# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_contact_author_name 'Evamarie Hey-Hawkins' _publ_contact_author_address ; Department of Inorganic Chemistry Faculty of Chemistry and Mineralogy Johannisallee 29 Leipzig Saxony 04103 GERMANY ; _publ_contact_author_phone '49 / 341 / 9736151' _publ_contact_author_fax '49 / 341 / 9736199' _publ_contact_author_email hey@rz.uni-leipzig.de _publ_section_title ; [Li(thf)3(P4tBu4CH)] - Synthesis, molecular structure and investigation of its dynamic behaviour ; loop_ _publ_author_name _publ_author_address R.Wolf ; Institut fur Anorganische Chemie Universitat Leipzig Johannisallee 29 04103 Leipzig Bundesrepublik Deutschland ; E.Hey-Hawkins ; Institut fur Anorganische Chemie Universitat Leipzig Johannisallee 29 04103 Leipzig Bundesrepublik Deutschland ; #------------------------------------------------------------------------------# # DATA BLOCK # #------------------------------------------------------------------------------# data_c1740n _database_code_depnum_ccdc_archive 'CCDC 242536' _audit_creation_method shelxl-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H61 Li O3 P4' _chemical_formula_weight 588.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_h-m P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.996(5) _cell_length_b 19.104(5) _cell_length_c 10.290(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 113.132(5) _cell_angle_gamma 90.000(5) _cell_volume 1807.0(13) _cell_formula_units_z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 105 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 27.0 _exptl_crystal_description plate _exptl_crystal_colour 'light pink' _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.082 _exptl_crystal_density_method 'not measured' _exptl_crystal_f_000 644 _exptl_absorpt_coefficient_mu 0.234 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_t_min 0.8725 _exptl_absorpt_correction_t_max 0.9770 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mok\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10532 _diffrn_reflns_av_r_equivalents 0.0342 _diffrn_reflns_av_sigmai/neti 0.0455 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 27.00 _reflns_number_total 5268 _reflns_number_gt 4596 _reflns_threshold_expression >2sigma(i) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR92 (A. Altomare et al., 1999)' _computing_structure_refinement 'Shelxl-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL PLUS' _computing_publication_material 'WINGX v1.64.05 (L. J. Farrugia, 1999)' _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. Two of the thf molecules exhibit site disorder. The atoms of these thf molecules were split over two positions and refined with equal occupancy factors for each molecule. The thermal displacement parameters were refined isotropically for these molecules. ; _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^)+(0.0555p)^2^+1.0273p] where p=(fo^2^+2fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'flack h d (1983), acta cryst. a39, 876-881' _refine_ls_abs_structure_flack 0.21(17) _refine_ls_number_reflns 5268 _refine_ls_number_parameters 361 _refine_ls_number_restraints 1 _refine_ls_r_factor_all 0.0741 _refine_ls_r_factor_gt 0.0628 _refine_ls_wr_factor_ref 0.1353 _refine_ls_wr_factor_gt 0.1313 _refine_ls_goodness_of_fit_ref 1.170 _refine_ls_restrained_s_all 1.170 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_u_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3521(5) 0.9639(3) 0.1131(4) 0.0319(10) Uani 1 1 d . A . C10 C 0.2983(5) 0.8342(3) -0.0670(5) 0.0471(14) Uani 1 1 d . . . C11 C 0.4406(6) 0.8420(4) -0.0843(6) 0.073(2) Uani 1 1 d . . . H11A H 0.5180 0.8207 -0.0044 0.109 Uiso 1 1 calc R . . H11B H 0.4615 0.8914 -0.0888 0.109 Uiso 1 1 calc R . . H11C H 0.4338 0.8191 -0.1708 0.109 Uiso 1 1 calc R . . C12 C 0.2610(7) 0.7572(4) -0.0624(8) 0.077(2) Uani 1 1 d . . . H12A H 0.1696 0.7532 -0.0508 0.115 Uiso 1 1 calc R . . H12B H 0.3375 0.7346 0.0164 0.115 Uiso 1 1 calc R . . H12C H 0.2522 0.7347 -0.1499 0.115 Uiso 1 1 calc R . . C13 C 0.1755(6) 0.8686(4) -0.1913(5) 0.073(2) Uani 1 1 d . . . H13A H 0.0848 0.8641 -0.1784 0.110 Uiso 1 1 calc R . . H13B H 0.1663 0.8458 -0.2786 0.110 Uiso 1 1 calc R . . H13C H 0.1975 0.9178 -0.1957 0.110 Uiso 1 1 calc R . . C20 C 0.3874(5) 0.8105(3) 0.4057(5) 0.0495(13) Uani 1 1 d . . . C21 C 0.3319(6) 0.8782(4) 0.4395(6) 0.0588(15) Uani 1 1 d . . . H21A H 0.4113 0.9115 0.4756 0.088 Uiso 1 1 calc R . . H21B H 0.2922 0.8700 0.5103 0.088 Uiso 1 1 calc R . . H21C H 0.2565 0.8968 0.3545 0.088 Uiso 1 1 calc R . . C22 C 0.5062(7) 0.7812(4) 0.5398(6) 0.0656(18) Uani 1 1 d . . . H22A H 0.5425 0.7376 0.5178 0.098 Uiso 1 1 calc R . . H22B H 0.4661 0.7727 0.6103 0.098 Uiso 1 1 calc R . . H22C H 0.5852 0.8147 0.5763 0.098 Uiso 1 1 calc R . . C23 C 0.2634(7) 0.7572(4) 0.3480(7) 0.077(2) Uani 1 1 d . . . H23A H 0.3006 0.7138 0.3262 0.116 Uiso 1 1 calc R . . H23B H 0.1879 0.7755 0.2629 0.116 Uiso 1 1 calc R . . H23C H 0.2233 0.7484 0.4184 0.116 Uiso 1 1 calc R . . C30 C 0.8043(5) 0.8600(3) 0.3553(5) 0.0448(13) Uani 1 1 d . . . C31 C 0.9204(5) 0.9159(4) 0.3967(7) 0.0653(17) Uani 1 1 d . . . H31A H 0.8932 0.9520 0.3247 0.098 Uiso 1 1 calc R . . H31B H 1.0123 0.8953 0.4057 0.098 Uiso 1 1 calc R . . H31C H 0.9304 0.9364 0.4863 0.098 Uiso 1 1 calc R . . C32 C 0.8501(6) 0.8044(4) 0.4709(6) 0.0626(17) Uani 1 1 d . . . H32A H 0.7767 0.7680 0.4467 0.094 Uiso 1 1 calc R . . H32B H 0.8606 0.8257 0.5600 0.094 Uiso 1 1 calc R . . H32C H 0.9423 0.7842 0.4797 0.094 Uiso 1 1 calc R . . C33 C 0.7880(5) 0.8280(4) 0.2155(6) 0.0602(17) Uani 1 1 d . . . H33A H 0.7132 0.7922 0.1894 0.090 Uiso 1 1 calc R . . H33B H 0.8796 0.8072 0.2242 0.090 Uiso 1 1 calc R . . H33C H 0.7606 0.8640 0.1434 0.090 Uiso 1 1 calc R . . C40 C 0.5762(5) 1.0649(3) 0.2669(5) 0.0407(11) Uani 1 1 d . . . C41 C 0.5099(6) 1.0704(3) 0.3746(6) 0.0557(14) Uani 1 1 d . . . H41A H 0.4060 1.0619 0.3294 0.084 Uiso 1 1 calc R . . H41B H 0.5268 1.1169 0.4157 0.084 Uiso 1 1 calc R . . H41C H 0.5539 1.0359 0.4484 0.084 Uiso 1 1 calc R . . C42 C 0.7401(6) 1.0779(4) 0.3398(7) 0.0652(18) Uani 1 1 d . . . H42A H 0.7837 1.0744 0.2709 0.098 Uiso 1 1 calc R . . H42B H 0.7832 1.0432 0.4133 0.098 Uiso 1 1 calc R . . H42C H 0.7572 1.1243 0.3814 0.098 Uiso 1 1 calc R . . C43 C 0.5119(6) 1.1205(3) 0.1509(7) 0.0633(17) Uani 1 1 d . . . H43A H 0.5556 1.1159 0.0822 0.095 Uiso 1 1 calc R . . H43B H 0.5320 1.1667 0.1929 0.095 Uiso 1 1 calc R . . H43C H 0.4075 1.1138 0.1044 0.095 Uiso 1 1 calc R . . O1 O -0.0294(11) 1.0005(6) -0.0970(11) 0.046(3) Uiso 0.50 1 d P A 1 C100 C -0.0861(13) 0.9585(7) -0.0131(14) 0.044(3) Uiso 0.50 1 d P A 1 H10A H -0.0655 0.9801 0.0791 0.053 Uiso 0.50 1 calc PR A 1 H10B H -0.0448 0.9112 0.0013 0.053 Uiso 0.50 1 calc PR A 1 C101 C -0.2454(17) 0.9569(10) -0.1004(18) 0.085(5) Uiso 0.50 1 d P A 1 H10C H -0.2716 0.9158 -0.1624 0.101 Uiso 0.50 1 calc PR A 1 H10D H -0.3011 0.9562 -0.0405 0.101 Uiso 0.50 1 calc PR A 1 C102 C -0.2728(18) 1.0230(11) -0.1847(19) 0.090(5) Uiso 0.50 1 d P A 1 H10E H -0.3533 1.0159 -0.2765 0.108 Uiso 0.50 1 calc PR A 1 H10F H -0.3004 1.0603 -0.1348 0.108 Uiso 0.50 1 calc PR A 1 C103 C -0.1519(14) 1.0419(9) -0.2044(14) 0.061(4) Uiso 0.50 1 d P A 1 H10G H -0.1343 1.0923 -0.1889 0.073 Uiso 0.50 1 calc PR A 1 H10H H -0.1617 1.0305 -0.3005 0.073 Uiso 0.50 1 calc PR A 1 O11 O -0.0342(10) 0.9908(6) -0.1295(10) 0.046(3) Uiso 0.50 1 d P A 2 C104 C -0.0915(18) 0.9428(10) -0.0545(17) 0.070(5) Uiso 0.50 1 d P A 2 H10I H -0.0342 0.8995 -0.0323 0.084 Uiso 0.50 1 calc PR A 2 H10J H -0.0852 0.9640 0.0344 0.084 Uiso 0.50 1 calc PR A 2 C105 C -0.2357(18) 0.9279(10) -0.1393(18) 0.085(5) Uiso 0.50 1 d P A 2 H10K H -0.2930 0.9205 -0.0820 0.102 Uiso 0.50 1 calc PR A 2 H10L H -0.2430 0.8861 -0.1970 0.102 Uiso 0.50 1 calc PR A 2 C106 C -0.2824(13) 0.9872(8) -0.2235(14) 0.060(3) Uiso 0.50 1 d P A 2 H10M H -0.3206 1.0225 -0.1780 0.072 Uiso 0.50 1 calc PR A 2 H10N H -0.3577 0.9754 -0.3161 0.072 Uiso 0.50 1 calc PR A 2 C107 C -0.1457(14) 1.0124(8) -0.2370(14) 0.058(3) Uiso 0.50 1 d P A 2 H10O H -0.1414 0.9944 -0.3244 0.070 Uiso 0.50 1 calc PR A 2 H10P H -0.1455 1.0637 -0.2408 0.070 Uiso 0.50 1 calc PR A 2 C200 C 0.0816(8) 1.1233(4) 0.1400(8) 0.0617(17) Uani 1 1 d . . . C201 C 0.1398(10) 1.1915(5) 0.2127(8) 0.079(2) Uani 1 1 d . . . C202 C 0.1581(11) 1.2368(4) 0.1002(11) 0.088(3) Uani 1 1 d . . . C203 C 0.1332(9) 1.1884(4) -0.0226(8) 0.0701(19) Uani 1 1 d . . . O3 O 0.2138(8) 1.0730(4) -0.2093(8) 0.036(2) Uiso 0.55 1 d P A 3 C300 C 0.1166(17) 1.1050(10) -0.3351(17) 0.080(5) Uiso 0.55 1 d P A 3 H30A H 0.1060 1.1553 -0.3233 0.096 Uiso 0.55 1 calc PR A 3 H30B H 0.0207 1.0826 -0.3715 0.096 Uiso 0.55 1 calc PR A 3 C301 C 0.2120(19) 1.0878(11) -0.4385(19) 0.089(6) Uiso 0.55 1 d P A 3 H30C H 0.1898 1.0411 -0.4809 0.107 Uiso 0.55 1 calc PR A 3 H30D H 0.1920 1.1228 -0.5135 0.107 Uiso 0.55 1 calc PR A 3 C302 C 0.3456(14) 1.0918(9) -0.3466(14) 0.074(4) Uiso 0.55 1 d P A 3 H30E H 0.3844 1.1387 -0.3495 0.089 Uiso 0.55 1 calc PR A 3 H30F H 0.4059 1.0576 -0.3699 0.089 Uiso 0.55 1 calc PR A 3 C303 C 0.3507(13) 1.0790(8) -0.2155(13) 0.066(3) Uiso 0.55 1 d P A 3 H30G H 0.4046 1.1169 -0.1525 0.079 Uiso 0.55 1 calc PR A 3 H30H H 0.4048 1.0354 -0.1804 0.079 Uiso 0.55 1 calc PR A 3 O33 O 0.2089(10) 1.0506(6) -0.2210(10) 0.042(3) Uiso 0.45 1 d P A 4 C304 C 0.1103(15) 1.0779(8) -0.3534(14) 0.044(3) Uiso 0.45 1 d P A 4 H30I H 0.0280 1.0454 -0.3911 0.053 Uiso 0.45 1 calc PR A 4 H30J H 0.0721 1.1223 -0.3348 0.053 Uiso 0.45 1 calc PR A 4 C305 C 0.1585(18) 1.0887(9) -0.4511(16) 0.056(4) Uiso 0.45 1 d P A 4 H30K H 0.1682 1.1387 -0.4672 0.067 Uiso 0.45 1 calc PR A 4 H30L H 0.0986 1.0659 -0.5403 0.067 Uiso 0.45 1 calc PR A 4 C306 C 0.3146(19) 1.0507(12) -0.3729(17) 0.080(5) Uiso 0.45 1 d P A 4 H30M H 0.3142 1.0057 -0.4187 0.096 Uiso 0.45 1 calc PR A 4 H30N H 0.3911 1.0799 -0.3820 0.096 Uiso 0.45 1 calc PR A 4 C307 C 0.3432(15) 1.0403(9) -0.2358(15) 0.059(4) Uiso 0.45 1 d P A 4 H30O H 0.4165 1.0736 -0.1769 0.071 Uiso 0.45 1 calc PR A 4 H30P H 0.3793 0.9926 -0.2076 0.071 Uiso 0.45 1 calc PR A 4 P1 P 0.29050(11) 0.87578(7) 0.09787(12) 0.0332(3) Uani 1 1 d . . . P2 P 0.47163(12) 0.81764(7) 0.26865(12) 0.0349(3) Uani 1 1 d . . . P3 P 0.63024(11) 0.90188(7) 0.35677(11) 0.0318(3) Uani 1 1 d . . . P4 P 0.54448(12) 0.97721(7) 0.17035(12) 0.0328(3) Uani 1 1 d . . . Li1 Li 0.1775(8) 1.0283(5) -0.0463(8) 0.0401(19) Uani 1 1 d . . . O2 O 0.1341(4) 1.1188(2) 0.0290(4) 0.0525(9) Uani 1 1 d . A . H67 H 0.049(7) 1.199(4) -0.095(7) 0.07(2) Uiso 1 1 d . . . H63 H 0.070(8) 1.215(4) 0.240(7) 0.09(3) Uiso 1 1 d . . . H1 H 0.317(5) 0.983(3) 0.165(5) 0.033(13) Uiso 1 1 d . . . H65 H 0.257(12) 1.258(6) 0.124(11) 0.16(4) Uiso 1 1 d . . . H66 H 0.086(11) 1.262(6) 0.084(11) 0.14(4) Uiso 1 1 d . . . H61 H -0.019(10) 1.118(5) 0.105(9) 0.13(4) Uiso 1 1 d . . . H64 H 0.226(9) 1.175(5) 0.266(9) 0.11(3) Uiso 1 1 d . . . H62 H 0.110(7) 1.087(4) 0.210(7) 0.07(2) Uiso 1 1 d . . . H68 H 0.199(7) 1.184(4) -0.061(6) 0.07(2) 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 C1 0.031(2) 0.035(3) 0.030(2) 0.000(2) 0.0123(18) 0.002(2) C10 0.039(3) 0.055(4) 0.040(3) -0.024(3) 0.007(2) 0.003(2) C11 0.057(3) 0.116(7) 0.048(3) -0.035(4) 0.023(3) -0.001(4) C12 0.070(4) 0.063(5) 0.089(5) -0.037(4) 0.022(4) -0.006(4) C13 0.067(4) 0.102(6) 0.033(3) -0.023(3) 0.000(2) 0.017(4) C20 0.042(3) 0.054(4) 0.053(3) 0.017(3) 0.019(2) -0.003(3) C21 0.056(3) 0.070(4) 0.064(3) 0.013(3) 0.038(3) 0.010(3) C22 0.072(4) 0.076(5) 0.050(3) 0.025(3) 0.026(3) 0.003(4) C23 0.062(4) 0.080(5) 0.084(5) 0.025(4) 0.022(3) -0.018(4) C30 0.027(2) 0.051(4) 0.050(3) -0.002(2) 0.0075(19) 0.016(2) C31 0.033(3) 0.066(4) 0.092(4) -0.002(4) 0.019(3) -0.004(3) C32 0.043(3) 0.059(4) 0.077(4) 0.007(3) 0.013(3) 0.019(3) C33 0.038(3) 0.078(5) 0.063(3) -0.012(3) 0.020(2) 0.013(3) C40 0.040(2) 0.029(3) 0.046(3) -0.004(2) 0.008(2) -0.003(2) C41 0.068(3) 0.046(4) 0.052(3) -0.011(3) 0.023(3) -0.001(3) C42 0.053(3) 0.049(4) 0.072(4) -0.006(3) 0.000(3) -0.012(3) C43 0.060(3) 0.037(3) 0.078(4) 0.014(3) 0.011(3) -0.008(3) C200 0.065(4) 0.063(5) 0.064(4) -0.001(4) 0.033(3) 0.006(4) C201 0.078(5) 0.080(6) 0.066(5) -0.015(4) 0.013(4) 0.010(5) C202 0.084(6) 0.049(5) 0.137(8) -0.019(5) 0.049(6) -0.007(4) C203 0.077(5) 0.053(4) 0.074(5) 0.021(4) 0.023(4) 0.022(4) P1 0.0256(5) 0.0355(7) 0.0342(6) -0.0033(5) 0.0074(4) 0.0011(5) P2 0.0307(6) 0.0298(6) 0.0403(6) 0.0015(6) 0.0097(5) 0.0023(5) P3 0.0277(5) 0.0346(7) 0.0302(5) 0.0000(5) 0.0083(4) 0.0038(5) P4 0.0311(6) 0.0362(7) 0.0297(6) 0.0017(5) 0.0105(5) -0.0010(5) Li1 0.039(4) 0.042(5) 0.039(4) 0.004(4) 0.015(3) 0.000(4) O2 0.064(2) 0.041(2) 0.058(2) 0.0041(19) 0.0295(18) 0.0065(19) _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 C1 P1 1.778(5) . ? C1 P4 1.794(4) . ? C1 Li1 2.236(9) . ? C10 C11 1.509(7) . ? C10 C13 1.531(8) . ? C10 C12 1.523(9) . ? C10 P1 1.903(5) . ? C20 C21 1.500(9) . ? C20 C23 1.533(9) . ? C20 C22 1.530(7) . ? C20 P2 1.911(5) . ? C30 C31 1.510(8) . ? C30 C32 1.525(8) . ? C30 C33 1.512(7) . ? C30 P3 1.920(5) . ? C40 C41 1.502(7) . ? C40 C42 1.531(7) . ? C40 C43 1.537(7) . ? C40 P4 1.909(5) . ? O1 C100 1.448(16) . ? O1 C103 1.510(17) . ? O1 Li1 1.996(13) . ? C100 C101 1.489(19) . ? C101 C102 1.49(2) . ? C102 C103 1.35(2) . ? O11 C107 1.291(15) . ? O11 C104 1.453(19) . ? O11 Li1 2.073(13) . ? C104 C105 1.39(2) . ? C105 C106 1.39(2) . ? C106 C107 1.507(18) . ? C200 O2 1.434(7) . ? C200 C201 1.502(11) . ? C201 C202 1.513(13) . ? C202 C203 1.507(12) . ? C203 O2 1.430(8) . ? O3 C303 1.400(14) . ? O3 C300 1.416(18) . ? O3 Li1 2.038(11) . ? C300 C301 1.72(2) . ? C301 C302 1.30(2) . ? C302 C303 1.352(17) . ? O33 C307 1.422(17) . ? O33 C304 1.429(17) . ? O33 Li1 1.989(13) . ? C304 C305 1.29(2) . ? C305 C306 1.62(2) . ? C306 C307 1.34(2) . ? P1 P2 2.2584(17) . ? P2 P3 2.1900(18) . ? P3 P4 2.2789(18) . ? Li1 O2 2.010(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 C1 P4 116.9(3) . . ? P1 C1 Li1 108.2(3) . . ? P4 C1 Li1 126.2(3) . . ? C11 C10 C13 110.0(5) . . ? C11 C10 C12 110.7(5) . . ? C13 C10 C12 108.4(5) . . ? C11 C10 P1 115.7(3) . . ? C13 C10 P1 105.4(4) . . ? C12 C10 P1 106.3(4) . . ? C21 C20 C23 110.3(5) . . ? C21 C20 C22 109.5(5) . . ? C23 C20 C22 109.2(5) . . ? C21 C20 P2 114.9(4) . . ? C23 C20 P2 106.5(4) . . ? C22 C20 P2 106.3(4) . . ? C31 C30 C32 108.1(4) . . ? C31 C30 C33 109.8(5) . . ? C32 C30 C33 110.3(5) . . ? C31 C30 P3 107.6(4) . . ? C32 C30 P3 106.2(4) . . ? C33 C30 P3 114.6(3) . . ? C41 C40 C42 109.0(4) . . ? C41 C40 C43 110.7(5) . . ? C42 C40 C43 108.0(5) . . ? C41 C40 P4 114.5(4) . . ? C42 C40 P4 108.9(4) . . ? C43 C40 P4 105.6(4) . . ? C100 O1 C103 109.3(10) . . ? C100 O1 Li1 126.9(8) . . ? C103 O1 Li1 120.8(9) . . ? O1 C100 C101 103.1(11) . . ? C102 C101 C100 104.0(14) . . ? C103 C102 C101 110.0(15) . . ? C102 C103 O1 105.5(13) . . ? C107 O11 C104 105.6(11) . . ? C107 O11 Li1 129.8(9) . . ? C104 O11 Li1 123.3(9) . . ? C105 C104 O11 108.9(13) . . ? C104 C105 C106 103.6(15) . . ? C105 C106 C107 102.9(12) . . ? O11 C107 C106 109.1(11) . . ? O2 C200 C201 104.9(6) . . ? C202 C201 C200 104.8(6) . . ? C203 C202 C201 105.1(7) . . ? O2 C203 C202 106.6(6) . . ? C303 O3 C300 104.8(10) . . ? C303 O3 Li1 124.4(7) . . ? C300 O3 Li1 130.7(8) . . ? O3 C300 C301 97.8(12) . . ? C302 C301 C300 101.5(13) . . ? C301 C302 C303 109.9(13) . . ? C302 C303 O3 114.0(11) . . ? C307 O33 C304 106.0(10) . . ? C307 O33 Li1 123.9(9) . . ? C304 O33 Li1 130.1(8) . . ? C305 C304 O33 118.2(13) . . ? C304 C305 C306 97.0(13) . . ? C307 C306 C305 110.8(14) . . ? C306 C307 O33 105.8(12) . . ? C1 P1 C10 109.9(3) . . ? C1 P1 P2 104.65(15) . . ? C10 P1 P2 100.79(17) . . ? C20 P2 P3 101.76(19) . . ? C20 P2 P1 99.11(17) . . ? P3 P2 P1 100.92(7) . . ? C30 P3 P2 101.63(18) . . ? C30 P3 P4 107.38(17) . . ? P2 P3 P4 98.27(6) . . ? C1 P4 C40 103.4(2) . . ? C1 P4 P3 100.79(16) . . ? C40 P4 P3 100.67(16) . . ? O33 Li1 O1 109.6(6) . . ? O33 Li1 O2 107.4(5) . . ? O1 Li1 O2 88.3(5) . . ? O33 Li1 O3 12.5(4) . . ? O1 Li1 O3 113.4(5) . . ? O2 Li1 O3 95.3(4) . . ? O33 Li1 O11 101.5(5) . . ? O1 Li1 O11 10.2(4) . . ? O2 Li1 O11 96.7(5) . . ? O3 Li1 O11 106.7(5) . . ? O33 Li1 C1 115.2(5) . . ? O1 Li1 C1 118.4(5) . . ? O2 Li1 C1 114.5(4) . . ? O3 Li1 C1 119.6(4) . . ? O11 Li1 C1 119.3(5) . . ? C200 O2 C203 106.8(5) . . ? C200 O2 Li1 124.1(5) . . ? C203 O2 Li1 128.8(5) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.357 _refine_diff_density_min -0.257 _refine_diff_density_rms 0.054 #------------------------------------------------------------------------------# # END OF DATA BLOCK # #------------------------------------------------------------------------------#