Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_cambridge 222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_requested_category FM _publ_contact_author_name 'Peter Hitchcock' _publ_contact_author_email P.B.Hitchcock@sussex.ac.uk loop_ _publ_author_name N.E.Mansfield M.P.Coles P.B.Hitchcock data_jul2201 _database_code_depnum_ccdc_archive 'CCDC 182913' _audit_creation_date 2001-07-24T16:29:39-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[{Li(thf)(Ph2PC(NiPr)2)}2]' _chemical_formula_moiety 'C46 H64 Li2 N4 O2 P2' _chemical_formula_sum 'C46 H64 Li2 N4 O2 P2' _chemical_formula_weight 780.83 _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 9.9739(7) _cell_length_b 19.6236(13) _cell_length_c 11.6860(8) _cell_angle_alpha 90 _cell_angle_beta 94.531(3) _cell_angle_gamma 90 _cell_volume 2280.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 13436 _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 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.137 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.135 _exptl_absorpt_correction_T_min 0.948 _exptl_absorpt_correction_T_max 0.9607 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _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_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 8491 _diffrn_reflns_av_R_equivalents 0.0881 _diffrn_reflns_av_unetI/netI 0.0792 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 25.05 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.975 _diffrn_measured_fraction_theta_max 0.975 _reflns_number_total 3937 _reflns_number_gt 3047 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _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^)+(0.0833P)^2^+1.2719P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 3937 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0849 _refine_ls_R_factor_gt 0.0634 _refine_ls_wR_factor_ref 0.1769 _refine_ls_wR_factor_gt 0.1616 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.599 _refine_diff_density_min -0.28 _refine_diff_density_rms 0.052 #----------------------------------------------------------------------------# # 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' Li Li -0.0003 0.0001 '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' O O 0.0106 0.006 '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' 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 P P 0.01649(7) 0.35094(3) 0.27824(6) 0.0351(2) Uani 1 1 d . . . O O 0.0205(2) 0.38413(10) -0.15953(17) 0.0490(5) Uani 1 1 d . . . N1 N 0.1447(2) 0.41326(11) 0.10590(18) 0.0345(5) Uani 1 1 d . . . N2 N -0.07246(19) 0.44838(10) 0.09920(17) 0.0303(5) Uani 1 1 d . . . C1 C 0.0261(2) 0.40897(12) 0.1474(2) 0.0294(6) Uani 1 1 d . . . C2 C 0.2658(3) 0.38187(15) 0.1630(2) 0.0396(7) Uani 1 1 d . . . H2 H 0.2399 0.3383 0.1998 0.047 Uiso 1 1 calc R . . C3 C 0.3304(3) 0.42875(18) 0.2551(3) 0.0587(9) Uani 1 1 d . . . H3A H 0.2659 0.4384 0.312 0.088 Uiso 1 1 calc R . . H3B H 0.357 0.4715 0.2198 0.088 Uiso 1 1 calc R . . H3C H 0.4101 0.4066 0.2929 0.088 Uiso 1 1 calc R . . C4 C 0.3631(3) 0.3660(2) 0.0733(3) 0.0596(9) Uani 1 1 d . . . H4A H 0.3194 0.336 0.0147 0.089 Uiso 1 1 calc R . . H4B H 0.4429 0.3434 0.11 0.089 Uiso 1 1 calc R . . H4C H 0.3899 0.4085 0.0374 0.089 Uiso 1 1 calc R . . C5 C -0.2149(2) 0.43115(14) 0.1051(2) 0.0344(6) Uani 1 1 d . . . H5 H -0.2221 0.3899 0.1544 0.041 Uiso 1 1 calc R . . C6 C -0.2771(3) 0.41536(16) -0.0160(2) 0.0435(7) Uani 1 1 d . . . H6A H -0.2282 0.3776 -0.0485 0.065 Uiso 1 1 calc R . . H6B H -0.2712 0.4558 -0.0646 0.065 Uiso 1 1 calc R . . H6C H -0.3717 0.4026 -0.0124 0.065 Uiso 1 1 calc R . . C7 C -0.2905(3) 0.48966(15) 0.1559(3) 0.0445(7) Uani 1 1 d . . . H7A H -0.2507 0.4995 0.2335 0.067 Uiso 1 1 calc R . . H7B H -0.3852 0.477 0.1593 0.067 Uiso 1 1 calc R . . H7C H -0.2844 0.5302 0.1077 0.067 Uiso 1 1 calc R . . C8 C -0.1251(3) 0.38040(14) 0.3552(2) 0.0349(6) Uani 1 1 d . . . C9 C -0.2378(3) 0.34174(15) 0.3753(2) 0.0434(7) Uani 1 1 d . . . H9 H -0.249 0.298 0.3412 0.052 Uiso 1 1 calc R . . C10 C -0.3333(3) 0.36590(17) 0.4438(3) 0.0512(8) Uani 1 1 d . . . H10 H -0.4093 0.3385 0.4564 0.061 Uiso 1 1 calc R . . C11 C -0.3204(3) 0.42920(18) 0.4941(3) 0.0525(8) Uani 1 1 d . . . H11 H -0.3875 0.446 0.5401 0.063 Uiso 1 1 calc R . . C12 C -0.2085(3) 0.46781(16) 0.4768(2) 0.0486(8) Uani 1 1 d . . . H12 H -0.1982 0.5114 0.5117 0.058 Uiso 1 1 calc R . . C13 C -0.1114(3) 0.44384(15) 0.4093(2) 0.0439(7) Uani 1 1 d . . . H13 H -0.0341 0.4708 0.3995 0.053 Uiso 1 1 calc R . . C14 C -0.0399(3) 0.26875(14) 0.2179(2) 0.0401(6) Uani 1 1 d . . . C15 C -0.0067(3) 0.21069(15) 0.2828(3) 0.0548(8) Uani 1 1 d . . . H15 H 0.044 0.2156 0.3547 0.066 Uiso 1 1 calc R . . C16 C -0.0447(4) 0.14687(17) 0.2464(4) 0.0672(10) Uani 1 1 d . . . H16 H -0.021 0.1083 0.2929 0.081 Uiso 1 1 calc R . . C17 C -0.1172(4) 0.13855(16) 0.1427(3) 0.0620(10) Uani 1 1 d . . . H17 H -0.1447 0.0943 0.1176 0.074 Uiso 1 1 calc R . . C18 C -0.1500(4) 0.19478(17) 0.0747(3) 0.0607(9) Uani 1 1 d . . . H18 H -0.2 0.1891 0.0027 0.073 Uiso 1 1 calc R . . C19 C -0.1101(3) 0.25964(16) 0.1116(3) 0.0510(8) Uani 1 1 d . . . H19 H -0.131 0.2979 0.0637 0.061 Uiso 1 1 calc R . . C20 C 0.0742(4) 0.31743(16) -0.1558(3) 0.0570(9) Uani 1 1 d . . . H20A H 0.0729 0.2981 -0.0776 0.068 Uiso 1 1 calc R . . H20B H 0.1682 0.3177 -0.1775 0.068 Uiso 1 1 calc R . . C21 C -0.0118(6) 0.2772(2) -0.2384(5) 0.129(3) Uani 1 1 d . . . H21A H 0.0439 0.248 -0.2849 0.155 Uiso 1 1 calc R . . H21B H -0.0729 0.2477 -0.1976 0.155 Uiso 1 1 calc R . . C22 C -0.0885(7) 0.3251(3) -0.3112(5) 0.125(2) Uani 1 1 d . . . H22A H -0.1861 0.3178 -0.3063 0.15 Uiso 1 1 calc R . . H22B H -0.0679 0.3194 -0.3922 0.15 Uiso 1 1 calc R . . C23 C -0.0498(4) 0.39337(18) -0.2702(3) 0.0675(10) Uani 1 1 d . . . H23A H 0.0091 0.4155 -0.3234 0.081 Uiso 1 1 calc R . . H23B H -0.1305 0.4221 -0.2641 0.081 Uiso 1 1 calc R . . Li1 Li 0.0567(4) 0.4518(2) -0.0422(4) 0.0340(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P 0.0359(4) 0.0366(4) 0.0323(4) 0.0079(3) -0.0008(3) -0.0007(3) O 0.0688(14) 0.0356(11) 0.0402(11) -0.0051(9) -0.0102(10) 0.0086(10) N1 0.0300(11) 0.0398(12) 0.0331(12) 0.0078(10) -0.0019(9) 0.0040(9) N2 0.0288(10) 0.0306(11) 0.0307(11) 0.0033(9) -0.0020(8) -0.0006(9) C1 0.0360(14) 0.0275(13) 0.0241(12) 0.0014(10) -0.0020(10) -0.0017(11) C2 0.0309(13) 0.0470(16) 0.0402(15) 0.0135(13) -0.0002(11) 0.0036(12) C3 0.0425(17) 0.071(2) 0.059(2) 0.0096(17) -0.0183(15) -0.0016(16) C4 0.0412(16) 0.085(2) 0.0532(19) 0.0237(18) 0.0072(14) 0.0242(16) C5 0.0310(13) 0.0376(14) 0.0339(14) 0.0070(11) -0.0010(11) -0.0038(11) C6 0.0350(14) 0.0548(18) 0.0391(15) 0.0026(14) -0.0073(12) -0.0061(13) C7 0.0363(14) 0.0531(18) 0.0438(16) 0.0042(14) 0.0026(12) 0.0063(13) C8 0.0387(14) 0.0364(14) 0.0284(13) 0.0064(11) -0.0052(11) -0.0008(12) C9 0.0428(15) 0.0477(17) 0.0397(16) -0.0019(13) 0.0030(12) -0.0080(13) C10 0.0444(17) 0.065(2) 0.0440(17) 0.0004(16) 0.0042(13) -0.0085(15) C11 0.0513(18) 0.068(2) 0.0384(16) 0.0004(16) 0.0039(13) 0.0127(16) C12 0.0599(19) 0.0470(17) 0.0378(16) -0.0044(14) -0.0037(14) 0.0041(15) C13 0.0478(16) 0.0467(17) 0.0362(15) 0.0005(13) -0.0029(12) -0.0055(13) C14 0.0422(15) 0.0394(15) 0.0398(15) 0.0074(13) 0.0089(12) 0.0028(12) C15 0.068(2) 0.0406(17) 0.055(2) 0.0120(15) 0.0033(16) -0.0010(15) C16 0.089(3) 0.0396(19) 0.074(3) 0.0108(17) 0.010(2) -0.0021(18) C17 0.070(2) 0.0370(17) 0.081(3) -0.0061(17) 0.022(2) -0.0083(16) C18 0.067(2) 0.055(2) 0.059(2) -0.0155(17) 0.0027(17) -0.0018(17) C19 0.0629(19) 0.0408(16) 0.0481(18) -0.0016(14) -0.0028(15) 0.0063(15) C20 0.075(2) 0.0402(17) 0.0523(19) -0.0082(15) -0.0142(16) 0.0114(16) C21 0.181(6) 0.055(2) 0.132(4) -0.026(3) -0.108(4) 0.015(3) C22 0.186(6) 0.079(3) 0.096(4) -0.017(3) -0.081(4) 0.017(4) C23 0.103(3) 0.053(2) 0.0428(19) 0.0038(16) -0.0205(18) 0.007(2) Li1 0.038(2) 0.032(2) 0.032(2) 0.0005(18) -0.0006(18) 0.0030(18) #----------------------------------------------------------------------------# # 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 P C8 1.827(3) . ? P C14 1.831(3) . ? P C1 1.915(2) . ? O C20 1.414(4) . ? O C23 1.433(4) . ? O Li1 1.923(5) . ? N1 C1 1.316(3) . ? N1 C2 1.469(3) . ? N1 Li1 2.024(5) . ? N2 C1 1.339(3) . ? N2 C5 1.468(3) . ? N2 Li1 2.078(5) 3_565 ? N2 Li1 2.175(5) . ? C1 Li1 2.411(5) . ? C2 C4 1.516(4) . ? C2 C3 1.520(4) . ? C5 C7 1.520(4) . ? C5 C6 1.531(4) . ? C8 C9 1.391(4) . ? C8 C13 1.398(4) . ? C9 C10 1.376(4) . ? C10 C11 1.376(5) . ? C11 C12 1.376(5) . ? C12 C13 1.379(4) . ? C14 C19 1.389(4) . ? C14 C15 1.394(4) . ? C15 C16 1.367(5) . ? C16 C17 1.371(5) . ? C17 C18 1.384(5) . ? C18 C19 1.392(4) . ? C20 C21 1.470(5) . ? C21 C22 1.446(6) . ? C22 C23 1.464(6) . ? Li1 N2 2.078(5) 3_565 ? Li1 Li1 2.450(8) 3_565 ? 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 P C14 104.03(12) . . ? C8 P C1 107.13(11) . . ? C14 P C1 104.45(11) . . ? C20 O C23 107.6(2) . . ? C20 O Li1 124.6(2) . . ? C23 O Li1 127.4(2) . . ? C1 N1 C2 122.5(2) . . ? C1 N1 Li1 89.83(19) . . ? C2 N1 Li1 146.2(2) . . ? C1 N2 C5 121.9(2) . . ? C1 N2 Li1 127.4(2) . 3_565 ? C5 N2 Li1 109.28(19) . 3_565 ? C1 N2 Li1 83.00(18) . . ? C5 N2 Li1 132.58(19) . . ? Li1 N2 Li1 70.30(19) 3_565 . ? N1 C1 N2 117.3(2) . . ? N1 C1 P 115.80(18) . . ? N2 C1 P 126.70(18) . . ? N1 C1 Li1 57.09(16) . . ? N2 C1 Li1 63.54(16) . . ? P C1 Li1 163.52(16) . . ? N1 C2 C4 108.7(2) . . ? N1 C2 C3 110.8(2) . . ? C4 C2 C3 110.8(3) . . ? N2 C5 C7 110.9(2) . . ? N2 C5 C6 109.0(2) . . ? C7 C5 C6 109.7(2) . . ? C9 C8 C13 117.4(3) . . ? C9 C8 P 125.2(2) . . ? C13 C8 P 116.9(2) . . ? C10 C9 C8 121.1(3) . . ? C9 C10 C11 120.9(3) . . ? C10 C11 C12 118.9(3) . . ? C11 C12 C13 120.7(3) . . ? C12 C13 C8 120.9(3) . . ? C19 C14 C15 117.6(3) . . ? C19 C14 P 125.2(2) . . ? C15 C14 P 117.2(2) . . ? C16 C15 C14 122.1(3) . . ? C15 C16 C17 119.9(3) . . ? C16 C17 C18 119.8(3) . . ? C17 C18 C19 120.2(3) . . ? C14 C19 C18 120.4(3) . . ? O C20 C21 106.0(3) . . ? C22 C21 C20 107.0(4) . . ? C21 C22 C23 106.8(3) . . ? O C23 C22 106.1(3) . . ? O Li1 N1 113.3(2) . . ? O Li1 N2 115.9(2) . 3_565 ? N1 Li1 N2 126.0(2) . 3_565 ? O Li1 N2 115.5(2) . . ? N1 Li1 N2 65.28(15) . . ? N2 Li1 N2 109.70(19) 3_565 . ? O Li1 C1 112.6(2) . . ? N1 Li1 C1 33.08(10) . . ? N2 Li1 C1 129.9(2) 3_565 . ? N2 Li1 C1 33.46(10) . . ? O Li1 Li1 138.9(3) . 3_565 ? N1 Li1 Li1 97.3(2) . 3_565 ? N2 Li1 Li1 56.69(17) 3_565 3_565 ? N2 Li1 Li1 53.01(17) . 3_565 ? C1 Li1 Li1 78.7(2) . 3_565 ? #===END data_mar402 _database_code_depnum_ccdc_archive 'CCDC 182914' _audit_creation_date 2002-03-16T16:05:32-00:00 _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_COMMON ; '[Li(tmeda){Ph2PC(NiPr)2}]' ; _chemical_formula_moiety 'C24 H40 Li1 N4 P1' _chemical_formula_sum 'C25 H40 Li N4 P' _chemical_formula_weight 434.52 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5099(2) _cell_length_b 11.9348(2) _cell_length_c 28.6122(6) _cell_angle_alpha 98.125(1) _cell_angle_beta 75.908(1) _cell_angle_gamma 122.665(3) _cell_volume 2651.37(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 27799 _cell_measurement_theta_min 4 _cell_measurement_theta_max 23 _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 0.2 _exptl_crystal_density_diffrn 1.089 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.121 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0653 _diffrn_reflns_av_unetI/netI 0.0536 _diffrn_reflns_number 22110 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 23.06 _diffrn_reflns_theta_full 23.06 _diffrn_measured_fraction_theta_full 0.975 _diffrn_measured_fraction_theta_max 0.975 _reflns_number_total 7271 _reflns_number_gt 5713 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _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^)+(0.0764P)^2^+2.2163P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 7271 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0813 _refine_ls_R_factor_gt 0.0579 _refine_ls_wR_factor_ref 0.1562 _refine_ls_wR_factor_gt 0.141 _refine_ls_goodness_of_fit_ref 1.04 _refine_ls_restrained_S_all 1.04 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.394 _refine_diff_density_min -0.288 _refine_diff_density_rms 0.056 #----------------------------------------------------------------------------# # 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' Li Li -0.0003 0.0001 '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' 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 Li Li 0.6824(6) -0.2031(5) 0.36647(19) 0.0362(12) Uani 1 1 d . A 1 P P 0.86780(9) 0.01994(7) 0.41104(3) 0.0274(2) Uani 1 1 d . A 1 N1 N 0.6636(3) -0.0585(2) 0.35298(8) 0.0278(6) Uani 1 1 d . A 1 N2 N 0.7502(3) 0.1652(2) 0.37519(9) 0.0313(6) Uani 1 1 d . A 1 N3 N 0.8231(3) -0.2766(3) 0.31921(9) 0.0420(7) Uani 1 1 d . A 1 N4 N 0.5364(4) -0.3857(3) 0.40107(10) 0.0469(7) Uani 1 1 d . A 1 C1 C 0.7512(3) 0.0573(3) 0.37673(10) 0.0276(7) Uani 1 1 d . A 1 C2 C 0.5746(4) -0.0542(3) 0.31847(11) 0.0324(7) Uani 1 1 d . A 1 H2 H 0.5051 -0.0148 0.3349 0.039 Uiso 1 1 calc R A 1 C3 C 0.7009(4) 0.0305(3) 0.27507(12) 0.0465(9) Uani 1 1 d . A 1 H3A H 0.7754 0.1216 0.2859 0.07 Uiso 1 1 calc R A 1 H3B H 0.6384 0.0314 0.2526 0.07 Uiso 1 1 calc R A 1 H3C H 0.7699 -0.0072 0.2588 0.07 Uiso 1 1 calc R A 1 C4 C 0.4556(4) -0.1965(3) 0.30300(12) 0.0409(8) Uani 1 1 d . A 1 H4A H 0.3754 -0.2489 0.3314 0.061 Uiso 1 1 calc R A 1 H4B H 0.5226 -0.236 0.2869 0.061 Uiso 1 1 calc R A 1 H4C H 0.392 -0.1964 0.2807 0.061 Uiso 1 1 calc R A 1 C5 C 0.8654(4) 0.2895(3) 0.39725(11) 0.0329(7) Uani 1 1 d . A 1 H5 H 0.9548 0.2815 0.4062 0.04 Uiso 1 1 calc R A 1 C6 C 0.7681(4) 0.3219(3) 0.44229(12) 0.0446(8) Uani 1 1 d . A 1 H6A H 0.7148 0.2509 0.4658 0.067 Uiso 1 1 calc R A 1 H6B H 0.6797 0.3291 0.4336 0.067 Uiso 1 1 calc R A 1 H6C H 0.8473 0.4065 0.4563 0.067 Uiso 1 1 calc R A 1 C7 C 0.9497(5) 0.3994(3) 0.36050(13) 0.0496(9) Uani 1 1 d . A 1 H7A H 1.0122 0.3781 0.3318 0.074 Uiso 1 1 calc R A 1 H7B H 1.029 0.484 0.3745 0.074 Uiso 1 1 calc R A 1 H7C H 0.8621 0.4071 0.3515 0.074 Uiso 1 1 calc R A 1 C8 C 0.8630(4) 0.0988(3) 0.47079(10) 0.0287(7) Uani 1 1 d . A 1 C9 C 0.7073(4) 0.0362(3) 0.50318(11) 0.0368(8) Uani 1 1 d . A 1 H9 H 0.6148 -0.0444 0.4937 0.044 Uiso 1 1 calc R A 1 C10 C 0.6837(4) 0.0884(4) 0.54888(11) 0.0446(9) Uani 1 1 d . A 1 H10 H 0.5757 0.0454 0.5701 0.053 Uiso 1 1 calc R A 1 C11 C 0.8193(5) 0.2035(4) 0.56284(12) 0.0492(9) Uani 1 1 d . A 1 H11 H 0.8048 0.2411 0.5939 0.059 Uiso 1 1 calc R A 1 C12 C 0.9765(5) 0.2647(4) 0.53200(12) 0.0473(9) Uani 1 1 d . A 1 H12 H 1.0702 0.3427 0.5423 0.057 Uiso 1 1 calc R A 1 C13 C 0.9987(4) 0.2133(3) 0.48615(11) 0.0367(8) Uani 1 1 d . A 1 H13 H 1.1072 0.2566 0.4651 0.044 Uiso 1 1 calc R A 1 C14 C 1.0904(4) 0.1118(3) 0.37994(10) 0.0276(7) Uani 1 1 d . A 1 C15 C 1.1397(4) 0.1657(3) 0.33451(11) 0.0331(7) Uani 1 1 d . A 1 H15 H 1.0601 0.17 0.3214 0.04 Uiso 1 1 calc R A 1 C16 C 1.3044(4) 0.2133(3) 0.30838(12) 0.0402(8) Uani 1 1 d . A 1 H16 H 1.3369 0.2498 0.2774 0.048 Uiso 1 1 calc R A 1 C17 C 1.4215(4) 0.2080(3) 0.32705(12) 0.0424(8) Uani 1 1 d . A 1 H17 H 1.5334 0.2393 0.3087 0.051 Uiso 1 1 calc R A 1 C18 C 1.3759(4) 0.1571(3) 0.37251(12) 0.0379(8) Uani 1 1 d . A 1 H18 H 1.4572 0.1559 0.3859 0.046 Uiso 1 1 calc R A 1 C19 C 1.2112(4) 0.1081(3) 0.39827(11) 0.0334(7) Uani 1 1 d . A 1 H19 H 1.1794 0.071 0.4291 0.04 Uiso 1 1 calc R A 1 C20 C 0.7131(5) -0.4194(3) 0.32813(13) 0.0529(9) Uani 1 1 d . A 1 H20A H 0.7798 -0.4625 0.3161 0.064 Uiso 1 1 calc R A 1 H20B H 0.6192 -0.4584 0.3103 0.064 Uiso 1 1 calc R A 1 C21 C 0.6388(5) -0.4471(4) 0.38146(14) 0.0553(10) Uani 1 1 d . A 1 H21A H 0.5661 -0.5444 0.3864 0.066 Uiso 1 1 calc R A 1 H21B H 0.7326 -0.4113 0.3991 0.066 Uiso 1 1 calc R A 1 C22 C 0.8535(6) -0.2487(5) 0.26809(13) 0.0658(11) Uani 1 1 d . A 1 H22A H 0.9274 -0.1525 0.2629 0.099 Uiso 1 1 calc R A 1 H22B H 0.7445 -0.2813 0.259 0.099 Uiso 1 1 calc R A 1 H22C H 0.9089 -0.2936 0.2483 0.099 Uiso 1 1 calc R A 1 C23 C 0.9873(5) -0.2202(4) 0.33288(15) 0.0608(11) Uani 1 1 d . A 1 H23A H 1.0568 -0.1243 0.3267 0.091 Uiso 1 1 calc R A 1 H23B H 1.0466 -0.2632 0.3139 0.091 Uiso 1 1 calc R A 1 H23C H 0.9688 -0.2351 0.3672 0.091 Uiso 1 1 calc R A 1 C24 C 0.5167(6) -0.3736(5) 0.45344(14) 0.0750(13) Uani 1 1 d . A 1 H24A H 0.449 -0.3327 0.4662 0.113 Uiso 1 1 calc R A 1 H24B H 0.6293 -0.3178 0.4619 0.113 Uiso 1 1 calc R A 1 H24C H 0.4585 -0.4621 0.4673 0.113 Uiso 1 1 calc R A 1 C25 C 0.3687(5) -0.4650(4) 0.38798(18) 0.0728(13) Uani 1 1 d . A 1 H25A H 0.3828 -0.4726 0.3528 0.109 Uiso 1 1 calc R A 1 H25B H 0.3042 -0.4215 0.4006 0.109 Uiso 1 1 calc R A 1 H25C H 0.3068 -0.554 0.4018 0.109 Uiso 1 1 calc R A 1 Li1B Li 1.0200(6) -0.6032(5) 0.12411(19) 0.0367(12) Uani 1 1 d . B 2 P1B P 1.26544(9) -0.36589(7) 0.09508(3) 0.0271(2) Uani 1 1 d . B 2 N1B N 1.2285(3) -0.5434(2) 0.14620(8) 0.0278(6) Uani 1 1 d . B 2 N2B N 1.5200(3) -0.3744(2) 0.13055(9) 0.0312(6) Uani 1 1 d . B 2 N3B N 0.7942(3) -0.6142(3) 0.15971(10) 0.0421(7) Uani 1 1 d . B 2 N4B N 0.8795(3) -0.7531(3) 0.07801(10) 0.0433(7) Uani 1 1 d . B 2 C1B C 1.3631(4) -0.4269(3) 0.12715(10) 0.0267(7) Uani 1 1 d . B 2 C2B C 1.2663(4) -0.6054(3) 0.17840(11) 0.0349(7) Uani 1 1 d . B 2 H2B H 1.3712 -0.6066 0.1621 0.042 Uiso 1 1 calc R B 2 C3B C 1.2971(5) -0.5269(4) 0.22602(12) 0.0550(10) Uani 1 1 d . B 2 H3B1 H 1.3941 -0.4357 0.2194 0.083 Uiso 1 1 calc R B 2 H3B2 H 1.3218 -0.57 0.2468 0.083 Uiso 1 1 calc R B 2 H3B3 H 1.195 -0.5248 0.2422 0.083 Uiso 1 1 calc R B 2 C4B C 1.1173(4) -0.7478(3) 0.18742(13) 0.0479(9) Uani 1 1 d . B 2 H4B1 H 1.1005 -0.7963 0.1566 0.072 Uiso 1 1 calc R B 2 H4B2 H 1.0138 -0.7476 0.2033 0.072 Uiso 1 1 calc R B 2 H4B3 H 1.1417 -0.7915 0.2081 0.072 Uiso 1 1 calc R B 2 C5B C 1.6540(4) -0.2415(3) 0.11357(10) 0.0307(7) Uani 1 1 d . B 2 H5B H 1.6017 -0.1956 0.1049 0.037 Uiso 1 1 calc R B 2 C6B C 1.7769(4) -0.2484(3) 0.06940(12) 0.0417(8) Uani 1 1 d . B 2 H6B1 H 1.7149 -0.2972 0.0434 0.063 Uiso 1 1 calc R B 2 H6B2 H 1.8272 -0.2943 0.0776 0.063 Uiso 1 1 calc R B 2 H6B3 H 1.8675 -0.158 0.0588 0.063 Uiso 1 1 calc R B 2 C7B C 1.7480(4) -0.1646(3) 0.15432(12) 0.0442(8) Uani 1 1 d . B 2 H7B1 H 1.6677 -0.1604 0.1824 0.066 Uiso 1 1 calc R B 2 H7B2 H 1.8384 -0.0741 0.1437 0.066 Uiso 1 1 calc R B 2 H7B3 H 1.7985 -0.2098 0.1631 0.066 Uiso 1 1 calc R B 2 C8B C 1.4092(4) -0.2997(3) 0.03701(10) 0.0285(7) Uani 1 1 d . B 2 C9B C 1.4135(4) -0.3947(3) 0.00300(11) 0.0335(7) Uani 1 1 d . B 2 H9B H 1.3449 -0.4861 0.0114 0.04 Uiso 1 1 calc R B 2 C10B C 1.5152(4) -0.3588(3) -0.04258(11) 0.0392(8) Uani 1 1 d . B 2 H10B H 1.5167 -0.4248 -0.0652 0.047 Uiso 1 1 calc R B 2 C11B C 1.6144(4) -0.2260(3) -0.05488(11) 0.0415(8) Uani 1 1 d . B 2 H11B H 1.6861 -0.2001 -0.0859 0.05 Uiso 1 1 calc R B 2 C12B C 1.6095(4) -0.1307(3) -0.02195(11) 0.0419(8) Uani 1 1 d . B 2 H12B H 1.6764 -0.0395 -0.0307 0.05 Uiso 1 1 calc R B 2 C13B C 1.5078(4) -0.1671(3) 0.02355(11) 0.0332(7) Uani 1 1 d . B 2 H13B H 1.5053 -0.1008 0.0458 0.04 Uiso 1 1 calc R B 2 C14B C 1.2779(3) -0.2214(3) 0.13020(10) 0.0271(7) Uani 1 1 d . B 2 C15B C 1.3298(4) -0.1844(3) 0.17440(11) 0.0340(7) Uani 1 1 d . B 2 H15B H 1.3736 -0.2287 0.1854 0.041 Uiso 1 1 calc R B 2 C16B C 1.3183(4) -0.0834(3) 0.20251(12) 0.0432(8) Uani 1 1 d . B 2 H16B H 1.3535 -0.0596 0.2326 0.052 Uiso 1 1 calc R B 2 C17B C 1.2557(4) -0.0177(3) 0.18662(13) 0.0443(9) Uani 1 1 d . B 2 H17B H 1.2493 0.0521 0.2055 0.053 Uiso 1 1 calc R B 2 C18B C 1.2027(4) -0.0539(3) 0.14322(12) 0.0405(8) Uani 1 1 d . B 2 H18B H 1.1595 -0.009 0.1322 0.049 Uiso 1 1 calc R B 2 C19B C 1.2122(4) -0.1554(3) 0.11565(11) 0.0354(7) Uani 1 1 d . B 2 H19B H 1.173 -0.1806 0.0861 0.042 Uiso 1 1 calc R B 2 C20B C 0.6698(5) -0.7077(4) 0.13000(16) 0.0637(11) Uani 1 1 d . B 2 H20C H 0.5546 -0.7526 0.1508 0.076 Uiso 1 1 calc R B 2 H20D H 0.6695 -0.6568 0.1056 0.076 Uiso 1 1 calc R B 2 C21B C 0.7048(5) -0.8091(4) 0.10535(17) 0.0725(13) Uani 1 1 d . B 2 H21C H 0.6831 -0.871 0.1296 0.087 Uiso 1 1 calc R B 2 H21D H 0.625 -0.8611 0.0831 0.087 Uiso 1 1 calc R B 2 C22B C 0.7478(7) -0.6631(7) 0.20792(16) 0.108(2) Uani 1 1 d . B 2 H22D H 0.8344 -0.5989 0.2264 0.162 Uiso 1 1 calc R B 2 H22E H 0.7404 -0.7487 0.2062 0.162 Uiso 1 1 calc R B 2 H22F H 0.637 -0.675 0.2238 0.162 Uiso 1 1 calc R B 2 C23B C 0.8046(6) -0.4862(4) 0.1616(2) 0.0801(14) Uani 1 1 d . B 2 H23D H 0.8351 -0.4544 0.1287 0.12 Uiso 1 1 calc R B 2 H23E H 0.8917 -0.4209 0.1797 0.12 Uiso 1 1 calc R B 2 H23F H 0.6939 -0.498 0.1775 0.12 Uiso 1 1 calc R B 2 C24B C 0.9002(6) -0.6952(5) 0.03287(15) 0.0771(13) Uani 1 1 d . B 2 H24D H 1.0183 -0.6565 0.0152 0.116 Uiso 1 1 calc R B 2 H24E H 0.8728 -0.6256 0.0403 0.116 Uiso 1 1 calc R B 2 H24F H 0.8232 -0.7649 0.0131 0.116 Uiso 1 1 calc R B 2 C25B C 0.9217(6) -0.8571(4) 0.06528(18) 0.0751(13) Uani 1 1 d . B 2 H25D H 1.0389 -0.8177 0.0468 0.113 Uiso 1 1 calc R B 2 H25E H 0.843 -0.9265 0.0458 0.113 Uiso 1 1 calc R B 2 H25F H 0.9113 -0.8962 0.0948 0.113 Uiso 1 1 calc R 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 Li 0.039(3) 0.035(3) 0.039(3) 0.001(2) -0.006(2) 0.024(2) P 0.0274(4) 0.0295(4) 0.0271(4) 0.0004(3) -0.0072(3) 0.0154(4) N1 0.0283(13) 0.0314(14) 0.0265(13) -0.0021(11) -0.0085(11) 0.0170(11) N2 0.0312(14) 0.0316(14) 0.0361(15) -0.0018(11) -0.0086(11) 0.0195(12) N3 0.0469(17) 0.0460(16) 0.0398(16) -0.0053(13) -0.0078(13) 0.0304(14) N4 0.0498(18) 0.0386(16) 0.0500(18) 0.0076(14) -0.0100(14) 0.0202(14) C1 0.0229(15) 0.0350(17) 0.0234(15) 0.0029(13) -0.0003(13) 0.0155(14) C2 0.0361(17) 0.0364(17) 0.0324(17) -0.0037(14) -0.0139(14) 0.0222(15) C3 0.052(2) 0.051(2) 0.0363(19) 0.0062(16) -0.0130(17) 0.0242(18) C4 0.0421(19) 0.0458(19) 0.0375(19) -0.0031(15) -0.0164(16) 0.0224(16) C5 0.0350(17) 0.0286(16) 0.0415(18) -0.0004(14) -0.0105(14) 0.0197(14) C6 0.054(2) 0.0412(19) 0.047(2) -0.0094(16) -0.0157(17) 0.0309(17) C7 0.050(2) 0.0376(19) 0.062(2) 0.0064(17) -0.0145(18) 0.0208(17) C8 0.0278(16) 0.0380(17) 0.0269(16) 0.0048(13) -0.0034(13) 0.0214(15) C9 0.0360(18) 0.0475(19) 0.0326(18) 0.0073(15) -0.0079(15) 0.0237(16) C10 0.046(2) 0.074(3) 0.0273(18) 0.0096(17) 0.0009(16) 0.041(2) C11 0.066(3) 0.078(3) 0.0256(18) -0.0087(18) -0.0102(18) 0.054(2) C12 0.058(2) 0.053(2) 0.037(2) -0.0129(17) -0.0217(18) 0.0315(19) C13 0.0377(18) 0.0407(18) 0.0332(18) -0.0003(15) -0.0106(15) 0.0204(16) C14 0.0300(16) 0.0267(15) 0.0292(17) -0.0048(13) -0.0072(13) 0.0176(13) C15 0.0327(17) 0.0377(17) 0.0335(18) 0.0014(14) -0.0055(14) 0.0216(15) C16 0.0403(19) 0.0440(19) 0.0357(18) 0.0070(15) 0.0016(15) 0.0239(16) C17 0.0331(18) 0.0425(19) 0.047(2) -0.0002(16) 0.0028(16) 0.0217(16) C18 0.0328(18) 0.0417(18) 0.049(2) -0.0073(16) -0.0131(16) 0.0255(16) C19 0.0360(18) 0.0362(17) 0.0352(17) -0.0031(14) -0.0109(15) 0.0229(15) C20 0.065(2) 0.047(2) 0.058(2) -0.0123(18) -0.016(2) 0.039(2) C21 0.073(3) 0.041(2) 0.068(3) 0.0018(18) -0.022(2) 0.038(2) C22 0.074(3) 0.085(3) 0.044(2) -0.001(2) 0.004(2) 0.051(3) C23 0.052(2) 0.067(3) 0.072(3) -0.016(2) -0.017(2) 0.039(2) C24 0.095(3) 0.081(3) 0.048(3) 0.018(2) 0.005(2) 0.049(3) C25 0.043(2) 0.057(3) 0.106(4) 0.020(2) -0.009(2) 0.016(2) Li1B 0.031(3) 0.033(3) 0.040(3) 0.002(2) -0.005(2) 0.013(2) P1B 0.0276(4) 0.0268(4) 0.0269(4) 0.0036(3) -0.0057(3) 0.0135(3) N1B 0.0317(14) 0.0284(13) 0.0264(13) 0.0049(11) -0.0037(11) 0.0175(12) N2B 0.0300(14) 0.0326(14) 0.0328(14) 0.0013(11) -0.0073(11) 0.0171(12) N3B 0.0394(16) 0.0457(16) 0.0418(16) -0.0004(13) -0.0047(13) 0.0243(14) N4B 0.0344(15) 0.0408(16) 0.0508(18) -0.0079(13) -0.0092(13) 0.0189(13) C1B 0.0319(18) 0.0284(16) 0.0215(15) -0.0001(12) -0.0031(13) 0.0179(14) C2B 0.0387(18) 0.0373(17) 0.0311(17) 0.0089(14) -0.0016(14) 0.0218(15) C3B 0.079(3) 0.059(2) 0.037(2) 0.0070(18) -0.0157(19) 0.040(2) C4B 0.049(2) 0.0416(19) 0.058(2) 0.0209(17) -0.0019(17) 0.0253(17) C5B 0.0279(16) 0.0308(16) 0.0317(17) 0.0024(13) -0.0073(13) 0.0134(14) C6B 0.0350(18) 0.047(2) 0.0409(19) 0.0033(16) -0.0017(15) 0.0218(16) C7B 0.0384(19) 0.0425(19) 0.047(2) -0.0037(16) -0.0163(16) 0.0164(16) C8B 0.0307(16) 0.0335(16) 0.0257(16) 0.0000(13) -0.0087(13) 0.0186(14) C9B 0.0382(18) 0.0337(17) 0.0342(18) 0.0031(14) -0.0069(15) 0.0221(15) C10B 0.054(2) 0.046(2) 0.0280(18) -0.0046(15) -0.0078(16) 0.0347(18) C11B 0.0428(19) 0.053(2) 0.0264(17) 0.0076(16) -0.0005(15) 0.0246(17) C12B 0.0433(19) 0.0391(19) 0.0338(19) 0.0102(15) -0.0023(16) 0.0155(16) C13B 0.0362(17) 0.0287(16) 0.0298(17) 0.0013(13) -0.0080(14) 0.0132(14) C14B 0.0215(15) 0.0276(15) 0.0300(16) 0.0064(13) -0.0003(12) 0.0121(13) C15B 0.0370(17) 0.0400(18) 0.0308(17) -0.0008(14) -0.0061(14) 0.0245(15) C16B 0.049(2) 0.051(2) 0.0350(19) -0.0094(16) -0.0094(16) 0.0317(18) C17B 0.043(2) 0.0361(18) 0.051(2) -0.0004(16) 0.0036(17) 0.0249(17) C18B 0.0387(19) 0.0374(18) 0.054(2) 0.0097(16) -0.0029(16) 0.0258(16) C19B 0.0333(17) 0.0366(18) 0.0379(18) 0.0076(15) -0.0033(14) 0.0193(15) C20B 0.034(2) 0.064(3) 0.079(3) -0.018(2) -0.012(2) 0.0202(19) C21B 0.039(2) 0.061(3) 0.089(3) -0.023(2) -0.011(2) 0.014(2) C22B 0.101(4) 0.207(7) 0.045(3) 0.042(3) 0.025(3) 0.107(5) C23B 0.060(3) 0.063(3) 0.123(4) -0.013(3) -0.012(3) 0.043(2) C24B 0.083(3) 0.096(3) 0.053(3) -0.009(2) -0.029(2) 0.043(3) C25B 0.071(3) 0.062(3) 0.100(4) -0.028(2) -0.034(3) 0.040(2) #----------------------------------------------------------------------------# # 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 Li N1 1.927(5) . ? Li N4 2.081(6) . ? Li N3 2.107(6) . ? Li P 2.625(5) . ? P C14 1.825(3) . ? P C8 1.834(3) . ? P C1 1.892(3) . ? N1 C1 1.354(4) . ? N1 C2 1.470(4) . ? N2 C1 1.299(4) . ? N2 C5 1.455(4) . ? N3 C20 1.461(4) . ? N3 C23 1.461(4) . ? N3 C22 1.470(5) . ? N4 C24 1.460(5) . ? N4 C25 1.463(5) . ? N4 C21 1.478(5) . ? C2 C4 1.523(4) . ? C2 C3 1.524(4) . ? C5 C7 1.522(4) . ? C5 C6 1.527(4) . ? C8 C13 1.389(4) . ? C8 C9 1.394(4) . ? C9 C10 1.388(5) . ? C10 C11 1.376(5) . ? C11 C12 1.382(5) . ? C12 C13 1.385(5) . ? C14 C15 1.392(4) . ? C14 C19 1.396(4) . ? C15 C16 1.388(4) . ? C16 C17 1.380(5) . ? C17 C18 1.383(5) . ? C18 C19 1.382(4) . ? C20 C21 1.517(5) . ? Li1B N1B 1.948(5) . ? Li1B N3B 2.082(6) . ? Li1B N4B 2.082(6) . ? Li1B P1B 2.597(5) . ? Li1B C1B 2.785(6) . ? Li1B C21B 2.788(6) . ? P1B C14B 1.829(3) . ? P1B C8B 1.831(3) . ? P1B C1B 1.888(3) . ? N1B C1B 1.350(4) . ? N1B C2B 1.472(4) . ? N2B C1B 1.294(4) . ? N2B C5B 1.453(4) . ? N3B C22B 1.446(5) . ? N3B C20B 1.471(5) . ? N3B C23B 1.471(5) . ? N4B C21B 1.461(5) . ? N4B C24B 1.472(5) . ? N4B C25B 1.474(5) . ? C2B C4B 1.520(4) . ? C2B C3B 1.535(5) . ? C5B C7B 1.523(4) . ? C5B C6B 1.525(4) . ? C8B C13B 1.388(4) . ? C8B C9B 1.397(4) . ? C9B C10B 1.384(4) . ? C10B C11B 1.381(5) . ? C11B C12B 1.385(5) . ? C12B C13B 1.383(4) . ? C14B C19B 1.391(4) . ? C14B C15B 1.396(4) . ? C15B C16B 1.391(4) . ? C16B C17B 1.383(5) . ? C17B C18B 1.379(5) . ? C18B C19B 1.382(4) . ? C20B C21B 1.468(5) . ? 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 N1 Li N4 140.3(3) . . ? N1 Li N3 125.3(3) . . ? N4 Li N3 88.4(2) . . ? N1 Li P 66.54(16) . . ? N4 Li P 122.1(2) . . ? N3 Li P 114.4(2) . . ? C14 P C8 105.43(13) . . ? C14 P C1 105.06(13) . . ? C8 P C1 107.82(13) . . ? C14 P Li 112.64(14) . . ? C8 P Li 139.88(15) . . ? C1 P Li 74.49(14) . . ? C1 N1 C2 115.2(2) . . ? C1 N1 Li 115.7(2) . . ? C2 N1 Li 128.9(2) . . ? C1 N2 C5 121.9(2) . . ? C20 N3 C23 111.9(3) . . ? C20 N3 C22 110.8(3) . . ? C23 N3 C22 108.7(3) . . ? C20 N3 Li 101.6(2) . . ? C23 N3 Li 109.2(3) . . ? C22 N3 Li 114.4(3) . . ? C24 N4 C25 109.9(3) . . ? C24 N4 C21 109.8(3) . . ? C25 N4 C21 110.8(3) . . ? C24 N4 Li 113.4(3) . . ? C25 N4 Li 110.7(3) . . ? C21 N4 Li 102.0(2) . . ? N2 C1 N1 126.4(3) . . ? N2 C1 P 130.5(2) . . ? N1 C1 P 103.12(19) . . ? N1 C2 C4 108.0(2) . . ? N1 C2 C3 111.1(2) . . ? C4 C2 C3 110.9(3) . . ? N2 C5 C7 108.2(3) . . ? N2 C5 C6 110.7(2) . . ? C7 C5 C6 110.0(3) . . ? C13 C8 C9 118.1(3) . . ? C13 C8 P 126.1(2) . . ? C9 C8 P 115.8(2) . . ? C10 C9 C8 121.9(3) . . ? C11 C10 C9 118.8(3) . . ? C10 C11 C12 120.4(3) . . ? C11 C12 C13 120.6(3) . . ? C12 C13 C8 120.2(3) . . ? C15 C14 C19 118.3(3) . . ? C15 C14 P 122.1(2) . . ? C19 C14 P 118.7(2) . . ? C16 C15 C14 120.3(3) . . ? C17 C16 C15 120.5(3) . . ? C16 C17 C18 120.0(3) . . ? C19 C18 C17 119.4(3) . . ? C18 C19 C14 121.5(3) . . ? N3 C20 C21 111.2(3) . . ? N4 C21 C20 111.4(3) . . ? N1B Li1B N3B 131.2(3) . . ? N1B Li1B N4B 135.2(3) . . ? N3B Li1B N4B 87.6(2) . . ? N1B Li1B P1B 66.94(16) . . ? N3B Li1B P1B 113.9(2) . . ? N4B Li1B P1B 123.1(2) . . ? N1B Li1B C1B 26.30(11) . . ? N3B Li1B C1B 134.5(2) . . ? N4B Li1B C1B 136.9(2) . . ? P1B Li1B C1B 40.90(9) . . ? N1B Li1B C21B 149.9(3) . . ? N3B Li1B C21B 58.49(16) . . ? N4B Li1B C21B 30.80(13) . . ? P1B Li1B C21B 140.7(2) . . ? C1B Li1B C21B 167.0(2) . . ? C14B P1B C8B 105.39(13) . . ? C14B P1B C1B 105.22(13) . . ? C8B P1B C1B 107.37(12) . . ? C14B P1B Li1B 119.23(14) . . ? C8B P1B Li1B 133.29(15) . . ? C1B P1B Li1B 74.90(14) . . ? C1B N1B C2B 114.6(2) . . ? C1B N1B Li1B 114.0(2) . . ? C2B N1B Li1B 131.4(2) . . ? C1B N2B C5B 122.6(2) . . ? C22B N3B C20B 112.0(4) . . ? C22B N3B C23B 110.2(4) . . ? C20B N3B C23B 108.2(3) . . ? C22B N3B Li1B 109.4(3) . . ? C20B N3B Li1B 104.0(2) . . ? C23B N3B Li1B 113.0(3) . . ? C21B N4B C24B 110.3(3) . . ? C21B N4B C25B 110.8(3) . . ? C24B N4B C25B 107.7(3) . . ? C21B N4B Li1B 102.3(3) . . ? C24B N4B Li1B 110.1(3) . . ? C25B N4B Li1B 115.5(3) . . ? N2B C1B N1B 126.4(3) . . ? N2B C1B P1B 130.2(2) . . ? N1B C1B P1B 103.43(19) . . ? N2B C1B Li1B 164.4(2) . . ? N1B C1B Li1B 39.73(16) . . ? P1B C1B Li1B 64.20(13) . . ? N1B C2B C4B 108.3(3) . . ? N1B C2B C3B 110.9(3) . . ? C4B C2B C3B 110.8(3) . . ? N2B C5B C7B 108.1(2) . . ? N2B C5B C6B 110.5(2) . . ? C7B C5B C6B 110.4(3) . . ? C13B C8B C9B 118.1(3) . . ? C13B C8B P1B 126.5(2) . . ? C9B C8B P1B 115.4(2) . . ? C10B C9B C8B 121.6(3) . . ? C11B C10B C9B 119.3(3) . . ? C10B C11B C12B 119.9(3) . . ? C13B C12B C11B 120.5(3) . . ? C12B C13B C8B 120.6(3) . . ? C19B C14B C15B 117.8(3) . . ? C19B C14B P1B 118.7(2) . . ? C15B C14B P1B 123.0(2) . . ? C16B C15B C14B 120.9(3) . . ? C17B C16B C15B 120.0(3) . . ? C18B C17B C16B 119.8(3) . . ? C17B C18B C19B 120.1(3) . . ? C18B C19B C14B 121.4(3) . . ? C21B C20B N3B 113.5(3) . . ? N4B C21B C20B 113.2(3) . . ? N4B C21B Li1B 46.86(19) . . ? C20B C21B Li1B 76.2(2) . . ? #===END data_jan202 _database_code_depnum_ccdc_archive 'CCDC 193950' _audit_creation_date 2002-01-04T11:46:07-00:00 _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_name_common '[AlMe2{(NiPr)2CPPh2}]' _chemical_formula_moiety 'C21 H30 Al1 N2 P1' _chemical_formula_sum 'C21 H30 Al N2 P' _chemical_formula_weight 368.42 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _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 16.0218(9) _cell_length_b 8.3303(6) _cell_length_c 17.6419(9) _cell_angle_alpha 90 _cell_angle_beta 107.443(4) _cell_angle_gamma 90 _cell_volume 2246.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10071 _cell_measurement_theta_min 4.076 _cell_measurement_theta_max 22.986 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.089 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.167 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _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_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_unetI/netI 0.0438 _diffrn_reflns_number 9341 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 4.23 _diffrn_reflns_theta_max 23.02 _diffrn_reflns_theta_full 23.02 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _reflns_number_total 3095 _reflns_number_gt 2623 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _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^)+(0.0357P)^2^+1.4909P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 3095 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0516 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.1009 _refine_ls_wR_factor_gt 0.0957 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.255 _refine_diff_density_min -0.259 _refine_diff_density_rms 0.038 #===END #----------------------------------------------------------------------------# # ATOMIC COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 P P 0.98914(4) 0.15778(7) 0.32931(3) 0.02849(19) Uani 1 1 d . . . Al Al 1.05867(5) 0.46187(9) 0.16642(4) 0.0357(2) Uani 1 1 d . . . N1 N 1.02252(13) 0.2512(2) 0.18913(11) 0.0343(5) Uani 1 1 d . . . N2 N 1.05219(12) 0.4498(2) 0.27359(11) 0.0325(5) Uani 1 1 d . . . C1 C 1.02517(14) 0.2975(3) 0.26236(13) 0.0288(5) Uani 1 1 d . . . C2 C 1.00808(15) 0.0882(3) 0.15664(13) 0.0346(6) Uani 1 1 d . . . H2 H 0.9831 0.0209 0.1914 0.042 Uiso 1 1 calc R . . C3 C 1.09435(18) 0.0165(4) 0.15517(18) 0.0588(8) Uani 1 1 d . . . H3A H 1.1346 0.0129 0.2093 0.088 Uiso 1 1 calc R . . H3B H 1.1197 0.0826 0.1217 0.088 Uiso 1 1 calc R . . H3C H 1.0846 -0.0927 0.1335 0.088 Uiso 1 1 calc R . . C4 C 0.94334(17) 0.0945(3) 0.07401(15) 0.0488(7) Uani 1 1 d . . . H4A H 0.8879 0.1399 0.0769 0.073 Uiso 1 1 calc R . . H4B H 0.9333 -0.0143 0.0520 0.073 Uiso 1 1 calc R . . H4C H 0.9670 0.1619 0.0398 0.073 Uiso 1 1 calc R . . C5 C 1.05883(17) 0.5499(3) 0.34315(14) 0.0381(6) Uani 1 1 d . . . H5 H 1.0251 0.4989 0.3761 0.046 Uiso 1 1 calc R . . C6 C 1.0197(2) 0.7134(3) 0.31490(17) 0.0581(8) Uani 1 1 d . . . H6A H 0.9583 0.7006 0.2835 0.087 Uiso 1 1 calc R . . H6B H 1.0522 0.7632 0.2820 0.087 Uiso 1 1 calc R . . H6C H 1.0234 0.7819 0.3610 0.087 Uiso 1 1 calc R . . C7 C 1.15440(19) 0.5664(4) 0.39273(16) 0.0569(8) Uani 1 1 d . . . H7A H 1.1784 0.4600 0.4107 0.085 Uiso 1 1 calc R . . H7B H 1.1584 0.6345 0.4389 0.085 Uiso 1 1 calc R . . H7C H 1.1878 0.6151 0.3604 0.085 Uiso 1 1 calc R . . C8 C 1.17570(18) 0.4768(4) 0.15516(18) 0.0655(9) Uani 1 1 d . . . H8A H 1.1716 0.4825 0.0987 0.098 Uiso 1 1 calc R . . H8B H 1.2097 0.3820 0.1789 0.098 Uiso 1 1 calc R . . H8C H 1.2047 0.5736 0.1822 0.098 Uiso 1 1 calc R . . C9 C 0.96150(17) 0.5857(3) 0.09533(15) 0.0467(7) Uani 1 1 d . . . H9A H 0.9679 0.5882 0.0418 0.070 Uiso 1 1 calc R . . H9B H 0.9626 0.6956 0.1154 0.070 Uiso 1 1 calc R . . H9C H 0.9057 0.5349 0.0934 0.070 Uiso 1 1 calc R . . C10 C 0.88971(14) 0.2571(3) 0.33491(12) 0.0279(5) Uani 1 1 d . . . C11 C 0.84488(15) 0.3713(3) 0.28012(14) 0.0360(6) Uani 1 1 d . . . H11 H 0.8708 0.4134 0.2424 0.043 Uiso 1 1 calc R . . C12 C 0.76274(16) 0.4240(3) 0.28007(15) 0.0466(7) Uani 1 1 d . . . H12 H 0.7324 0.5008 0.2419 0.056 Uiso 1 1 calc R . . C13 C 0.72518(16) 0.3657(3) 0.33492(16) 0.0497(7) Uani 1 1 d . . . H13 H 0.6691 0.4027 0.3348 0.060 Uiso 1 1 calc R . . C14 C 0.76869(16) 0.2534(3) 0.39028(15) 0.0437(7) Uani 1 1 d . . . H14 H 0.7428 0.2140 0.4285 0.052 Uiso 1 1 calc R . . C15 C 0.84991(15) 0.1986(3) 0.38995(14) 0.0358(6) Uani 1 1 d . . . H15 H 0.8792 0.1200 0.4276 0.043 Uiso 1 1 calc R . . C16 C 1.07133(14) 0.1919(3) 0.42530(13) 0.0292(5) Uani 1 1 d . . . C17 C 1.15290(15) 0.1230(3) 0.43378(14) 0.0379(6) Uani 1 1 d . . . H17 H 1.1621 0.0625 0.3913 0.045 Uiso 1 1 calc R . . C18 C 1.22051(16) 0.1418(3) 0.50347(16) 0.0478(7) Uani 1 1 d . . . H18 H 1.2761 0.0958 0.5083 0.057 Uiso 1 1 calc R . . C19 C 1.20768(17) 0.2269(3) 0.56603(15) 0.0478(7) Uani 1 1 d . . . H19 H 1.2545 0.2407 0.6136 0.057 Uiso 1 1 calc R . . C20 C 1.12664(16) 0.2918(3) 0.55929(14) 0.0448(7) Uani 1 1 d . . . H20 H 1.1173 0.3484 0.6028 0.054 Uiso 1 1 calc R . . C21 C 1.05866(15) 0.2752(3) 0.48943(13) 0.0352(6) Uani 1 1 d . . . H21 H 1.0031 0.3208 0.4852 0.042 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 P 0.0328(3) 0.0262(3) 0.0272(3) -0.0013(3) 0.0100(3) 0.0009(3) Al 0.0350(4) 0.0426(5) 0.0314(4) 0.0030(3) 0.0129(3) -0.0046(3) N1 0.0434(12) 0.0349(11) 0.0274(11) -0.0027(9) 0.0152(9) -0.0016(9) N2 0.0403(11) 0.0290(11) 0.0297(10) -0.0012(9) 0.0125(9) -0.0043(9) C1 0.0278(12) 0.0303(13) 0.0282(13) 0.0001(10) 0.0082(10) 0.0027(10) C2 0.0395(14) 0.0353(14) 0.0300(12) -0.0076(11) 0.0117(11) -0.0010(11) C3 0.0465(16) 0.0580(19) 0.0659(19) -0.0191(16) 0.0080(15) 0.0095(14) C4 0.0495(16) 0.0532(17) 0.0390(15) -0.0079(13) 0.0061(13) 0.0013(14) C5 0.0537(16) 0.0290(13) 0.0345(13) -0.0029(11) 0.0175(12) -0.0050(12) C6 0.092(2) 0.0329(15) 0.0563(18) 0.0026(13) 0.0332(17) 0.0045(15) C7 0.0672(19) 0.0529(18) 0.0455(16) -0.0121(14) 0.0089(15) -0.0206(15) C8 0.0458(17) 0.097(3) 0.0584(19) 0.0018(18) 0.0227(15) -0.0116(17) C9 0.0476(16) 0.0468(16) 0.0413(15) 0.0077(13) 0.0068(13) -0.0033(13) C10 0.0268(12) 0.0296(12) 0.0241(12) -0.0058(10) 0.0030(10) -0.0048(10) C11 0.0345(13) 0.0403(14) 0.0303(13) -0.0014(11) 0.0055(11) 0.0017(12) C12 0.0376(15) 0.0542(17) 0.0420(15) -0.0001(14) 0.0027(13) 0.0108(13) C13 0.0289(14) 0.0640(19) 0.0538(17) -0.0164(15) 0.0089(13) 0.0038(14) C14 0.0347(14) 0.0585(17) 0.0394(15) -0.0089(14) 0.0135(12) -0.0076(13) C15 0.0309(13) 0.0428(14) 0.0316(13) -0.0013(11) 0.0059(11) -0.0044(11) C16 0.0298(13) 0.0314(13) 0.0279(13) 0.0043(10) 0.0108(10) 0.0013(10) C17 0.0357(14) 0.0397(14) 0.0396(14) 0.0025(11) 0.0134(12) 0.0047(11) C18 0.0311(14) 0.0567(18) 0.0521(17) 0.0106(14) 0.0074(13) 0.0079(13) C19 0.0384(15) 0.0654(19) 0.0326(14) 0.0084(14) 0.0000(12) -0.0050(14) C20 0.0414(16) 0.0636(18) 0.0291(14) -0.0047(13) 0.0101(12) -0.0058(14) C21 0.0285(13) 0.0450(15) 0.0317(13) -0.0012(12) 0.0085(11) 0.0010(11) #----------------------------------------------------------------------------# # BOND LENGTHS AND ANGLES # #----------------------------------------------------------------------------# _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 P C10 1.824(2) . ? P C16 1.829(2) . ? P C1 1.869(2) . ? Al N2 1.9270(19) . ? Al N1 1.928(2) . ? Al C8 1.948(3) . ? Al C9 1.972(3) . ? N1 C1 1.337(3) . ? N1 C2 1.465(3) . ? N2 C1 1.336(3) . ? N2 C5 1.461(3) . ? C2 C3 1.513(3) . ? C2 C4 1.516(3) . ? C5 C6 1.520(3) . ? C5 C7 1.525(4) . ? C10 C11 1.392(3) . ? C10 C15 1.399(3) . ? C11 C12 1.387(3) . ? C12 C13 1.373(4) . ? C13 C14 1.380(4) . ? C14 C15 1.381(3) . ? C16 C21 1.393(3) . ? C16 C17 1.394(3) . ? C17 C18 1.383(3) . ? C18 C19 1.378(4) . ? C19 C20 1.378(4) . ? C20 C21 1.386(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 C10 P C16 106.12(10) . . ? C10 P C1 101.07(10) . . ? C16 P C1 102.44(10) . . ? N2 Al N1 68.95(8) . . ? N2 Al C8 116.11(11) . . ? N1 Al C8 115.96(13) . . ? N2 Al C9 112.75(10) . . ? N1 Al C9 112.30(10) . . ? C8 Al C9 120.14(13) . . ? C1 N1 C2 126.97(19) . . ? C1 N1 Al 90.76(14) . . ? C2 N1 Al 141.69(15) . . ? C1 N2 C5 127.26(19) . . ? C1 N2 Al 90.82(13) . . ? C5 N2 Al 141.50(15) . . ? N2 C1 N1 109.43(19) . . ? N2 C1 P 130.21(16) . . ? N1 C1 P 120.30(17) . . ? N1 C2 C3 109.6(2) . . ? N1 C2 C4 109.1(2) . . ? C3 C2 C4 111.2(2) . . ? N2 C5 C6 108.5(2) . . ? N2 C5 C7 109.9(2) . . ? C6 C5 C7 110.6(2) . . ? C11 C10 C15 118.2(2) . . ? C11 C10 P 123.33(17) . . ? C15 C10 P 117.83(17) . . ? C12 C11 C10 120.6(2) . . ? C13 C12 C11 120.3(2) . . ? C12 C13 C14 120.2(2) . . ? C13 C14 C15 119.9(2) . . ? C14 C15 C10 120.9(2) . . ? C21 C16 C17 118.6(2) . . ? C21 C16 P 126.13(17) . . ? C17 C16 P 115.28(17) . . ? C18 C17 C16 120.5(2) . . ? C19 C18 C17 120.4(2) . . ? C20 C19 C18 119.7(2) . . ? C19 C20 C21 120.4(2) . . ? C20 C21 C16 120.4(2) . . ? data_sep2004 _database_code_depnum_ccdc_archive 'CCDC 262953' _audit_creation_date 2004-09-16T09:46:44-00:00 _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 'C31 H34 Al N2 P' _chemical_formula_sum 'C31 H34 Al N2 P' _chemical_formula_weight 492.55 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc _symmetry_space_group_name_Hall 'C -2yc' _symmetry_Int_Tables_number 9 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 15.9891(5) _cell_length_b 11.2621(3) _cell_length_c 15.4755(3) _cell_angle_alpha 90 _cell_angle_beta 104.277(2) _cell_angle_gamma 90 _cell_volume 2700.62(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 14200 _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 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.211 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.156 _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 -0.101941E-1 _diffrn_orient_matrix_ub_12 -0.6764E-2 _diffrn_orient_matrix_ub_13 0.610194E-1 _diffrn_orient_matrix_ub_21 0.637221E-1 _diffrn_orient_matrix_ub_22 -0.20325E-2 _diffrn_orient_matrix_ub_23 0.263592E-1 _diffrn_orient_matrix_ub_31 0.6843E-3 _diffrn_orient_matrix_ub_32 0.88512E-1 _diffrn_orient_matrix_ub_33 0.52683E-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 0.0554 _diffrn_reflns_av_unetI/netI 0.037 _diffrn_reflns_number 19322 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.76 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 4664 _reflns_number_gt 4382 _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^)+(0.0375P)^2^+1.1173P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 4664 _refine_ls_number_parameters 316 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0337 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_ref 0.0743 _refine_ls_wR_factor_gt 0.072 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(7) _refine_diff_density_max 0.157 _refine_diff_density_min -0.144 _refine_diff_density_rms 0.03 #----------------------------------------------------------------------------# # 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' Al Al 0.0645 0.0514 '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' 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 P P 0.43760(3) 0.58095(4) 0.43117(3) 0.02539(12) Uani 1 1 d . . . Al Al 0.49567(3) 0.36963(5) 0.66452(3) 0.02349(14) Uani 1 1 d . . . N1 N 0.43077(10) 0.50635(13) 0.61079(10) 0.0242(4) Uani 1 1 d . . . N2 N 0.50788(10) 0.39325(14) 0.54520(10) 0.0263(4) Uani 1 1 d . . . C1 C 0.45715(12) 0.48932(16) 0.53627(12) 0.0232(4) Uani 1 1 d . . . C2 C 0.37826(13) 0.60477(17) 0.62902(13) 0.0263(4) Uani 1 1 d . . . H2 H 0.3545 0.6492 0.5723 0.032 Uiso 1 1 calc R . . C3 C 0.43267(16) 0.6892(2) 0.69697(15) 0.0388(5) Uani 1 1 d . . . H3A H 0.4802 0.7201 0.6739 0.058 Uiso 1 1 calc R . . H3B H 0.4561 0.6466 0.7529 0.058 Uiso 1 1 calc R . . H3C H 0.3967 0.7553 0.7078 0.058 Uiso 1 1 calc R . . C4 C 0.30357(15) 0.5563(2) 0.66321(16) 0.0395(5) Uani 1 1 d . . . H4A H 0.2691 0.5022 0.6188 0.059 Uiso 1 1 calc R . . H4B H 0.2673 0.6222 0.6737 0.059 Uiso 1 1 calc R . . H4C H 0.3262 0.5133 0.7191 0.059 Uiso 1 1 calc R . . C5 C 0.54547(13) 0.33855(18) 0.47801(12) 0.0270(4) Uani 1 1 d . . . H5 H 0.5488 0.3989 0.4315 0.032 Uiso 1 1 calc R . . C6 C 0.48957(16) 0.2365(2) 0.43483(16) 0.0398(5) Uani 1 1 d . . . H6A H 0.4316 0.2658 0.4063 0.06 Uiso 1 1 calc R . . H6B H 0.4858 0.1775 0.4803 0.06 Uiso 1 1 calc R . . H6C H 0.5149 0.1997 0.3898 0.06 Uiso 1 1 calc R . . C7 C 0.63615(14) 0.2963(2) 0.52322(15) 0.0423(6) Uani 1 1 d . . . H7A H 0.6711 0.364 0.5509 0.063 Uiso 1 1 calc R . . H7B H 0.6625 0.26 0.4788 0.063 Uiso 1 1 calc R . . H7C H 0.6332 0.2375 0.5691 0.063 Uiso 1 1 calc R . . C8 C 0.32019(13) 0.59477(17) 0.39606(12) 0.0250(4) Uani 1 1 d . . . C9 C 0.28586(13) 0.67867(19) 0.33082(13) 0.0291(5) Uani 1 1 d . . . H9 H 0.3228 0.7363 0.3149 0.035 Uiso 1 1 calc R . . C10 C 0.19893(14) 0.67926(19) 0.28894(13) 0.0334(5) Uani 1 1 d . . . H10 H 0.1765 0.7381 0.2454 0.04 Uiso 1 1 calc R . . C11 C 0.14443(14) 0.5950(2) 0.30992(14) 0.0349(5) Uani 1 1 d . . . H11 H 0.0849 0.5943 0.2799 0.042 Uiso 1 1 calc R . . C12 C 0.17730(14) 0.5116(2) 0.37514(13) 0.0337(5) Uani 1 1 d . . . H12 H 0.14 0.4542 0.3907 0.04 Uiso 1 1 calc R . . C13 C 0.26443(14) 0.51140(18) 0.41794(13) 0.0307(5) Uani 1 1 d . . . H13 H 0.2863 0.4538 0.4626 0.037 Uiso 1 1 calc R . . C14 C 0.47923(13) 0.72364(17) 0.48127(12) 0.0264(4) Uani 1 1 d . . . C15 C 0.43053(14) 0.81966(18) 0.49772(13) 0.0304(5) Uani 1 1 d . . . H15 H 0.3693 0.8161 0.4803 0.037 Uiso 1 1 calc R . . C16 C 0.47126(16) 0.92076(19) 0.53950(15) 0.0379(5) Uani 1 1 d . . . H16 H 0.4377 0.9861 0.5504 0.045 Uiso 1 1 calc R . . C17 C 0.56030(16) 0.9269(2) 0.56532(16) 0.0421(6) Uani 1 1 d . . . H17 H 0.588 0.9952 0.5953 0.05 Uiso 1 1 calc R . . C18 C 0.60887(15) 0.8324(2) 0.54707(16) 0.0442(6) Uani 1 1 d . . . H18 H 0.6701 0.8366 0.5639 0.053 Uiso 1 1 calc R . . C19 C 0.56874(14) 0.7325(2) 0.50467(14) 0.0366(5) Uani 1 1 d . . . H19 H 0.6026 0.669 0.4913 0.044 Uiso 1 1 calc R . . C20 C 0.60406(13) 0.39049(18) 0.75688(13) 0.0270(4) Uani 1 1 d . . . C21 C 0.63330(13) 0.4963(2) 0.80113(14) 0.0325(5) Uani 1 1 d . . . H21 H 0.5986 0.5654 0.787 0.039 Uiso 1 1 calc R . . C22 C 0.71119(14) 0.5043(2) 0.86492(14) 0.0372(5) Uani 1 1 d . . . H22 H 0.7284 0.5777 0.8942 0.045 Uiso 1 1 calc R . . C23 C 0.76374(15) 0.4058(2) 0.88591(14) 0.0374(5) Uani 1 1 d . . . H23 H 0.8173 0.4112 0.9293 0.045 Uiso 1 1 calc R . . C24 C 0.73786(14) 0.2999(2) 0.84348(15) 0.0371(5) Uani 1 1 d . . . H24 H 0.7736 0.2316 0.8573 0.045 Uiso 1 1 calc R . . C25 C 0.65949(13) 0.2928(2) 0.78041(14) 0.0337(5) Uani 1 1 d . . . H25 H 0.6427 0.2187 0.752 0.04 Uiso 1 1 calc R . . C26 C 0.42739(13) 0.22842(17) 0.67834(12) 0.0258(4) Uani 1 1 d . . . C27 C 0.45254(13) 0.14868(18) 0.75008(13) 0.0296(5) Uani 1 1 d . . . H27 H 0.5051 0.1625 0.7935 0.036 Uiso 1 1 calc R . . C28 C 0.40287(14) 0.05022(19) 0.75950(14) 0.0342(5) Uani 1 1 d . . . H28 H 0.4221 -0.0024 0.8084 0.041 Uiso 1 1 calc R . . C29 C 0.32547(14) 0.02868(19) 0.69785(15) 0.0350(5) Uani 1 1 d . . . H29 H 0.2911 -0.0379 0.7045 0.042 Uiso 1 1 calc R . . C30 C 0.29896(14) 0.1050(2) 0.62681(15) 0.0366(5) Uani 1 1 d . . . H30 H 0.2461 0.0908 0.584 0.044 Uiso 1 1 calc R . . C31 C 0.34915(13) 0.20262(18) 0.61736(13) 0.0307(5) Uani 1 1 d . . . H31 H 0.3296 0.2537 0.5676 0.037 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 P 0.0275(3) 0.0258(3) 0.0228(2) 0.0031(2) 0.0059(2) 0.0024(2) Al 0.0252(3) 0.0226(3) 0.0218(3) 0.0015(2) 0.0042(2) 0.0016(2) N1 0.0275(9) 0.0211(8) 0.0238(8) 0.0020(7) 0.0062(7) 0.0042(7) N2 0.0289(9) 0.0268(9) 0.0238(8) 0.0026(7) 0.0075(7) 0.0056(7) C1 0.0235(10) 0.0233(10) 0.0216(10) -0.0006(8) 0.0030(8) -0.0010(8) C2 0.0299(11) 0.0252(10) 0.0240(10) 0.0026(8) 0.0068(8) 0.0056(9) C3 0.0449(14) 0.0320(12) 0.0357(12) -0.0059(9) 0.0026(10) 0.0074(10) C4 0.0382(13) 0.0422(13) 0.0427(13) 0.0030(10) 0.0185(11) 0.0071(10) C5 0.0308(11) 0.0270(11) 0.0251(10) 0.0002(8) 0.0103(8) 0.0034(9) C6 0.0434(13) 0.0392(13) 0.0373(12) -0.0102(10) 0.0113(10) -0.0028(11) C7 0.0336(13) 0.0496(14) 0.0430(13) -0.0087(11) 0.0084(10) 0.0072(11) C8 0.0284(11) 0.0241(10) 0.0212(9) -0.0035(8) 0.0037(8) 0.0005(8) C9 0.0318(12) 0.0291(11) 0.0270(10) 0.0009(8) 0.0085(9) 0.0010(9) C10 0.0362(13) 0.0335(12) 0.0276(11) -0.0004(9) 0.0021(9) 0.0075(10) C11 0.0278(12) 0.0430(13) 0.0310(11) -0.0091(9) 0.0018(9) 0.0016(10) C12 0.0325(12) 0.0367(12) 0.0307(11) -0.0058(9) 0.0056(9) -0.0097(9) C13 0.0378(12) 0.0267(10) 0.0261(10) -0.0001(8) 0.0053(9) -0.0024(9) C14 0.0287(11) 0.0262(10) 0.0233(10) 0.0075(8) 0.0048(8) -0.0022(8) C15 0.0301(11) 0.0281(11) 0.0314(11) 0.0051(9) 0.0042(9) 0.0010(9) C16 0.0462(14) 0.0260(11) 0.0391(12) 0.0064(9) 0.0058(10) 0.0018(10) C17 0.0470(15) 0.0303(12) 0.0425(13) 0.0031(10) -0.0012(11) -0.0132(11) C18 0.0306(13) 0.0440(14) 0.0533(14) 0.0091(11) 0.0013(10) -0.0072(11) C19 0.0320(12) 0.0347(12) 0.0423(13) 0.0075(10) 0.0078(10) -0.0003(10) C20 0.0263(11) 0.0308(11) 0.0246(10) 0.0032(8) 0.0075(8) -0.0009(9) C21 0.0279(12) 0.0323(12) 0.0373(12) 0.0016(9) 0.0079(10) 0.0033(9) C22 0.0361(13) 0.0386(13) 0.0362(12) -0.0095(10) 0.0074(10) -0.0077(10) C23 0.0282(12) 0.0496(14) 0.0302(11) 0.0054(10) -0.0008(9) -0.0046(10) C24 0.0278(12) 0.0339(12) 0.0452(13) 0.0133(10) 0.0005(10) 0.0034(10) C25 0.0300(12) 0.0313(12) 0.0380(12) 0.0023(9) 0.0050(9) -0.0007(9) C26 0.0255(10) 0.0270(10) 0.0254(10) -0.0015(8) 0.0076(8) 0.0032(8) C27 0.0274(11) 0.0316(12) 0.0285(11) 0.0021(9) 0.0044(8) 0.0024(9) C28 0.0398(13) 0.0307(12) 0.0343(12) 0.0078(9) 0.0132(10) 0.0032(10) C29 0.0395(13) 0.0268(11) 0.0419(12) -0.0006(9) 0.0161(10) -0.0062(10) C30 0.0294(12) 0.0400(13) 0.0386(12) -0.0048(10) 0.0047(9) -0.0059(10) C31 0.0322(12) 0.0311(11) 0.0269(10) 0.0049(8) 0.0038(8) 0.0020(9) #----------------------------------------------------------------------------# # 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 P C8 1.828(2) . ? P C14 1.836(2) . ? P C1 1.8860(18) . ? Al N2 1.9226(16) . ? Al N1 1.9270(16) . ? Al C20 1.970(2) . ? Al C26 1.970(2) . ? N1 C1 1.336(2) . ? N1 C2 1.459(2) . ? N2 C1 1.339(2) . ? N2 C5 1.459(2) . ? C2 C3 1.522(3) . ? C2 C4 1.522(3) . ? C5 C6 1.508(3) . ? C5 C7 1.523(3) . ? C8 C13 1.393(3) . ? C8 C9 1.393(3) . ? C9 C10 1.381(3) . ? C10 C11 1.380(3) . ? C11 C12 1.384(3) . ? C12 C13 1.387(3) . ? C14 C19 1.391(3) . ? C14 C15 1.392(3) . ? C15 C16 1.390(3) . ? C16 C17 1.382(3) . ? C17 C18 1.387(4) . ? C18 C19 1.379(3) . ? C20 C21 1.396(3) . ? C20 C25 1.404(3) . ? C21 C22 1.388(3) . ? C22 C23 1.381(3) . ? C23 C24 1.375(3) . ? C24 C25 1.388(3) . ? C26 C31 1.399(3) . ? C26 C27 1.407(3) . ? C27 C28 1.392(3) . ? C28 C29 1.385(3) . ? C29 C30 1.377(3) . ? C30 C31 1.390(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 C8 P C14 106.84(9) . . ? C8 P C1 104.04(8) . . ? C14 P C1 98.57(8) . . ? N2 Al N1 69.30(7) . . ? N2 Al C20 113.63(8) . . ? N1 Al C20 120.10(8) . . ? N2 Al C26 113.97(8) . . ? N1 Al C26 115.98(8) . . ? C20 Al C26 115.43(8) . . ? C1 N1 C2 126.52(15) . . ? C1 N1 Al 90.38(11) . . ? C2 N1 Al 142.91(13) . . ? C1 N2 C5 127.81(16) . . ? C1 N2 Al 90.49(11) . . ? C5 N2 Al 141.54(13) . . ? N1 C1 N2 109.83(15) . . ? N1 C1 P 130.20(14) . . ? N2 C1 P 119.90(14) . . ? N1 C2 C3 110.49(17) . . ? N1 C2 C4 109.45(16) . . ? C3 C2 C4 110.35(18) . . ? N2 C5 C6 109.53(16) . . ? N2 C5 C7 108.51(16) . . ? C6 C5 C7 111.00(18) . . ? C13 C8 C9 118.17(19) . . ? C13 C8 P 122.85(15) . . ? C9 C8 P 117.74(15) . . ? C10 C9 C8 120.96(19) . . ? C11 C10 C9 120.47(19) . . ? C10 C11 C12 119.3(2) . . ? C11 C12 C13 120.4(2) . . ? C12 C13 C8 120.69(19) . . ? C19 C14 C15 118.87(19) . . ? C19 C14 P 114.53(16) . . ? C15 C14 P 126.59(15) . . ? C16 C15 C14 120.2(2) . . ? C17 C16 C15 120.4(2) . . ? C16 C17 C18 119.4(2) . . ? C19 C18 C17 120.3(2) . . ? C18 C19 C14 120.7(2) . . ? C21 C20 C25 115.36(19) . . ? C21 C20 Al 125.87(15) . . ? C25 C20 Al 118.75(15) . . ? C22 C21 C20 122.5(2) . . ? C23 C22 C21 120.1(2) . . ? C24 C23 C22 119.4(2) . . ? C23 C24 C25 119.9(2) . . ? C24 C25 C20 122.7(2) . . ? C31 C26 C27 115.69(18) . . ? C31 C26 Al 121.44(14) . . ? C27 C26 Al 122.86(15) . . ? C28 C27 C26 122.10(19) . . ? C29 C28 C27 120.22(19) . . ? C30 C29 C28 119.2(2) . . ? C29 C30 C31 120.4(2) . . ? C30 C31 C26 122.45(19) . . ? #===END