(4) C13 0.065(6) 0.084(8) 0.050(5) 0.015(5) 0.001(5) -0.031(5) C14 0.062(6) 0.070(7) 0.124(9) 0.018(7) 0.028(6) 0.003(5) #----------------------------------------------------------------------------# # 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 Tl C2 2.522(7) . ? Tl C1 2.580(6) . ? Li O4 1.975(13) . ? Li O2 1.994(12) 3_666 ? Li O1 2.014(12) . ? Li O3 2.057(12) . ? Li O1 2.295(12) 3_666 ? Si1 O2 1.676(5) . ? Si1 O1 1.695(4) . ? Si1 C1 1.771(7) . ? Si1 C5 1.872(7) . ? Si2 C1 1.844(6) . ? Si2 C7 1.870(7) . ? Si2 C6 1.881(8) . ? Si2 C8 1.884(8) . ? Si3 O4 1.666(5) . ? Si3 O3 1.680(5) . ? Si3 C2 1.793(7) . ? Si3 C11 1.862(8) . ? Si4 C2 1.817(7) . ? Si4 C13 1.869(8) . ? Si4 C14 1.878(9) . ? Si4 C12 1.879(8) . ? O1 C3 1.435(7) . ? O2 C4 1.429(8) . ? O3 C9 1.436(8) . ? O4 C10 1.441(9) . ? 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 Tl C1 91.1(2) . . ? O4 Li O2 132.3(6) . 3_666 ? O4 Li O1 118.0(6) . . ? O2 Li O1 108.9(6) 3_666 . ? O4 Li O3 73.3(4) . . ? O2 Li O3 106.0(5) 3_666 . ? O1 Li O3 101.6(5) . . ? O4 Li O1 98.9(5) . 3_666 ? O2 Li O1 67.9(4) 3_666 3_666 ? O1 Li O1 95.0(5) . 3_666 ? O3 Li O1 163.4(6) . 3_666 ? O2 Si1 O1 91.2(2) . . ? O2 Si1 C1 116.3(3) . . ? O1 Si1 C1 116.6(3) . . ? O2 Si1 C5 107.6(3) . . ? O1 Si1 C5 105.5(3) . . ? C1 Si1 C5 116.4(3) . . ? C1 Si2 C7 115.5(3) . . ? C1 Si2 C6 112.3(3) . . ? C7 Si2 C6 105.9(4) . . ? C1 Si2 C8 109.9(3) . . ? C7 Si2 C8 106.1(4) . . ? C6 Si2 C8 106.7(4) . . ? O4 Si3 O3 92.0(2) . . ? O4 Si3 C2 113.6(3) . . ? O3 Si3 C2 114.3(3) . . ? O4 Si3 C11 109.0(3) . . ? O3 Si3 C11 106.5(3) . . ? C2 Si3 C11 118.1(4) . . ? C2 Si4 C13 108.5(3) . . ? C2 Si4 C14 115.3(4) . . ? C13 Si4 C14 107.4(5) . . ? C2 Si4 C12 110.2(4) . . ? C13 Si4 C12 108.7(4) . . ? C14 Si4 C12 106.5(5) . . ? C3 O1 Si1 118.8(4) . . ? C3 O1 Li 104.3(5) . . ? Si1 O1 Li 126.8(4) . . ? C3 O1 Li 128.6(5) . 3_666 ? Si1 O1 Li 90.8(3) . 3_666 ? Li O1 Li 85.0(5) . 3_666 ? C4 O2 Si1 122.2(4) . . ? C4 O2 Li 132.5(5) . 3_666 ? Si1 O2 Li 102.7(4) . 3_666 ? C9 O3 Si3 122.7(5) . . ? C9 O3 Li 139.4(6) . . ? Si3 O3 Li 95.5(4) . . ? C10 O4 Si3 121.9(5) . . ? C10 O4 Li 137.9(6) . . ? Si3 O4 Li 99.1(4) . . ? Si1 C1 Si2 122.8(4) . . ? Si1 C1 Tl 115.6(3) . . ? Si2 C1 Tl 99.1(3) . . ? Si3 C2 Si4 124.8(4) . . ? Si3 C2 Tl 102.9(3) . . ? Si4 C2 Tl 108.8(3) . . ? #===END data_(5)-jun904 _database_code_depnum_ccdc_archive 'CCDC 275752' _audit_creation_date 2004-06-09T14:32:08-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C22 H60 Li4 O7 Si6' _chemical_formula_sum 'C22 H60 Li4 O7 Si6' _chemical_formula_weight 633 _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 10.0199(1) _cell_length_b 22.1861(4) _cell_length_c 18.1958(4) _cell_angle_alpha 90 _cell_angle_beta 99.023(1) _cell_angle_gamma 90 _cell_volume 3994.92(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 43405 _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 0.35 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.052 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.239 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _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_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.511728E-1 _diffrn_orient_matrix_ub_12 0.191838E-1 _diffrn_orient_matrix_ub_13 -0.456345E-1 _diffrn_orient_matrix_ub_21 -0.866984E-1 _diffrn_orient_matrix_ub_22 -0.15137E-1 _diffrn_orient_matrix_ub_23 0.13877E-1 _diffrn_orient_matrix_ub_31 -0.87305E-2 _diffrn_orient_matrix_ub_32 0.378742E-1 _diffrn_orient_matrix_ub_33 0.286607E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.1012 _diffrn_reflns_av_unetI/netI 0.0409 _diffrn_reflns_number 48461 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.99 _diffrn_measured_fraction_theta_max 0.99 _reflns_number_total 6930 _reflns_number_gt 5984 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _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 ; The H atoms on C1,C8,C15, and C22 were refined; other H atoms were riding. 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^)+(0.0798P)^2^+2.6784P] 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 6930 _refine_ls_number_parameters 376 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0664 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.152 _refine_ls_wR_factor_gt 0.1441 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.565 _refine_diff_density_min -0.369 _refine_diff_density_rms 0.063 #----------------------------------------------------------------------------# # 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' 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' Li Li -0.0003 0.0001 '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 Li1 Li -0.1879(5) 0.6610(2) 0.7141(3) 0.0410(10) Uani 1 1 d . . . Li2 Li -0.0339(4) 0.7508(2) 0.6862(2) 0.0368(9) Uani 1 1 d . . . Li3 Li 0.0022(5) 0.6807(2) 0.8300(3) 0.0379(10) Uani 1 1 d . . . Li4 Li 0.0478(4) 0.6181(2) 0.6871(3) 0.0399(10) Uani 1 1 d . . . Si1 Si -0.37016(7) 0.78896(3) 0.68969(4) 0.03350(19) Uani 1 1 d . . . Si2 Si -0.10969(7) 0.80384(3) 0.80594(4) 0.03187(19) Uani 1 1 d . . . Si3 Si -0.25929(9) 0.58693(4) 0.86482(5) 0.0484(2) Uani 1 1 d . . . Si4 Si 0.02915(8) 0.55961(3) 0.83219(4) 0.0373(2) Uani 1 1 d . . . Si5 Si -0.22851(7) 0.56740(3) 0.56662(4) 0.0384(2) Uani 1 1 d . . . Si6 Si -0.02789(7) 0.67268(3) 0.55263(4) 0.03411(19) Uani 1 1 d . . . O1 O -0.00833(18) 0.82570(8) 0.74615(10) 0.0379(4) Uani 1 1 d . . . O2 O -0.01951(18) 0.76044(8) 0.87114(10) 0.0388(4) Uani 1 1 d . . . O3 O 0.10585(19) 0.61513(9) 0.88522(10) 0.0421(4) Uani 1 1 d . . . O4 O 0.10762(19) 0.55328(8) 0.75771(11) 0.0409(4) Uani 1 1 d . . . O5 O 0.10646(17) 0.63191(9) 0.58976(10) 0.0392(4) Uani 1 1 d . . . O6 O -0.00618(19) 0.74429(8) 0.58266(10) 0.0396(4) Uani 1 1 d . . . O7 O 0.06989(17) 0.69086(8) 0.74031(10) 0.0352(4) Uani 1 1 d . . . C1 C -0.2291(2) 0.75538(11) 0.75195(15) 0.0311(5) Uani 1 1 d . . . H1 H -0.259(3) 0.7333(13) 0.7854(16) 0.036(7) Uiso 1 1 d . . . C2 C -0.3081(3) 0.83440(14) 0.61563(18) 0.0500(7) Uani 1 1 d . . . H2C H -0.2491 0.8667 0.6386 0.075 Uiso 1 1 calc R . . H2B H -0.3853 0.852 0.5829 0.075 Uiso 1 1 calc R . . H2A H -0.2573 0.8083 0.5864 0.075 Uiso 1 1 calc R . . C3 C -0.4853(3) 0.83883(15) 0.73579(19) 0.0564(8) Uani 1 1 d . . . H3C H -0.5254 0.8153 0.7723 0.085 Uiso 1 1 calc R . . H3B H -0.5571 0.8548 0.698 0.085 Uiso 1 1 calc R . . H3A H -0.433 0.8723 0.761 0.085 Uiso 1 1 calc R . . C4 C -0.4877(3) 0.72997(14) 0.64247(17) 0.0446(7) Uani 1 1 d . . . H4C H -0.4382 0.7034 0.6132 0.067 Uiso 1 1 calc R . . H4B H -0.5619 0.7495 0.6095 0.067 Uiso 1 1 calc R . . H4A H -0.5245 0.7062 0.6801 0.067 Uiso 1 1 calc R . . C5 C -0.1580(3) 0.87315(13) 0.85326(17) 0.0484(7) Uani 1 1 d . . . H5C H -0.0765 0.8927 0.8795 0.073 Uiso 1 1 calc R . . H5B H -0.2177 0.8623 0.889 0.073 Uiso 1 1 calc R . . H5A H -0.2052 0.901 0.8161 0.073 Uiso 1 1 calc R . . C6 C 0.0926(4) 0.87155(16) 0.7584(2) 0.0663(10) Uani 1 1 d . . . H6C H 0.0503 0.9101 0.7676 0.099 Uiso 1 1 calc R . . H6B H 0.1371 0.8752 0.7143 0.099 Uiso 1 1 calc R . . H6A H 0.1596 0.8609 0.8016 0.099 Uiso 1 1 calc R . . C7 C 0.0534(5) 0.77902(17) 0.94034(19) 0.0759(12) Uani 1 1 d . . . H7C H 0.1234 0.8079 0.9319 0.114 Uiso 1 1 calc R . . H7B H 0.0957 0.7439 0.9671 0.114 Uiso 1 1 calc R . . H7A H -0.0085 0.7982 0.97 0.114 Uiso 1 1 calc R . . C8 C -0.1359(3) 0.58862(12) 0.80046(16) 0.0376(6) Uani 1 1 d . . . H8 H -0.173(3) 0.5668(15) 0.755(2) 0.059(10) Uiso 1 1 d . . . C9 C -0.4260(3) 0.62102(19) 0.8229(3) 0.0805(13) Uani 1 1 d . . . H9C H -0.4122 0.6631 0.8094 0.121 Uiso 1 1 calc R . . H9B H -0.4886 0.6194 0.8592 0.121 Uiso 1 1 calc R . . H9A H -0.4639 0.5983 0.7783 0.121 Uiso 1 1 calc R . . C10 C -0.1943(4) 0.62899(18) 0.9530(2) 0.0726(11) Uani 1 1 d . . . H10C H -0.1103 0.6103 0.9773 0.109 Uiso 1 1 calc R . . H10B H -0.2619 0.6276 0.9864 0.109 Uiso 1 1 calc R . . H10A H -0.1769 0.671 0.941 0.109 Uiso 1 1 calc R . . C11 C -0.3069(4) 0.50894(17) 0.8937(3) 0.0818(13) Uani 1 1 d . . . H11C H -0.3469 0.4861 0.8496 0.123 Uiso 1 1 calc R . . H11B H -0.3727 0.5122 0.9281 0.123 Uiso 1 1 calc R . . H11A H -0.226 0.488 0.9184 0.123 Uiso 1 1 calc R . . C12 C 0.0622(4) 0.48880(14) 0.8868(2) 0.0591(9) Uani 1 1 d . . . H12C H 0.0266 0.4544 0.856 0.089 Uiso 1 1 calc R . . H12B H 0.0175 0.4908 0.931 0.089 Uiso 1 1 calc R . . H12A H 0.1597 0.4839 0.9022 0.089 Uiso 1 1 calc R . . C13 C 0.2398(3) 0.61147(17) 0.92491(18) 0.0591(9) Uani 1 1 d . . . H13C H 0.2458 0.578 0.9604 0.089 Uiso 1 1 calc R . . H13B H 0.2627 0.6493 0.9519 0.089 Uiso 1 1 calc R . . H13A H 0.3031 0.6047 0.8898 0.089 Uiso 1 1 calc R . . C14 C 0.2103(3) 0.51059(16) 0.7472(2) 0.0603(9) Uani 1 1 d . . . H14C H 0.2884 0.5158 0.7865 0.09 Uiso 1 1 calc R . . H14B H 0.2381 0.5172 0.6986 0.09 Uiso 1 1 calc R . . H14A H 0.1746 0.4696 0.7495 0.09 Uiso 1 1 calc R . . C15 C -0.1615(2) 0.64205(11) 0.59516(14) 0.0325(5) Uani 1 1 d . . . H15 H -0.237(3) 0.6689(14) 0.5867(17) 0.047(8) Uiso 1 1 d . . . C16 C -0.3874(3) 0.55244(15) 0.6062(3) 0.0654(10) Uani 1 1 d . . . H16C H -0.3678 0.5541 0.6607 0.098 Uiso 1 1 calc R . . H16B H -0.4222 0.5124 0.5906 0.098 Uiso 1 1 calc R . . H16A H -0.4552 0.583 0.5881 0.098 Uiso 1 1 calc R . . C17 C -0.1046(3) 0.50577(13) 0.59823(18) 0.0485(7) Uani 1 1 d . . . H17C H -0.0219 0.5121 0.5767 0.073 Uiso 1 1 calc R . . H17B H -0.1443 0.4667 0.5819 0.073 Uiso 1 1 calc R . . H17A H -0.0827 0.5063 0.6526 0.073 Uiso 1 1 calc R . . C18 C -0.2752(4) 0.55506(15) 0.46272(19) 0.0609(9) Uani 1 1 d . . . H18C H -0.3451 0.584 0.4423 0.091 Uiso 1 1 calc R . . H18B H -0.3096 0.514 0.4533 0.091 Uiso 1 1 calc R . . H18A H -0.1951 0.5608 0.4388 0.091 Uiso 1 1 calc R . . C19 C -0.0268(3) 0.67526(16) 0.45003(16) 0.0537(8) Uani 1 1 d . . . H19C H 0.0572 0.6941 0.4403 0.08 Uiso 1 1 calc R . . H19B H -0.1042 0.6989 0.426 0.08 Uiso 1 1 calc R . . H19A H -0.0328 0.6342 0.43 0.08 Uiso 1 1 calc R . . C20 C 0.2334(3) 0.62840(15) 0.56453(19) 0.0530(8) Uani 1 1 d . . . H20C H 0.2204 0.6131 0.5134 0.079 Uiso 1 1 calc R . . H20B H 0.2931 0.6011 0.5968 0.079 Uiso 1 1 calc R . . H20A H 0.2743 0.6686 0.566 0.079 Uiso 1 1 calc R . . C21 C 0.0689(4) 0.78956(15) 0.5511(2) 0.0599(9) Uani 1 1 d . . . H21C H 0.1629 0.7765 0.5539 0.09 Uiso 1 1 calc R . . H21B H 0.0659 0.8273 0.5788 0.09 Uiso 1 1 calc R . . H21A H 0.0293 0.796 0.4989 0.09 Uiso 1 1 calc R . . C22 C 0.2066(3) 0.70766(18) 0.7527(2) 0.0523(8) Uani 1 1 d . . . H22B H 0.232(4) 0.7272(19) 0.801(3) 0.093(14) Uiso 1 1 d . . . H22C H 0.266(4) 0.671(2) 0.749(2) 0.089(13) Uiso 1 1 d . . . H22A H 0.235(4) 0.7324(17) 0.712(2) 0.073(11) Uiso 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 Li1 0.050(3) 0.035(2) 0.038(2) 0.0009(18) 0.007(2) 0.0018(19) Li2 0.041(2) 0.040(2) 0.030(2) -0.0019(17) 0.0065(18) -0.0015(18) Li3 0.039(2) 0.040(2) 0.035(2) -0.0009(18) 0.0061(18) 0.0045(18) Li4 0.038(2) 0.044(2) 0.037(2) 0.0034(19) 0.0037(19) 0.0042(19) Si1 0.0298(4) 0.0352(4) 0.0346(4) 0.0003(3) 0.0021(3) 0.0030(3) Si2 0.0346(4) 0.0303(4) 0.0297(4) -0.0041(3) 0.0018(3) -0.0004(3) Si3 0.0475(5) 0.0404(4) 0.0626(6) 0.0150(4) 0.0252(4) 0.0056(3) Si4 0.0406(4) 0.0362(4) 0.0351(4) 0.0038(3) 0.0055(3) 0.0088(3) Si5 0.0284(4) 0.0353(4) 0.0480(5) -0.0069(3) -0.0051(3) -0.0006(3) Si6 0.0330(4) 0.0416(4) 0.0280(4) -0.0029(3) 0.0055(3) -0.0020(3) O1 0.0397(10) 0.0334(9) 0.0397(11) -0.0025(8) 0.0035(8) -0.0099(7) O2 0.0452(11) 0.0388(10) 0.0290(9) -0.0052(7) -0.0050(8) 0.0032(8) O3 0.0403(10) 0.0490(11) 0.0350(10) -0.0016(8) -0.0009(8) 0.0076(8) O4 0.0401(10) 0.0428(10) 0.0399(11) 0.0000(8) 0.0066(8) 0.0152(8) O5 0.0277(9) 0.0531(11) 0.0377(10) -0.0041(8) 0.0082(8) 0.0020(8) O6 0.0470(11) 0.0386(10) 0.0354(10) 0.0024(8) 0.0136(8) -0.0095(8) O7 0.0291(9) 0.0408(10) 0.0354(10) -0.0014(7) 0.0041(7) 0.0003(7) C1 0.0307(13) 0.0296(12) 0.0334(14) -0.0004(10) 0.0061(11) -0.0022(10) C2 0.0493(17) 0.0509(17) 0.0474(18) 0.0127(14) 0.0002(14) -0.0002(13) C3 0.0485(18) 0.061(2) 0.058(2) -0.0062(15) 0.0015(15) 0.0214(15) C4 0.0294(14) 0.0550(17) 0.0470(17) -0.0036(13) -0.0013(12) -0.0012(12) C5 0.0571(18) 0.0383(15) 0.0484(18) -0.0125(13) 0.0043(14) 0.0029(13) C6 0.071(2) 0.058(2) 0.072(2) -0.0140(17) 0.0181(18) -0.0388(18) C7 0.111(3) 0.058(2) 0.044(2) -0.0102(16) -0.032(2) 0.009(2) C8 0.0365(14) 0.0374(14) 0.0397(15) 0.0047(12) 0.0090(12) 0.0011(11) C9 0.0414(19) 0.083(3) 0.124(4) 0.040(2) 0.034(2) 0.0086(17) C10 0.086(3) 0.074(2) 0.067(2) -0.0011(19) 0.042(2) 0.015(2) C11 0.085(3) 0.056(2) 0.114(4) 0.028(2) 0.046(3) -0.0005(19) C12 0.074(2) 0.0477(18) 0.055(2) 0.0150(15) 0.0101(17) 0.0167(16) C13 0.0449(17) 0.082(2) 0.0462(18) -0.0041(16) -0.0060(14) 0.0101(16) C14 0.0551(19) 0.068(2) 0.059(2) -0.0029(16) 0.0111(16) 0.0307(16) C15 0.0263(12) 0.0338(13) 0.0362(14) -0.0041(10) 0.0009(10) -0.0008(10) C16 0.0384(17) 0.0522(19) 0.107(3) -0.0109(19) 0.0151(18) -0.0136(14) C17 0.0464(16) 0.0374(15) 0.0576(19) -0.0068(13) -0.0043(14) 0.0030(12) C18 0.062(2) 0.0521(19) 0.058(2) -0.0156(15) -0.0231(16) 0.0039(15) C19 0.060(2) 0.071(2) 0.0317(15) -0.0037(14) 0.0109(14) -0.0015(16) C20 0.0339(15) 0.069(2) 0.058(2) -0.0150(16) 0.0148(14) -0.0044(14) C21 0.076(2) 0.0532(19) 0.056(2) 0.0055(15) 0.0270(18) -0.0187(16) C22 0.0339(15) 0.073(2) 0.050(2) -0.0020(17) 0.0069(14) -0.0049(15) #----------------------------------------------------------------------------# # 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 Li1 C8 2.250(5) . ? Li1 C15 2.261(5) . ? Li1 C1 2.263(5) . ? Li2 O7 1.871(5) . ? Li2 O6 1.952(5) . ? Li2 O1 1.982(5) . ? Li3 O7 1.876(5) . ? Li3 O2 1.946(5) . ? Li3 O3 1.970(5) . ? Li4 O7 1.877(5) . ? Li4 O4 1.958(5) . ? Li4 O5 1.976(5) . ? Si1 C1 1.826(3) . ? Si1 C2 1.866(3) . ? Si1 C4 1.877(3) . ? Si1 C3 1.887(3) . ? Si2 O1 1.6724(19) . ? Si2 O2 1.6777(19) . ? Si2 C1 1.785(3) . ? Si2 C5 1.863(3) . ? Si3 C8 1.832(3) . ? Si3 C10 1.881(4) . ? Si3 C9 1.882(4) . ? Si3 C11 1.891(4) . ? Si4 O3 1.675(2) . ? Si4 O4 1.676(2) . ? Si4 C8 1.784(3) . ? Si4 C12 1.861(3) . ? Si5 C15 1.831(3) . ? Si5 C17 1.876(3) . ? Si5 C16 1.877(3) . ? Si5 C18 1.895(3) . ? Si6 O5 1.6738(19) . ? Si6 O6 1.6832(19) . ? Si6 C15 1.783(3) . ? Si6 C19 1.870(3) . ? O1 C6 1.427(3) . ? O2 C7 1.414(4) . ? O3 C13 1.423(3) . ? O4 C14 1.433(3) . ? O5 C20 1.421(3) . ? O6 C21 1.428(3) . ? O7 C22 1.403(4) . ? 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 C8 Li1 C15 119.2(2) . . ? C8 Li1 C1 118.8(2) . . ? C15 Li1 C1 121.2(2) . . ? O7 Li2 O6 107.7(2) . . ? O7 Li2 O1 107.0(2) . . ? O6 Li2 O1 124.6(2) . . ? O7 Li3 O2 107.7(2) . . ? O7 Li3 O3 107.4(2) . . ? O2 Li3 O3 123.8(2) . . ? O7 Li4 O4 107.1(2) . . ? O7 Li4 O5 107.5(2) . . ? O4 Li4 O5 126.7(2) . . ? C1 Si1 C2 110.82(13) . . ? C1 Si1 C4 111.64(12) . . ? C2 Si1 C4 107.60(14) . . ? C1 Si1 C3 115.53(13) . . ? C2 Si1 C3 107.48(15) . . ? C4 Si1 C3 103.23(14) . . ? O1 Si2 O2 108.16(10) . . ? O1 Si2 C1 103.88(11) . . ? O2 Si2 C1 106.49(11) . . ? O1 Si2 C5 106.83(12) . . ? O2 Si2 C5 107.29(12) . . ? C1 Si2 C5 123.45(13) . . ? C8 Si3 C10 110.90(16) . . ? C8 Si3 C9 112.18(16) . . ? C10 Si3 C9 108.2(2) . . ? C8 Si3 C11 114.93(16) . . ? C10 Si3 C11 106.6(2) . . ? C9 Si3 C11 103.51(19) . . ? O3 Si4 O4 107.24(10) . . ? O3 Si4 C8 103.85(12) . . ? O4 Si4 C8 107.29(12) . . ? O3 Si4 C12 106.62(14) . . ? O4 Si4 C12 107.13(13) . . ? C8 Si4 C12 123.75(15) . . ? C15 Si5 C17 112.12(13) . . ? C15 Si5 C16 110.26(14) . . ? C17 Si5 C16 108.31(16) . . ? C15 Si5 C18 115.83(14) . . ? C17 Si5 C18 104.40(15) . . ? C16 Si5 C18 105.41(18) . . ? O5 Si6 O6 108.92(10) . . ? O5 Si6 C15 103.30(11) . . ? O6 Si6 C15 106.65(11) . . ? O5 Si6 C19 106.82(13) . . ? O6 Si6 C19 105.94(13) . . ? C15 Si6 C19 124.58(14) . . ? C6 O1 Si2 126.4(2) . . ? C6 O1 Li2 135.3(2) . . ? Si2 O1 Li2 94.36(15) . . ? C7 O2 Si2 127.43(19) . . ? C7 O2 Li3 122.3(2) . . ? Si2 O2 Li3 109.25(16) . . ? C13 O3 Si4 124.1(2) . . ? C13 O3 Li3 132.9(2) . . ? Si4 O3 Li3 95.27(16) . . ? C14 O4 Si4 126.91(19) . . ? C14 O4 Li4 123.4(2) . . ? Si4 O4 Li4 109.54(16) . . ? C20 O5 Si6 127.1(2) . . ? C20 O5 Li4 133.5(2) . . ? Si6 O5 Li4 96.45(15) . . ? C21 O6 Si6 125.64(19) . . ? C21 O6 Li2 120.0(2) . . ? Si6 O6 Li2 110.65(16) . . ? C22 O7 Li2 110.1(2) . . ? C22 O7 Li3 111.6(2) . . ? Li2 O7 Li3 107.2(2) . . ? C22 O7 Li4 110.2(2) . . ? Li2 O7 Li4 109.2(2) . . ? Li3 O7 Li4 108.4(2) . . ? Si2 C1 Si1 118.86(14) . . ? Si2 C1 Li1 125.89(18) . . ? Si1 C1 Li1 110.46(17) . . ? Si4 C8 Si3 118.03(15) . . ? Si4 C8 Li1 125.78(18) . . ? Si3 C8 Li1 110.84(17) . . ? Si6 C15 Si5 119.24(14) . . ? Si6 C15 Li1 123.58(17) . . ? Si5 C15 Li1 110.30(17) . . ? #===END data_(6)-oct2204 _database_code_depnum_ccdc_archive 'CCDC 275753' _audit_creation_date 2004-11-01T09:09:37-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C29 H79 Ce Li2 O9 Si8' _chemical_formula_sum 'C29 H79 Ce Li2 O9 Si8' _chemical_formula_weight 950.64 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6796(2) _cell_length_b 12.6308(3) _cell_length_c 22.7947(5) _cell_angle_alpha 74.111(1) _cell_angle_beta 80.214(1) _cell_angle_gamma 72.502(1) _cell_volume 2544.7(1) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 31233 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.241 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1002 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.121 _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 0.6178 _exptl_absorpt_correction_T_max 0.7731 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.502645E-1 _diffrn_orient_matrix_ub_12 -0.66288E-2 _diffrn_orient_matrix_ub_13 0.424464E-1 _diffrn_orient_matrix_ub_21 0.956475E-1 _diffrn_orient_matrix_ub_22 -0.397268E-1 _diffrn_orient_matrix_ub_23 0.172544E-1 _diffrn_orient_matrix_ub_31 0.129177E-1 _diffrn_orient_matrix_ub_32 0.753576E-1 _diffrn_orient_matrix_ub_33 0.5202E-3 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0753 _diffrn_reflns_av_unetI/netI 0.0673 _diffrn_reflns_number 33702 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 26.03 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 9968 _reflns_number_gt 7912 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _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 ; The H atoms on C1,C8, and C22 were located on a difference map and refined isotropically: other H atoms were in riding mode. There is resolved disorder of the atoms C(15),O(5),C(19) and C(20) around Si6. 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^)+(0.0487P)^2^+3.7099P] 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 9968 _refine_ls_number_parameters 471 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0691 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1136 _refine_ls_wR_factor_gt 0.1038 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.03 _refine_diff_density_min -1.091 _refine_diff_density_rms 0.099 #----------------------------------------------------------------------------# # 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' Ce Ce -0.2486 2.6331 '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' Li Li -0.0003 0.0001 '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 Ce Ce -0.18967(3) -0.23623(2) 0.211947(11) 0.02527(9) Uani 1 1 d . . . Li1 Li -0.1883(8) -0.0081(6) 0.2904(3) 0.0342(17) Uani 1 1 d . . . Li2 Li -0.2723(9) -0.1836(7) 0.3647(3) 0.0374(18) Uani 1 1 d . . . Si1 Si -0.40385(14) 0.06477(11) 0.10072(6) 0.0330(3) Uani 1 1 d . . . Si2 Si -0.11341(13) 0.01566(10) 0.15354(5) 0.0285(3) Uani 1 1 d . . . Si3 Si -0.14422(16) -0.53205(11) 0.35846(6) 0.0417(3) Uani 1 1 d . . . Si4 Si -0.41889(14) -0.33462(11) 0.32741(6) 0.0320(3) Uani 1 1 d . . . Si5 Si 0.15702(15) -0.46970(12) 0.14172(6) 0.0402(3) Uani 1 1 d . . . Si6 Si -0.16914(16) -0.38507(12) 0.11017(6) 0.0409(3) Uani 1 1 d . . . Si7 Si -0.24270(15) -0.01875(11) 0.41258(6) 0.0374(3) Uani 1 1 d . . . Si8 Si -0.48567(14) 0.16192(11) 0.33468(6) 0.0350(3) Uani 1 1 d . . . O1 O -0.0055(3) -0.1185(2) 0.15712(13) 0.0313(7) Uani 1 1 d . A . O2 O -0.0836(3) 0.0543(3) 0.21367(14) 0.0347(7) Uani 1 1 d . A . O3 O -0.4495(3) -0.2139(2) 0.27053(13) 0.0337(7) Uani 1 1 d . A . O4 O -0.3977(3) -0.2852(3) 0.38542(13) 0.0382(8) Uani 1 1 d . A . O6 O -0.3131(3) -0.2926(3) 0.13999(15) 0.0397(8) Uani 1 1 d . A . O7 O -0.1038(4) 0.0138(3) 0.36335(15) 0.0427(8) Uani 1 1 d . A . O8 O -0.2001(4) -0.1613(3) 0.43606(14) 0.0425(8) Uani 1 1 d . A . O9 O -0.1375(3) -0.1730(2) 0.29280(13) 0.0286(6) Uani 1 1 d . A . C1 C -0.2917(5) -0.0050(4) 0.1649(2) 0.0300(10) Uani 1 1 d . A . H1 H -0.330(5) 0.017(4) 0.193(2) 0.040(15) Uiso 1 1 d . . . C2 C -0.5942(5) 0.0502(5) 0.1196(2) 0.0437(12) Uani 1 1 d . A . H2C H -0.5919 -0.031 0.1313 0.066 Uiso 1 1 calc R . . H2B H -0.6489 0.0884 0.0837 0.066 Uiso 1 1 calc R . . H2A H -0.6416 0.0855 0.1537 0.066 Uiso 1 1 calc R . . C3 C -0.4297(6) 0.2244(5) 0.0749(3) 0.0595(16) Uani 1 1 d . A . H3C H -0.4785 0.26 0.1088 0.089 Uiso 1 1 calc R . . H3B H -0.4894 0.2556 0.0403 0.089 Uiso 1 1 calc R . . H3A H -0.3346 0.2404 0.0622 0.089 Uiso 1 1 calc R . . C4 C -0.3223(6) 0.0020(6) 0.0329(2) 0.0615(17) Uani 1 1 d . A . H4C H -0.2244 0.0125 0.0203 0.092 Uiso 1 1 calc R . . H4B H -0.3833 0.0405 -0.001 0.092 Uiso 1 1 calc R . . H4A H -0.3165 -0.0797 0.0441 0.092 Uiso 1 1 calc R . . C5 C -0.0436(5) 0.1069(4) 0.0824(2) 0.0428(12) Uani 1 1 d . A . H5C H -0.095 0.1873 0.0804 0.064 Uiso 1 1 calc R . . H5B H -0.06 0.0854 0.0465 0.064 Uiso 1 1 calc R . . H5A H 0.0609 0.0957 0.083 0.064 Uiso 1 1 calc R . . C6 C 0.1490(5) -0.1461(4) 0.1412(3) 0.0476(13) Uani 1 1 d . . . H6C H 0.1699 -0.1084 0.0982 0.071 Uiso 1 1 calc R A . H6B H 0.1878 -0.229 0.1469 0.071 Uiso 1 1 calc R . . H6A H 0.195 -0.1196 0.1675 0.071 Uiso 1 1 calc R . . C7 C 0.0190(6) 0.1156(5) 0.2134(3) 0.0513(14) Uani 1 1 d . . . H7C H 0.1171 0.0714 0.2018 0.077 Uiso 1 1 calc R A . H7B H 0.0149 0.1279 0.2543 0.077 Uiso 1 1 calc R . . H7A H -0.0048 0.1896 0.1838 0.077 Uiso 1 1 calc R . . C8 C -0.2495(5) -0.4178(4) 0.3014(2) 0.0342(11) Uani 1 1 d . A . H8 H -0.263(6) -0.445(5) 0.278(3) 0.058(19) Uiso 1 1 d . . . C9 C -0.0306(9) -0.4790(5) 0.3971(3) 0.085(2) Uani 1 1 d . A . H9C H 0.0382 -0.4456 0.3664 0.128 Uiso 1 1 calc R . . H9B H 0.0232 -0.5429 0.4273 0.128 Uiso 1 1 calc R . . H9A H -0.094 -0.4208 0.4179 0.128 Uiso 1 1 calc R . . C10 C -0.2583(7) -0.6065(5) 0.4230(3) 0.0689(18) Uani 1 1 d . A . H10C H -0.3244 -0.5506 0.4445 0.103 Uiso 1 1 calc R . . H10B H -0.1945 -0.6657 0.4516 0.103 Uiso 1 1 calc R . . H10A H -0.3152 -0.6416 0.4061 0.103 Uiso 1 1 calc R . . C11 C -0.0192(7) -0.6477(5) 0.3234(3) 0.0622(16) Uani 1 1 d . A . H11C H -0.0762 -0.681 0.3054 0.093 Uiso 1 1 calc R . . H11B H 0.0359 -0.7071 0.355 0.093 Uiso 1 1 calc R . . H11A H 0.0484 -0.6157 0.2913 0.093 Uiso 1 1 calc R . . C12 C -0.5889(6) -0.3816(5) 0.3458(3) 0.0533(14) Uani 1 1 d . A . H12C H -0.582 -0.4422 0.3836 0.08 Uiso 1 1 calc R . . H12B H -0.6024 -0.4108 0.3121 0.08 Uiso 1 1 calc R . . H12A H -0.6719 -0.3167 0.3513 0.08 Uiso 1 1 calc R . . C13 C -0.5758(5) -0.1200(4) 0.2739(2) 0.0445(12) Uani 1 1 d . . . H13C H -0.6635 -0.1456 0.2773 0.067 Uiso 1 1 calc R A . H13B H -0.5736 -0.0587 0.2368 0.067 Uiso 1 1 calc R . . H13A H -0.5766 -0.0916 0.3099 0.067 Uiso 1 1 calc R . . C14 C -0.4808(7) -0.2947(6) 0.4440(3) 0.0682(18) Uani 1 1 d . . . H14C H -0.5837 -0.2567 0.4385 0.102 Uiso 1 1 calc R A . H14B H -0.4461 -0.2582 0.4693 0.102 Uiso 1 1 calc R . . H14A H -0.4694 -0.3755 0.4643 0.102 Uiso 1 1 calc R . . C16 C 0.2573(7) -0.4762(5) 0.2075(3) 0.0586(15) Uani 1 1 d . A . H16C H 0.2069 -0.5082 0.2463 0.088 Uiso 1 1 calc R . . H16B H 0.26 -0.399 0.207 0.088 Uiso 1 1 calc R . . H16A H 0.3569 -0.5248 0.2032 0.088 Uiso 1 1 calc R . . C17 C 0.2714(8) -0.4242(6) 0.0699(3) 0.0752(19) Uani 1 1 d . A . H17C H 0.3705 -0.4748 0.0718 0.113 Uiso 1 1 calc R . . H17B H 0.274 -0.3454 0.0655 0.113 Uiso 1 1 calc R . . H17A H 0.2296 -0.4285 0.0346 0.113 Uiso 1 1 calc R . . C18 C 0.1580(7) -0.6194(5) 0.1462(3) 0.0658(17) Uani 1 1 d . A . H18C H 0.1173 -0.6217 0.1101 0.099 Uiso 1 1 calc R . . H18B H 0.099 -0.647 0.1834 0.099 Uiso 1 1 calc R . . H18A H 0.2581 -0.6681 0.1473 0.099 Uiso 1 1 calc R . . C21 C -0.4586(6) -0.2820(5) 0.1310(3) 0.0706(19) Uani 1 1 d . . . H21C H -0.4706 -0.2577 0.0871 0.106 Uiso 1 1 calc R A . H21B H -0.5252 -0.2251 0.1518 0.106 Uiso 1 1 calc R . . H21A H -0.4806 -0.356 0.148 0.106 Uiso 1 1 calc R . . C22 C -0.3835(5) 0.0138(4) 0.3647(2) 0.0323(10) Uani 1 1 d . A . H22 H -0.452(5) -0.031(4) 0.3833(19) 0.028(12) Uiso 1 1 d . . . C23 C -0.6268(6) 0.1710(5) 0.2852(3) 0.0603(16) Uani 1 1 d . A . H23C H -0.5796 0.1369 0.2506 0.09 Uiso 1 1 calc R . . H23B H -0.6782 0.2513 0.2697 0.09 Uiso 1 1 calc R . . H23A H -0.6964 0.1295 0.3093 0.09 Uiso 1 1 calc R . . C24 C -0.3647(6) 0.2504(5) 0.2867(3) 0.0644(17) Uani 1 1 d . A . H24C H -0.2916 0.2509 0.3114 0.097 Uiso 1 1 calc R . . H24B H -0.4232 0.3287 0.2717 0.097 Uiso 1 1 calc R . . H24A H -0.316 0.2178 0.2518 0.097 Uiso 1 1 calc R . . C25 C -0.5893(7) 0.2397(5) 0.3950(3) 0.0713(19) Uani 1 1 d . A . H25C H -0.6608 0.2003 0.4192 0.107 Uiso 1 1 calc R . . H25B H -0.6396 0.3181 0.3753 0.107 Uiso 1 1 calc R . . H25A H -0.5214 0.2414 0.4219 0.107 Uiso 1 1 calc R . . C26 C -0.2539(7) 0.0406(5) 0.4803(2) 0.0624(17) Uani 1 1 d . A . H26C H -0.3292 0.0172 0.5113 0.094 Uiso 1 1 calc R . . H26B H -0.2785 0.1242 0.4675 0.094 Uiso 1 1 calc R . . H26A H -0.1598 0.0117 0.4976 0.094 Uiso 1 1 calc R . . C27 C 0.0312(7) 0.0136(6) 0.3793(3) 0.0690(18) Uani 1 1 d . . . H27C H 0.0149 0.068 0.4049 0.104 Uiso 1 1 calc R A . H27B H 0.0933 0.0359 0.342 0.104 Uiso 1 1 calc R . . H27A H 0.0791 -0.0632 0.4021 0.104 Uiso 1 1 calc R . . C28 C -0.0963(7) -0.2317(5) 0.4790(3) 0.0595(16) Uani 1 1 d . . . H28C H 0.0002 -0.2204 0.4631 0.089 Uiso 1 1 calc R A . H28B H -0.0928 -0.3122 0.4846 0.089 Uiso 1 1 calc R . . H28A H -0.1257 -0.2104 0.5184 0.089 Uiso 1 1 calc R . . C29 C 0.0128(5) -0.2182(4) 0.2994(2) 0.0415(12) Uani 1 1 d . . . H29C H 0.0416 -0.1791 0.3251 0.062 Uiso 1 1 calc R A . H29B H 0.0679 -0.2068 0.259 0.062 Uiso 1 1 calc R . . H29A H 0.0332 -0.3001 0.3188 0.062 Uiso 1 1 calc R . . O5 O -0.2010(7) -0.5106(6) 0.1454(4) 0.054(2) Uani 0.604(13) 1 d P A 1 C15 C -0.0247(9) -0.3569(10) 0.1352(5) 0.034(2) Uani 0.604(13) 1 d P A 1 H15 H -0.0008 -0.2958 0.0999 0.041 Uiso 0.604(13) 1 calc PR A 1 C19 C -0.1947(12) -0.3573(10) 0.0302(5) 0.060(3) Uani 0.604(13) 1 d P A 1 H19A H -0.1762 -0.2836 0.0084 0.09 Uiso 0.604(13) 1 calc PR A 1 H19B H -0.2948 -0.3551 0.0263 0.09 Uiso 0.604(13) 1 calc PR A 1 H19C H -0.1268 -0.418 0.0124 0.09 Uiso 0.604(13) 1 calc PR A 1 C20 C -0.2463(15) -0.5807(10) 0.1230(7) 0.080(4) Uani 0.604(13) 1 d P A 1 H20A H -0.255 -0.6481 0.1556 0.119 Uiso 0.604(13) 1 calc PR A 1 H20B H -0.1758 -0.6045 0.0897 0.119 Uiso 0.604(13) 1 calc PR A 1 H20C H -0.3413 -0.5406 0.1074 0.119 Uiso 0.604(13) 1 calc PR A 1 O5A O -0.2131(12) -0.4945(10) 0.1016(7) 0.067(4) Uiso 0.396(13) 1 d P A 2 C15A C -0.0252(17) -0.4026(16) 0.1575(8) 0.040(4) Uiso 0.396(13) 1 d P A 2 H15A H -0.0477 -0.4678 0.1903 0.049 Uiso 0.396(13) 1 calc PR A 2 C19A C -0.126(2) -0.3163(14) 0.0219(7) 0.059(5) Uiso 0.396(13) 1 d P A 2 H19D H -0.0967 -0.2467 0.0176 0.088 Uiso 0.396(13) 1 calc PR A 2 H19E H -0.2138 -0.2972 0.0006 0.088 Uiso 0.396(13) 1 calc PR A 2 H19F H -0.0476 -0.371 0.0038 0.088 Uiso 0.396(13) 1 calc PR A 2 C20A C -0.258(3) -0.569(2) 0.1568(11) 0.088(8) Uiso 0.396(13) 1 d P A 2 H20D H -0.2814 -0.6317 0.1463 0.132 Uiso 0.396(13) 1 calc PR A 2 H20E H -0.344 -0.5262 0.1781 0.132 Uiso 0.396(13) 1 calc PR A 2 H20F H -0.1787 -0.6009 0.1836 0.132 Uiso 0.396(13) 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 Ce 0.02297(13) 0.02687(14) 0.02580(14) -0.00828(10) -0.00128(9) -0.00518(9) Li1 0.034(4) 0.031(4) 0.038(4) -0.008(3) -0.009(3) -0.006(3) Li2 0.040(5) 0.040(4) 0.034(4) -0.008(3) -0.006(3) -0.013(4) Si1 0.0282(7) 0.0387(7) 0.0292(7) -0.0025(5) -0.0049(5) -0.0083(5) Si2 0.0235(6) 0.0313(6) 0.0286(6) -0.0058(5) 0.0006(5) -0.0073(5) Si3 0.0482(9) 0.0273(7) 0.0429(8) -0.0015(6) -0.0056(6) -0.0058(6) Si4 0.0342(7) 0.0319(7) 0.0301(7) -0.0062(5) 0.0005(5) -0.0121(5) Si5 0.0359(8) 0.0412(8) 0.0430(8) -0.0144(6) 0.0010(6) -0.0082(6) Si6 0.0449(8) 0.0395(8) 0.0424(8) -0.0167(6) -0.0075(6) -0.0093(6) Si7 0.0463(8) 0.0357(7) 0.0310(7) -0.0123(6) -0.0134(6) -0.0029(6) Si8 0.0322(7) 0.0322(7) 0.0364(7) -0.0110(6) -0.0026(5) -0.0002(5) O1 0.0202(15) 0.0330(17) 0.0388(17) -0.0119(14) 0.0027(13) -0.0042(13) O2 0.0329(18) 0.0359(17) 0.0390(18) -0.0089(14) -0.0027(14) -0.0151(14) O3 0.0297(17) 0.0315(17) 0.0325(17) -0.0058(13) 0.0009(13) -0.0011(13) O4 0.045(2) 0.0406(18) 0.0291(17) -0.0100(14) 0.0076(14) -0.0156(15) O6 0.0306(18) 0.0452(19) 0.047(2) -0.0164(16) -0.0096(15) -0.0076(15) O7 0.0394(19) 0.048(2) 0.047(2) -0.0140(16) -0.0163(16) -0.0106(16) O8 0.056(2) 0.0371(18) 0.0321(17) -0.0051(14) -0.0184(16) -0.0041(16) O9 0.0243(16) 0.0317(16) 0.0301(16) -0.0082(13) -0.0049(12) -0.0058(13) C1 0.025(2) 0.035(3) 0.028(2) -0.010(2) 0.0020(19) -0.0062(19) C2 0.032(3) 0.058(3) 0.040(3) -0.009(2) -0.010(2) -0.010(2) C3 0.041(3) 0.047(3) 0.076(4) 0.014(3) -0.017(3) -0.011(3) C4 0.052(4) 0.103(5) 0.038(3) -0.026(3) 0.004(3) -0.029(3) C5 0.037(3) 0.044(3) 0.043(3) -0.001(2) 0.005(2) -0.016(2) C6 0.027(3) 0.040(3) 0.070(4) -0.016(3) 0.012(2) -0.007(2) C7 0.045(3) 0.062(4) 0.061(3) -0.024(3) 0.003(3) -0.030(3) C8 0.045(3) 0.028(2) 0.030(3) -0.007(2) -0.007(2) -0.009(2) C9 0.133(7) 0.043(3) 0.082(5) 0.019(3) -0.070(5) -0.026(4) C10 0.073(4) 0.052(4) 0.055(4) 0.017(3) 0.001(3) -0.008(3) C11 0.055(4) 0.038(3) 0.077(4) -0.006(3) -0.002(3) 0.001(3) C12 0.048(3) 0.059(4) 0.056(3) -0.005(3) 0.000(3) -0.029(3) C13 0.031(3) 0.044(3) 0.047(3) -0.008(2) 0.002(2) 0.003(2) C14 0.082(5) 0.085(5) 0.047(3) -0.032(3) 0.028(3) -0.040(4) C16 0.059(4) 0.051(3) 0.066(4) -0.002(3) -0.022(3) -0.018(3) C17 0.079(5) 0.074(5) 0.070(4) -0.018(4) 0.016(4) -0.027(4) C18 0.078(5) 0.052(4) 0.071(4) -0.013(3) -0.016(3) -0.019(3) C21 0.036(3) 0.063(4) 0.126(6) -0.038(4) -0.030(3) -0.006(3) C22 0.036(3) 0.031(2) 0.028(2) -0.0073(19) -0.004(2) -0.006(2) C23 0.049(3) 0.042(3) 0.085(4) -0.020(3) -0.029(3) 0.012(3) C24 0.051(3) 0.038(3) 0.088(5) -0.003(3) -0.001(3) -0.002(3) C25 0.081(5) 0.056(4) 0.064(4) -0.026(3) 0.005(3) 0.006(3) C26 0.087(5) 0.057(4) 0.046(3) -0.022(3) -0.024(3) -0.005(3) C27 0.056(4) 0.083(5) 0.081(4) -0.013(4) -0.030(3) -0.030(3) C28 0.071(4) 0.051(3) 0.049(3) -0.008(3) -0.032(3) 0.005(3) C29 0.035(3) 0.043(3) 0.040(3) -0.003(2) -0.011(2) -0.003(2) O5 0.055(4) 0.058(4) 0.052(5) -0.018(3) -0.003(3) -0.017(3) C15 0.031(4) 0.036(5) 0.032(5) -0.008(4) -0.007(4) -0.003(4) C19 0.048(6) 0.072(7) 0.074(7) -0.035(6) -0.006(5) -0.019(5) C20 0.097(10) 0.055(7) 0.100(11) -0.016(7) -0.008(8) -0.042(7) #----------------------------------------------------------------------------# # 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 Ce O9 2.378(3) . ? Ce O6 2.538(3) . ? Ce O1 2.602(3) . ? Ce O3 2.612(3) . ? Ce C15 2.641(8) . ? Ce C15A 2.690(15) . ? Ce C1 2.750(5) . ? Ce C8 2.755(5) . ? Li1 O2 1.957(8) . ? Li1 O9 1.979(8) . ? Li1 O7 2.088(8) . ? Li1 C22 2.318(9) . ? Li2 O9 1.914(8) . ? Li2 O4 1.937(9) . ? Li2 O8 1.993(8) . ? Li2 C22 2.400(9) . ? Si1 C1 1.832(5) . ? Si1 C2 1.873(5) . ? Si1 C4 1.875(5) . ? Si1 C3 1.890(5) . ? Si2 O2 1.669(3) . ? Si2 O1 1.691(3) . ? Si2 C1 1.788(5) . ? Si2 C5 1.867(5) . ? Si3 C8 1.831(5) . ? Si3 C11 1.867(6) . ? Si3 C9 1.879(6) . ? Si3 C10 1.892(6) . ? Si4 O4 1.674(3) . ? Si4 O3 1.694(3) . ? Si4 C8 1.766(5) . ? Si4 C12 1.858(5) . ? Si5 C15A 1.735(15) . ? Si5 C18 1.862(6) . ? Si5 C17 1.868(6) . ? Si5 C16 1.891(6) . ? Si6 O5A 1.630(12) . ? Si6 O5 1.663(8) . ? Si6 O6 1.703(3) . ? Si6 C15 1.758(8) . ? Si7 O8 1.673(3) . ? Si7 O7 1.674(4) . ? Si7 C22 1.772(5) . ? Si7 C26 1.867(5) . ? Si8 C22 1.834(5) . ? Si8 C24 1.870(6) . ? Si8 C23 1.874(5) . ? Si8 C25 1.882(6) . ? O1 C6 1.436(5) . ? O2 C7 1.429(5) . ? O3 C13 1.433(5) . ? O4 C14 1.432(6) . ? O6 C21 1.419(6) . ? O7 C27 1.414(6) . ? O8 C28 1.442(6) . ? O9 C29 1.412(5) . ? O5 C20 1.339(16) . ? O5A C20A 1.44(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 O9 Ce O6 164.76(10) . . ? O9 Ce O1 77.25(9) . . ? O6 Ce O1 114.33(10) . . ? O9 Ce O3 84.31(9) . . ? O6 Ce O3 80.51(10) . . ? O1 Ce O3 141.51(9) . . ? O9 Ce C15 132.99(18) . . ? O6 Ce C15 61.61(18) . . ? O1 Ce C15 76.5(3) . . ? O3 Ce C15 137.3(2) . . ? O9 Ce C15A 129.1(3) . . ? O6 Ce C15A 63.6(3) . . ? O1 Ce C15A 87.1(4) . . ? O3 Ce C15A 129.8(4) . . ? O9 Ce C1 82.08(12) . . ? O6 Ce C1 94.84(12) . . ? O1 Ce C1 60.77(11) . . ? O3 Ce C1 83.59(11) . . ? C15 Ce C1 116.5(3) . . ? C15A Ce C1 130.6(4) . . ? O9 Ce C8 86.23(13) . . ? O6 Ce C8 87.49(13) . . ? O1 Ce C8 148.67(12) . . ? O3 Ce C8 60.58(12) . . ? C15 Ce C8 96.8(3) . . ? C15A Ce C8 82.9(4) . . ? C1 Ce C8 143.26(14) . . ? O2 Li1 O9 103.2(4) . . ? O2 Li1 O7 108.8(4) . . ? O9 Li1 O7 109.1(4) . . ? O2 Li1 C22 150.2(4) . . ? O9 Li1 C22 102.9(4) . . ? O7 Li1 C22 75.5(3) . . ? O9 Li2 O4 123.5(4) . . ? O9 Li2 O8 112.8(4) . . ? O4 Li2 O8 114.9(4) . . ? O9 Li2 C22 102.0(4) . . ? O4 Li2 C22 117.6(4) . . ? O8 Li2 C22 75.5(3) . . ? C1 Si1 C2 112.9(2) . . ? C1 Si1 C4 110.6(3) . . ? C2 Si1 C4 107.5(2) . . ? C1 Si1 C3 114.0(2) . . ? C2 Si1 C3 103.6(2) . . ? C4 Si1 C3 107.8(3) . . ? O2 Si2 O1 106.15(16) . . ? O2 Si2 C1 109.6(2) . . ? O1 Si2 C1 102.33(19) . . ? O2 Si2 C5 108.2(2) . . ? O1 Si2 C5 105.85(19) . . ? C1 Si2 C5 123.4(2) . . ? C8 Si3 C11 111.5(3) . . ? C8 Si3 C9 112.4(2) . . ? C11 Si3 C9 107.6(3) . . ? C8 Si3 C10 114.4(3) . . ? C11 Si3 C10 105.2(3) . . ? C9 Si3 C10 105.2(3) . . ? O4 Si4 O3 101.52(16) . . ? O4 Si4 C8 109.6(2) . . ? O3 Si4 C8 103.11(19) . . ? O4 Si4 C12 108.8(2) . . ? O3 Si4 C12 107.3(2) . . ? C8 Si4 C12 124.1(3) . . ? C15A Si5 C18 103.8(6) . . ? C15A Si5 C17 124.6(7) . . ? C18 Si5 C17 106.5(3) . . ? C15A Si5 C16 107.7(6) . . ? C18 Si5 C16 106.4(3) . . ? C17 Si5 C16 106.5(3) . . ? O5A Si6 O6 112.1(4) . . ? O5 Si6 O6 101.9(3) . . ? O5A Si6 C15 138.5(5) . . ? O5 Si6 C15 115.2(4) . . ? O6 Si6 C15 100.1(3) . . ? O8 Si7 O7 106.74(18) . . ? O8 Si7 C22 103.6(2) . . ? O7 Si7 C22 103.3(2) . . ? O8 Si7 C26 108.1(2) . . ? O7 Si7 C26 107.9(3) . . ? C22 Si7 C26 125.8(3) . . ? C22 Si8 C24 112.0(2) . . ? C22 Si8 C23 112.0(2) . . ? C24 Si8 C23 106.7(3) . . ? C22 Si8 C25 114.6(2) . . ? C24 Si8 C25 106.3(3) . . ? C23 Si8 C25 104.7(3) . . ? C6 O1 Si2 124.3(3) . . ? C6 O1 Ce 134.7(3) . . ? Si2 O1 Ce 100.29(12) . . ? C7 O2 Si2 125.6(3) . . ? C7 O2 Li1 120.8(4) . . ? Si2 O2 Li1 113.3(3) . . ? C13 O3 Si4 121.8(3) . . ? C13 O3 Ce 134.9(3) . . ? Si4 O3 Ce 100.30(13) . . ? C14 O4 Si4 126.3(3) . . ? C14 O4 Li2 117.8(4) . . ? Si4 O4 Li2 115.0(3) . . ? C21 O6 Si6 121.8(3) . . ? C21 O6 Ce 136.0(3) . . ? Si6 O6 Ce 100.80(14) . . ? C27 O7 Si7 125.8(4) . . ? C27 O7 Li1 139.0(4) . . ? Si7 O7 Li1 91.9(3) . . ? C28 O8 Si7 126.4(3) . . ? C28 O8 Li2 134.6(4) . . ? Si7 O8 Li2 94.7(3) . . ? C29 O9 Li2 118.7(3) . . ? C29 O9 Li1 107.7(3) . . ? Li2 O9 Li1 85.6(3) . . ? C29 O9 Ce 107.9(3) . . ? Li2 O9 Ce 115.3(3) . . ? Li1 O9 Ce 120.6(2) . . ? Si2 C1 Si1 116.1(3) . . ? Si2 C1 Ce 92.55(18) . . ? Si1 C1 Ce 126.8(2) . . ? Si4 C8 Si3 117.7(3) . . ? Si4 C8 Ce 93.36(19) . . ? Si3 C8 Ce 134.3(3) . . ? Si7 C22 Si8 121.2(3) . . ? Si7 C22 Li1 82.2(3) . . ? Si8 C22 Li1 101.3(3) . . ? Si7 C22 Li2 79.3(2) . . ? Si8 C22 Li2 156.6(3) . . ? Li1 C22 Li2 68.2(3) . . ? C20 O5 Si6 129.4(9) . . ? Si6 C15 Si5 119.1(5) . . ? Si6 C15 Ce 95.5(3) . . ? Si5 C15 Ce 132.1(4) . . ? C20A O5A Si6 116.4(16) . . ? Si5 C15A Si6 124.4(9) . . ? Si5 C15A Ce 139.4(8) . . ? Si6 C15A Ce 92.2(6) . . ? #===END data_(11)-nov803 _database_code_depnum_ccdc_archive 'CCDC 275754' _audit_creation_date 2003-11-11T11:03:39-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety '(C34 H74 Ce2 F6 O16 S2 Si4), 3(C4 H8 O1)' _chemical_formula_sum 'C46 H98 Ce2 F6 O19 S2 Si4' _chemical_formula_weight 1525.96 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6698(10) _cell_length_b 12.9987(2) _cell_length_c 13.1909(2) _cell_angle_alpha 86.761(1) _cell_angle_beta 80.802(1) _cell_angle_gamma 70.229(1) _cell_volume 1699.51(4) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 29513 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.531 _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 0.5107 _exptl_absorpt_correction_T_max 0.5513 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _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_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.978599E-1 _diffrn_orient_matrix_ub_12 0.351876E-1 _diffrn_orient_matrix_ub_13 -0.51256E-2 _diffrn_orient_matrix_ub_21 -0.233674E-1 _diffrn_orient_matrix_ub_22 -0.422816E-1 _diffrn_orient_matrix_ub_23 0.614999E-1 _diffrn_orient_matrix_ub_31 -0.48836E-2 _diffrn_orient_matrix_ub_32 0.604744E-1 _diffrn_orient_matrix_ub_33 0.457095E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_unetI/netI 0.0245 _diffrn_reflns_number 31410 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.77 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 0.986 _reflns_number_total 7672 _reflns_number_gt 7297 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _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 ; There are two disordered thf solvate molecules one in a general position and one on an inversion centre; both were included with all atoms as isotropic carbon and with hydrogens omitted. 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^)+(0.0344P)^2^+1.9619P] 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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 7672 _refine_ls_number_parameters 348 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0286 _refine_ls_R_factor_gt 0.0266 _refine_ls_wR_factor_ref 0.0713 _refine_ls_wR_factor_gt 0.0698 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.725 _refine_diff_density_min -0.664 _refine_diff_density_rms 0.077 #----------------------------------------------------------------------------# # 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' Ce Ce -0.2486 2.6331 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 Ce Ce 0.478080(12) 0.880866(9) 0.590215(9) 0.02099(5) Uani 1 1 d . . . S S 0.31442(6) 1.17230(5) 0.67348(5) 0.02853(12) Uani 1 1 d . . . Si1 Si 0.27429(7) 0.73020(6) 0.61135(6) 0.02861(14) Uani 1 1 d . B . Si2 Si 0.15200(8) 0.87991(6) 0.80644(6) 0.03398(16) Uani 1 1 d . B . F11 F 0.08323(19) 1.22135(16) 0.79390(15) 0.0540(5) Uani 1 1 d . . . F12 F 0.06756(18) 1.22284(17) 0.63343(17) 0.0544(5) Uani 1 1 d . . . F13 F 0.1108(2) 1.35339(14) 0.69734(18) 0.0610(6) Uani 1 1 d . . . O1 O 0.38731(18) 0.74797(14) 0.51305(13) 0.0304(4) Uani 1 1 d . . . O2 O 0.3241(2) 0.59497(16) 0.61940(17) 0.0417(5) Uani 1 1 d . . . O3 O 0.32267(18) 1.05831(13) 0.68018(14) 0.0299(4) Uani 1 1 d . . . O4 O 0.3683(2) 1.20880(18) 0.75143(16) 0.0439(5) Uani 1 1 d . . . O5 O 0.34953(18) 1.20798(14) 0.56999(14) 0.0323(4) Uani 1 1 d . . . O6 O 0.39603(16) 0.99548(13) 0.45283(13) 0.0253(3) Uani 1 1 d . . . O7 O 0.5680(2) 0.88051(16) 0.76366(14) 0.0384(4) Uani 1 1 d . . . O8 O 0.65475(18) 0.69332(14) 0.62594(15) 0.0335(4) Uani 1 1 d . . . C1 C 0.2963(2) 0.8049(2) 0.71283(19) 0.0276(5) Uani 1 1 d . . . H1 H 0.3533 0.7469 0.755 0.033 Uiso 1 1 calc R B . C2 C 0.1073(3) 0.7760(3) 0.5661(3) 0.0467(7) Uani 1 1 d . . . H2A H 0.0744 0.8559 0.5604 0.07 Uiso 1 1 calc R B . H2B H 0.0432 0.7524 0.6153 0.07 Uiso 1 1 calc R . . H2C H 0.1164 0.7438 0.4988 0.07 Uiso 1 1 calc R . . C3 C 0.4095(4) 0.6965(3) 0.4146(2) 0.0520(8) Uani 1 1 d . . . H3A H 0.4788 0.717 0.3683 0.078 Uiso 1 1 calc R . . H3B H 0.3254 0.7206 0.3852 0.078 Uiso 1 1 calc R . . H3C H 0.4394 0.6169 0.4234 0.078 Uiso 1 1 calc R . . C4 C 0.2606(4) 0.5419(3) 0.6952(3) 0.0631(10) Uani 1 1 d . . . H4A H 0.3038 0.4626 0.6876 0.095 Uiso 1 1 calc R . . H4B H 0.1653 0.5621 0.688 0.095 Uiso 1 1 calc R . . H4C H 0.2683 0.5638 0.7632 0.095 Uiso 1 1 calc R . . C5 C 0.0660(4) 0.7884(3) 0.8832(3) 0.0562(9) Uani 1 1 d . . . H5A H -0.0101 0.8328 0.9317 0.084 Uiso 1 1 calc R B . H5B H 0.1304 0.7343 0.9212 0.084 Uiso 1 1 calc R . . H5C H 0.0332 0.7507 0.8365 0.084 Uiso 1 1 calc R . . C6 C 0.0164(3) 0.9860(3) 0.7453(3) 0.0470(7) Uani 1 1 d . . . H6A H -0.0579 1.0236 0.7986 0.071 Uiso 1 1 calc R B . H6B H -0.017 0.9505 0.6971 0.071 Uiso 1 1 calc R . . H6C H 0.0535 1.0393 0.7082 0.071 Uiso 1 1 calc R . . C7 C 0.2012(4) 0.9528(3) 0.9040(2) 0.0480(7) Uani 1 1 d . . . H7A H 0.1211 0.9918 0.9521 0.072 Uiso 1 1 calc R B . H7B H 0.2416 1.0051 0.8691 0.072 Uiso 1 1 calc R . . H7C H 0.2666 0.8994 0.9417 0.072 Uiso 1 1 calc R . . C8 C 0.1335(3) 1.2460(2) 0.7010(2) 0.0400(6) Uani 1 1 d . . . C9 C 0.2586(3) 1.0117(2) 0.4518(3) 0.0408(6) Uani 1 1 d . . . H9A H 0.2279 1.0594 0.3941 0.061 Uiso 1 1 calc R . . H9B H 0.2057 1.046 0.5164 0.061 Uiso 1 1 calc R . . H9C H 0.2469 0.9411 0.4443 0.061 Uiso 1 1 calc R . . C10 C 0.5760(4) 0.8012(3) 0.8470(2) 0.0503(8) Uani 1 1 d . . . H10A H 0.6186 0.7258 0.8201 0.06 Uiso 1 1 calc R . . H10B H 0.485 0.8089 0.8841 0.06 Uiso 1 1 calc R . . C11 C 0.6598(6) 0.8257(5) 0.9164(4) 0.0943(18) Uani 1 1 d . . . H11A H 0.6152 0.8303 0.9886 0.113 Uiso 1 1 calc R . . H11B H 0.7494 0.7681 0.9111 0.113 Uiso 1 1 calc R . . C12 C 0.6728(7) 0.9325(5) 0.8810(4) 0.103(2) Uani 1 1 d . . . H12A H 0.6457 0.9841 0.9392 0.124 Uiso 1 1 calc R . . H12B H 0.7672 0.9231 0.8512 0.124 Uiso 1 1 calc R . . C13 C 0.5866(6) 0.9727(3) 0.8055(3) 0.0738(13) Uani 1 1 d . . . H13A H 0.6279 1.0117 0.7507 0.089 Uiso 1 1 calc R . . H13B H 0.4989 1.0243 0.8369 0.089 Uiso 1 1 calc R . . C14 C 0.6575(4) 0.5873(2) 0.5949(4) 0.0654(11) Uani 1 1 d . B . H14A H 0.6371 0.591 0.5239 0.079 Uiso 1 1 calc R A 1 H14B H 0.5892 0.564 0.6411 0.079 Uiso 1 1 calc R A 1 C18 C 0.5491(13) 0.4556(10) 0.8505(9) 0.182(4) Uiso 1 1 d . . . C19 C 0.5050(12) 0.3641(10) 0.8951(9) 0.170(4) Uiso 1 1 d . . . C20 C 0.6252(11) 0.2519(9) 0.8718(9) 0.085(3) Uiso 0.530(11) 1 d P . . C21 C 0.7402(12) 0.2758(10) 0.8388(9) 0.098(4) Uiso 0.530(11) 1 d P . . C22 C 0.7092(12) 0.3789(10) 0.8012(10) 0.095(3) Uiso 0.530(11) 1 d P . . C23 C 0.1680(11) 1.4320(9) 1.0406(8) 0.085(3) Uiso 0.5 1 d P . . C24 C 0.1210(15) 1.4146(12) 0.9541(10) 0.105(4) Uiso 0.5 1 d P . . C25 C 0.0303(13) 1.4685(10) 0.9439(8) 0.171(4) Uiso 1 1 d . . . C26 C -0.0531(15) 1.5017(11) 0.9011(11) 0.104(4) Uiso 0.5 1 d P . . C20A C 0.604(2) 0.302(2) 0.9220(19) 0.156(8) Uiso 0.470(11) 1 d P . . C21A C 0.724(2) 0.3726(17) 0.8760(16) 0.138(6) Uiso 0.470(11) 1 d P . . C22A C 0.6446(12) 0.4623(9) 0.8675(8) 0.079(3) Uiso 0.470(11) 1 d P . . C15 C 0.7937(4) 0.5086(3) 0.6007(4) 0.0683(11) Uani 0.640(16) 1 d P B 1 H15A H 0.842 0.4841 0.5312 0.082 Uiso 0.640(16) 1 calc PR B 1 H15B H 0.7883 0.4439 0.6421 0.082 Uiso 0.640(16) 1 calc PR B 1 C16 C 0.8647(6) 0.5694(5) 0.6510(9) 0.054(2) Uani 0.640(16) 1 d P B 1 H16A H 0.9615 0.5469 0.6222 0.064 Uiso 0.640(16) 1 calc PR B 1 H16B H 0.8556 0.5569 0.7261 0.064 Uiso 0.640(16) 1 calc PR B 1 C17 C 0.7931(3) 0.6870(3) 0.6259(3) 0.0462(7) Uani 0.640(16) 1 d P B 1 H17A H 0.7985 0.7362 0.6784 0.055 Uiso 0.640(16) 1 calc PR B 1 H17B H 0.8325 0.7071 0.5578 0.055 Uiso 0.640(16) 1 calc PR B 1 C15A C 0.7937(4) 0.5086(3) 0.6007(4) 0.0683(11) Uani 0.360(16) 1 d P B 2 H15C H 0.8224 0.4535 0.5454 0.082 Uiso 0.360(16) 1 calc PR B 2 H15D H 0.7986 0.4711 0.6681 0.082 Uiso 0.360(16) 1 calc PR B 2 C16A C 0.8781(10) 0.5849(9) 0.5861(15) 0.056(4) Uani 0.360(16) 1 d P B 2 H16C H 0.9566 0.556 0.6233 0.067 Uiso 0.360(16) 1 calc PR B 2 H16D H 0.9113 0.5915 0.5124 0.067 Uiso 0.360(16) 1 calc PR B 2 C17A C 0.7931(3) 0.6870(3) 0.6259(3) 0.0462(7) Uani 0.360(16) 1 d P B 2 H17C H 0.8125 0.7464 0.5831 0.055 Uiso 0.360(16) 1 calc PR B 2 H17D H 0.8081 0.6951 0.6967 0.055 Uiso 0.360(16) 1 calc PR B 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 Ce 0.01963(7) 0.01818(7) 0.02611(7) -0.00023(4) -0.00483(5) -0.00687(5) S 0.0279(3) 0.0234(3) 0.0328(3) -0.0051(2) 0.0003(2) -0.0080(2) Si1 0.0244(3) 0.0272(3) 0.0377(4) -0.0043(3) -0.0029(3) -0.0132(3) Si2 0.0309(4) 0.0360(4) 0.0362(4) -0.0062(3) 0.0030(3) -0.0154(3) F11 0.0451(10) 0.0504(10) 0.0552(11) -0.0070(8) 0.0182(8) -0.0118(8) F12 0.0336(9) 0.0558(11) 0.0716(13) 0.0033(9) -0.0126(9) -0.0104(8) F13 0.0505(11) 0.0248(8) 0.0917(15) -0.0051(9) 0.0108(10) -0.0008(8) O1 0.0334(9) 0.0314(9) 0.0317(9) -0.0064(7) -0.0023(7) -0.0178(7) O2 0.0434(11) 0.0294(9) 0.0547(12) -0.0048(8) 0.0036(9) -0.0193(8) O3 0.0293(9) 0.0225(8) 0.0353(9) -0.0019(7) 0.0001(7) -0.0071(7) O4 0.0507(12) 0.0449(11) 0.0420(11) -0.0106(9) -0.0070(9) -0.0220(10) O5 0.0318(9) 0.0239(8) 0.0373(9) -0.0016(7) 0.0016(7) -0.0070(7) O6 0.0209(8) 0.0270(8) 0.0310(8) 0.0011(6) -0.0082(6) -0.0102(6) O7 0.0465(11) 0.0381(10) 0.0338(10) 0.0027(8) -0.0179(8) -0.0134(9) O8 0.0264(9) 0.0249(8) 0.0489(11) 0.0036(7) -0.0108(8) -0.0065(7) C1 0.0248(11) 0.0287(11) 0.0310(12) -0.0005(9) -0.0028(9) -0.0115(9) C2 0.0330(15) 0.0545(18) 0.0587(19) -0.0125(14) -0.0123(13) -0.0182(13) C3 0.064(2) 0.067(2) 0.0389(15) -0.0203(14) 0.0038(14) -0.0423(18) C4 0.064(2) 0.0383(17) 0.083(3) 0.0089(17) 0.009(2) -0.0219(16) C5 0.058(2) 0.056(2) 0.056(2) -0.0035(16) 0.0147(16) -0.0311(17) C6 0.0309(14) 0.0418(16) 0.065(2) -0.0097(14) -0.0020(13) -0.0081(12) C7 0.0539(19) 0.0553(19) 0.0374(15) -0.0120(13) -0.0013(13) -0.0223(15) C8 0.0340(14) 0.0272(12) 0.0509(16) -0.0033(11) 0.0056(12) -0.0050(11) C9 0.0263(13) 0.0386(14) 0.0628(19) 0.0072(13) -0.0178(12) -0.0137(11) C10 0.0555(19) 0.062(2) 0.0375(15) 0.0160(14) -0.0166(14) -0.0225(16) C11 0.127(4) 0.124(4) 0.074(3) 0.047(3) -0.067(3) -0.080(4) C12 0.153(5) 0.130(5) 0.081(3) 0.034(3) -0.071(4) -0.099(4) C13 0.123(4) 0.057(2) 0.063(2) 0.0034(18) -0.054(3) -0.041(2) C14 0.0452(19) 0.0248(14) 0.131(4) -0.0030(18) -0.031(2) -0.0088(13) C15 0.048(2) 0.0332(16) 0.119(4) -0.0094(19) -0.019(2) -0.0042(14) C16 0.037(3) 0.039(3) 0.083(6) 0.008(3) -0.025(3) -0.004(2) C17 0.0277(14) 0.0384(15) 0.074(2) 0.0058(14) -0.0160(14) -0.0098(12) C15A 0.048(2) 0.0332(16) 0.119(4) -0.0094(19) -0.019(2) -0.0042(14) C16A 0.033(5) 0.047(6) 0.078(10) 0.004(6) -0.006(5) -0.004(4) C17A 0.0277(14) 0.0384(15) 0.074(2) 0.0058(14) -0.0160(14) -0.0098(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 Ce O6 2.3643(16) . ? Ce O6 2.4132(16) 2_676 ? Ce O3 2.5633(16) . ? Ce O1 2.5699(16) . ? Ce O8 2.6008(17) . ? Ce O5 2.6036(17) 2_676 ? Ce O7 2.6175(18) . ? Ce C1 2.732(2) . ? S O4 1.429(2) . ? S O5 1.4497(19) . ? S O3 1.4528(17) . ? S C8 1.827(3) . ? Si1 O2 1.658(2) . ? Si1 O1 1.6863(19) . ? Si1 C1 1.786(3) . ? Si1 C2 1.862(3) . ? Si2 C1 1.832(3) . ? Si2 C7 1.876(3) . ? Si2 C6 1.883(3) . ? Si2 C5 1.894(3) . ? F11 C8 1.325(3) . ? F12 C8 1.325(4) . ? F13 C8 1.332(3) . ? O1 C3 1.443(3) . ? O2 C4 1.399(4) . ? O6 C9 1.411(3) . ? O7 C13 1.432(4) . ? O7 C10 1.456(3) . ? O8 C14 1.449(4) . ? O8 C17 1.450(3) . ? C10 C11 1.492(5) . ? C11 C12 1.483(7) . ? C12 C13 1.420(6) . ? C14 C15 1.478(5) . ? C18 C22A 1.110(14) . ? C18 C19 1.481(14) . ? C19 C20A 1.19(2) . ? C19 C20 1.589(16) . ? C20 C21 1.365(15) . ? C21 C22 1.352(16) . ? C20A C21A 1.83(3) . ? C21A C22A 1.20(2) . ? C23 C24 1.376(16) . ? C23 C26 1.377(16) 2_587 ? C24 C25 1.009(16) . ? C25 C26 1.082(15) . ? C25 C25 1.66(2) 2_587 ? C15 C16 1.503(7) . ? C16 C17 1.504(7) . ? 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 O6 Ce O6 70.27(6) . 2_676 ? O6 Ce O3 76.68(6) . . ? O6 Ce O3 77.00(5) 2_676 . ? O6 Ce O1 83.80(6) . . ? O6 Ce O1 143.40(6) 2_676 . ? O3 Ce O1 122.46(6) . . ? O6 Ce O8 141.13(6) . . ? O6 Ce O8 105.58(6) 2_676 . ? O3 Ce O8 141.55(6) . . ? O1 Ce O8 78.63(6) . . ? O6 Ce O5 76.18(6) . 2_676 ? O6 Ce O5 76.06(6) 2_676 2_676 ? O3 Ce O5 146.77(5) . 2_676 ? O1 Ce O5 72.89(6) . 2_676 ? O8 Ce O5 65.61(6) . 2_676 ? O6 Ce O7 142.55(6) . . ? O6 Ce O7 79.85(6) 2_676 . ? O3 Ce O7 74.98(6) . . ? O1 Ce O7 132.47(6) . . ? O8 Ce O7 68.00(6) . . ? O5 Ce O7 118.41(6) 2_676 . ? O6 Ce C1 115.84(7) . . ? O6 Ce C1 153.72(6) 2_676 . ? O3 Ce C1 79.74(6) . . ? O1 Ce C1 61.42(6) . . ? O8 Ce C1 85.36(7) . . ? O5 Ce C1 129.86(6) 2_676 . ? O7 Ce C1 82.47(7) . . ? O4 S O5 115.49(12) . . ? O4 S O3 115.59(12) . . ? O5 S O3 113.69(10) . . ? O4 S C8 103.83(14) . . ? O5 S C8 102.57(13) . . ? O3 S C8 103.29(12) . . ? O2 Si1 O1 101.08(10) . . ? O2 Si1 C1 118.52(12) . . ? O1 Si1 C1 102.63(10) . . ? O2 Si1 C2 107.12(13) . . ? O1 Si1 C2 107.24(13) . . ? C1 Si1 C2 118.13(13) . . ? O2 Si1 Ce 125.15(8) . . ? O1 Si1 Ce 48.47(6) . . ? C1 Si1 Ce 54.34(8) . . ? C2 Si1 Ce 123.93(11) . . ? C1 Si2 C7 112.36(14) . . ? C1 Si2 C6 112.95(13) . . ? C7 Si2 C6 106.76(15) . . ? C1 Si2 C5 113.12(14) . . ? C7 Si2 C5 105.45(16) . . ? C6 Si2 C5 105.61(17) . . ? C3 O1 Si1 122.10(17) . . ? C3 O1 Ce 135.75(16) . . ? Si1 O1 Ce 102.12(8) . . ? C4 O2 Si1 121.4(2) . . ? S O3 Ce 135.45(10) . . ? S O5 Ce 135.38(10) . 2_676 ? C9 O6 Ce 111.54(15) . . ? C9 O6 Ce 130.27(15) . 2_676 ? Ce O6 Ce 109.73(6) . 2_676 ? C13 O7 C10 105.6(2) . . ? C13 O7 Ce 124.96(19) . . ? C10 O7 Ce 127.74(18) . . ? C14 O8 C17 107.3(2) . . ? C14 O8 Ce 126.07(18) . . ? C17 O8 Ce 118.89(15) . . ? Si1 C1 Si2 120.65(13) . . ? Si1 C1 Ce 93.57(10) . . ? Si2 C1 Ce 128.76(11) . . ? F12 C8 F11 108.3(2) . . ? F12 C8 F13 108.0(3) . . ? F11 C8 F13 108.1(2) . . ? F12 C8 S 111.70(19) . . ? F11 C8 S 110.8(2) . . ? F13 C8 S 109.8(2) . . ? O7 C10 C11 105.7(3) . . ? C12 C11 C10 105.5(3) . . ? C13 C12 C11 106.9(4) . . ? C12 C13 O7 107.3(4) . . ? O8 C14 C15 107.8(3) . . ? C22A C18 C19 119.4(13) . . ? C19 C18 C22 97.0(9) . . ? C20A C19 C18 103.2(15) . . ? C18 C19 C20 109.4(9) . . ? C21 C20 C19 107.8(10) . . ? C22 C21 C20 110.0(11) . . ? C21 C22 C18 110.7(10) . . ? C24 C23 C26 102.6(11) . 2_587 ? C25 C24 C23 114.6(15) . . ? C24 C25 C26 152.5(18) . . ? C24 C25 C25 104.4(16) . 2_587 ? C26 C25 C25 102.6(15) . 2_587 ? C25 C26 C23 113.0(14) . 2_587 ? C19 C20A C21A 100.2(17) . . ? C22A C21A C20A 98.2(15) . . ? C18 C22A C21A 109.5(15) . . ? C14 C15 C16 105.6(3) . . ? C15 C16 C17 103.2(4) . . ? O8 C17 C16 104.5(3) . . ? #===END