# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dominic S Wright' _publ_contact_author_email DSW1000@CAM.AC.UK _publ_section_title ; A Mechanistic study of the C-P Bond reaction of 1,2-(PH2)2-C6H4 with nBuLi/Sb(NMe2)3 ; loop_ _publ_author_name 'Dominic S Wright' 'Ruth Edge' 'Robert J Less' 'Eric McInnes' 'R E Mulvey' 'Vesal Naseri' # Attachment 'compound4Li2.cif' data_dw0807a _database_code_depnum_ccdc_archive 'CCDC 691462' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H38 Li2 N4 P2' _chemical_formula_sum 'C18 H38 Li2 N4 P2' _chemical_formula_weight 386.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C c' _symmetry_space_group_name_Hall 'C -2yc' 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 8.4325(3) _cell_length_b 25.183(1) _cell_length_c 11.7383(5) _cell_angle_alpha 90.00 _cell_angle_beta 106.450(2) _cell_angle_gamma 90.00 _cell_volume 2390.66(16) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 5177 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.073 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 0.190 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.916 _exptl_absorpt_correction_T_max 0.972 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; The crystals of the complex form as non-merohedral twins. The program ROTAX (Parsons, 2002) was used to determine that twinning occurred around the [1 0 2] direct lattice axis. The program WIN-GX (Farrugia, 1999) was used to prepare an HKLF5 file which was used for the final refinement of the structure. The R values, K values, esds and background noise were all significantly improved indicating the correct TWIN assignment. ; _diffrn_ambient_temperature 180(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 'Nonius Kappa CCD' _diffrn_measurement_method 'phi\omega scans' _diffrn_reflns_number 6293 _diffrn_reflns_av_R_equivalents 0.0640 _diffrn_reflns_av_sigmaI/netI 0.0585 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 26.37 _reflns_number_total 4718 _reflns_number_gt 4154 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _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^)+(0.0000P)^2^+1.3758P] 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 0.03(10) _refine_ls_number_reflns 4718 _refine_ls_number_parameters 252 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0552 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1019 _refine_ls_wR_factor_gt 0.0944 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.40699(10) 0.87659(3) 0.17947(6) 0.0348(2) Uani 1 1 d . . . H1 H 0.332(4) 0.8772(11) 0.064(2) 0.039(9) Uiso 1 1 d . . . P2 P 0.45355(9) 0.87214(3) 0.44991(6) 0.0364(2) Uani 1 1 d . . . H2 H 0.428(4) 0.8697(11) 0.560(2) 0.027(7) Uiso 1 1 d . . . N1 N 0.2904(3) 0.73263(10) 0.29906(19) 0.0314(6) Uani 1 1 d . . . N2 N 0.6348(3) 0.73433(11) 0.3056(2) 0.0341(6) Uani 1 1 d . . . N3 N 0.3082(3) 1.02053(10) 0.30333(17) 0.0322(6) Uani 1 1 d . . . N4 N 0.6617(3) 1.00993(10) 0.36553(19) 0.0295(6) Uani 1 1 d . . . Li1 Li 0.4616(7) 0.79377(18) 0.3119(4) 0.0374(12) Uani 1 1 d . . . Li2 Li 0.4707(6) 0.95536(17) 0.3224(4) 0.0341(11) Uani 1 1 d . . . C1 C 0.2212(4) 0.87718(11) 0.2287(2) 0.0317(7) Uani 1 1 d . . . C2 C 0.0574(5) 0.87998(13) 0.1521(3) 0.0413(8) Uani 1 1 d . . . H2A H 0.0422 0.8831 0.0691 0.050 Uiso 1 1 calc R . . C3 C -0.0795(5) 0.87836(14) 0.1930(3) 0.0477(9) Uani 1 1 d . . . H3A H -0.1871 0.8799 0.1388 0.057 Uiso 1 1 calc R . . C4 C -0.0599(7) 0.87448(13) 0.3126(4) 0.0492(8) Uani 1 1 d . . . H4A H -0.1545 0.8732 0.3413 0.059 Uiso 1 1 calc R . . C5 C 0.0974(5) 0.87238(13) 0.3924(3) 0.0435(8) Uani 1 1 d . . . H5A H 0.1083 0.8699 0.4750 0.052 Uiso 1 1 calc R . . C6 C 0.2417(5) 0.87380(11) 0.3534(2) 0.0351(8) Uani 1 1 d . . . C7 C 0.2704(5) 0.72520(14) 0.4185(3) 0.0468(9) Uani 1 1 d . . . H7A H 0.2007 0.6941 0.4186 0.070 Uiso 1 1 calc R . . H7B H 0.2180 0.7568 0.4408 0.070 Uiso 1 1 calc R . . H7C H 0.3790 0.7198 0.4757 0.070 Uiso 1 1 calc R . . C8 C 0.1258(4) 0.74115(15) 0.2158(3) 0.0400(8) Uani 1 1 d . . . H8A H 0.0587 0.7091 0.2122 0.060 Uiso 1 1 calc R . . H8B H 0.1369 0.7489 0.1366 0.060 Uiso 1 1 calc R . . H8C H 0.0719 0.7711 0.2430 0.060 Uiso 1 1 calc R . . C9 C 0.3696(5) 0.68656(13) 0.2614(3) 0.0473(8) Uani 1 1 d . . . H9A H 0.3512 0.6880 0.1744 0.057 Uiso 1 1 calc R . . H9B H 0.3179 0.6536 0.2800 0.057 Uiso 1 1 calc R . . C10 C 0.5521(5) 0.68503(13) 0.3221(3) 0.0490(9) Uani 1 1 d . . . H10A H 0.5702 0.6788 0.4081 0.059 Uiso 1 1 calc R . . H10B H 0.6021 0.6550 0.2901 0.059 Uiso 1 1 calc R . . C11 C 0.6633(5) 0.73726(17) 0.1881(3) 0.0496(10) Uani 1 1 d . . . H11A H 0.7279 0.7064 0.1767 0.074 Uiso 1 1 calc R . . H11B H 0.7243 0.7698 0.1825 0.074 Uiso 1 1 calc R . . H11C H 0.5569 0.7375 0.1265 0.074 Uiso 1 1 calc R . . C12 C 0.7979(4) 0.73659(17) 0.3953(3) 0.0442(9) Uani 1 1 d . . . H12A H 0.8644 0.7060 0.3853 0.066 Uiso 1 1 calc R . . H12B H 0.7827 0.7358 0.4751 0.066 Uiso 1 1 calc R . . H12C H 0.8546 0.7695 0.3851 0.066 Uiso 1 1 calc R . . C13 C 0.1692(5) 1.02338(16) 0.1946(3) 0.0556(11) Uani 1 1 d . . . H13A H 0.1004 1.0543 0.1987 0.083 Uiso 1 1 calc R . . H13B H 0.1026 0.9910 0.1871 0.083 Uiso 1 1 calc R . . H13C H 0.2119 1.0268 0.1255 0.083 Uiso 1 1 calc R . . C14 C 0.2393(5) 1.01660(14) 0.4050(3) 0.0422(8) Uani 1 1 d . . . H14A H 0.1712 1.0479 0.4069 0.063 Uiso 1 1 calc R . . H14B H 0.3298 1.0147 0.4788 0.063 Uiso 1 1 calc R . . H14C H 0.1711 0.9846 0.3969 0.063 Uiso 1 1 calc R . . C15 C 0.4156(5) 1.06747(11) 0.3140(3) 0.0369(7) Uani 1 1 d . . . H15A H 0.3637 1.0981 0.3425 0.044 Uiso 1 1 calc R . . H15B H 0.4279 1.0766 0.2349 0.044 Uiso 1 1 calc R . . C16 C 0.5841(4) 1.05711(12) 0.3993(3) 0.0366(7) Uani 1 1 d . . . H16A H 0.6560 1.0883 0.4008 0.044 Uiso 1 1 calc R . . H16B H 0.5729 1.0522 0.4804 0.044 Uiso 1 1 calc R . . C17 C 0.7180(5) 1.01922(15) 0.2585(3) 0.0468(9) Uani 1 1 d . . . H17A H 0.8031 1.0469 0.2754 0.070 Uiso 1 1 calc R . . H17B H 0.6240 1.0306 0.1927 0.070 Uiso 1 1 calc R . . H17C H 0.7641 0.9863 0.2368 0.070 Uiso 1 1 calc R . . C18 C 0.8090(4) 0.99452(15) 0.4631(2) 0.0442(8) Uani 1 1 d . . . H18A H 0.8874 1.0242 0.4811 0.066 Uiso 1 1 calc R . . H18B H 0.8619 0.9636 0.4386 0.066 Uiso 1 1 calc R . . H18C H 0.7750 0.9856 0.5340 0.066 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 P1 0.0510(5) 0.0255(4) 0.0280(4) 0.0003(3) 0.0117(3) -0.0003(4) P2 0.0504(6) 0.0277(5) 0.0272(4) 0.0001(3) 0.0049(3) -0.0007(5) N1 0.0285(16) 0.0251(14) 0.0409(14) -0.0014(10) 0.0101(11) 0.0020(12) N2 0.0288(15) 0.0309(15) 0.0439(14) 0.0021(10) 0.0125(11) -0.0007(13) N3 0.0345(16) 0.0318(15) 0.0281(12) -0.0046(9) 0.0056(10) 0.0016(13) N4 0.0318(16) 0.0304(13) 0.0278(12) -0.0032(10) 0.0111(10) -0.0014(13) Li1 0.043(3) 0.028(2) 0.040(2) 0.002(2) 0.011(2) 0.003(3) Li2 0.039(3) 0.022(2) 0.040(2) -0.0036(19) 0.009(2) 0.000(2) C1 0.043(2) 0.0127(14) 0.0369(15) 0.0008(10) 0.0070(12) 0.0033(15) C2 0.042(2) 0.0292(17) 0.0450(17) -0.0017(12) -0.0008(15) 0.0021(16) C3 0.044(2) 0.0228(17) 0.069(2) -0.0024(15) 0.0034(17) 0.0074(18) C4 0.042(2) 0.0279(16) 0.082(2) -0.0065(17) 0.0247(15) 0.000(2) C5 0.060(3) 0.0297(18) 0.0483(18) -0.0026(14) 0.0282(16) -0.0022(19) C6 0.056(2) 0.0143(14) 0.0351(15) -0.0004(12) 0.0135(13) 0.0006(16) C7 0.050(2) 0.045(2) 0.0449(18) 0.0063(15) 0.0124(14) -0.009(2) C8 0.029(2) 0.043(2) 0.0455(18) -0.0053(13) 0.0072(13) -0.0040(17) C9 0.044(2) 0.0234(17) 0.078(2) -0.0108(14) 0.0230(16) -0.0051(18) C10 0.042(2) 0.0273(19) 0.079(2) 0.0036(15) 0.0193(16) 0.0067(18) C11 0.037(2) 0.071(3) 0.0428(18) -0.0037(17) 0.0132(14) 0.005(2) C12 0.0308(19) 0.056(2) 0.0472(19) 0.0069(15) 0.0126(14) 0.0027(18) C13 0.046(2) 0.062(3) 0.0462(18) -0.0158(16) -0.0068(16) 0.017(2) C14 0.043(2) 0.0347(19) 0.059(2) -0.0050(15) 0.0309(16) -0.0071(18) C15 0.043(2) 0.0245(14) 0.0482(15) 0.0015(14) 0.0204(13) 0.0031(17) C16 0.0365(19) 0.0245(17) 0.0534(17) -0.0108(12) 0.0201(14) -0.0082(15) C17 0.049(2) 0.051(2) 0.0487(19) 0.0060(16) 0.0277(15) 0.005(2) C18 0.0323(19) 0.056(2) 0.0428(17) -0.0052(14) 0.0077(13) 0.0051(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 P1 C1 1.817(4) . ? P1 Li2 2.555(4) . ? P1 Li1 2.564(5) . ? P2 C6 1.825(4) . ? P2 Li1 2.567(5) . ? P2 Li2 2.603(5) . ? N1 C9 1.468(4) . ? N1 C8 1.470(4) . ? N1 C7 1.470(4) . ? N1 Li1 2.087(6) . ? N2 C10 1.463(4) . ? N2 C11 1.468(4) . ? N2 C12 1.478(4) . ? N2 Li1 2.107(6) . ? N3 C13 1.470(4) . ? N3 C14 1.471(4) . ? N3 C15 1.473(4) . ? N3 Li2 2.109(5) . ? N4 C16 1.464(4) . ? N4 C17 1.482(4) . ? N4 C18 1.483(4) . ? N4 Li2 2.068(6) . ? C1 C2 1.420(5) . ? C1 C6 1.427(4) . ? C2 C3 1.371(6) . ? C3 C4 1.369(6) . ? C4 C5 1.391(7) . ? C5 C6 1.416(5) . ? C9 C10 1.503(5) . ? C15 C16 1.512(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 C1 P1 Li2 79.92(16) . . ? C1 P1 Li1 80.61(16) . . ? Li2 P1 Li1 105.38(16) . . ? C6 P2 Li1 79.75(16) . . ? C6 P2 Li2 80.14(14) . . ? Li1 P2 Li2 103.91(16) . . ? C9 N1 C8 109.9(2) . . ? C9 N1 C7 111.8(3) . . ? C8 N1 C7 108.1(3) . . ? C9 N1 Li1 103.9(3) . . ? C8 N1 Li1 116.4(3) . . ? C7 N1 Li1 106.8(2) . . ? C10 N2 C11 112.2(3) . . ? C10 N2 C12 108.7(3) . . ? C11 N2 C12 107.5(3) . . ? C10 N2 Li1 103.7(3) . . ? C11 N2 Li1 107.3(2) . . ? C12 N2 Li1 117.5(3) . . ? C13 N3 C14 107.9(3) . . ? C13 N3 C15 110.8(3) . . ? C14 N3 C15 111.1(2) . . ? C13 N3 Li2 117.7(2) . . ? C14 N3 Li2 104.8(2) . . ? C15 N3 Li2 104.5(2) . . ? C16 N4 C17 112.1(2) . . ? C16 N4 C18 110.1(2) . . ? C17 N4 C18 107.3(3) . . ? C16 N4 Li2 103.2(2) . . ? C17 N4 Li2 108.2(2) . . ? C18 N4 Li2 116.0(2) . . ? N1 Li1 N2 86.9(2) . . ? N1 Li1 P1 123.7(2) . . ? N2 Li1 P1 124.3(3) . . ? N1 Li1 P2 118.1(3) . . ? N2 Li1 P2 135.3(3) . . ? P1 Li1 P2 74.03(13) . . ? N4 Li2 N3 86.93(19) . . ? N4 Li2 P1 132.9(3) . . ? N3 Li2 P1 121.7(2) . . ? N4 Li2 P2 124.1(2) . . ? N3 Li2 P2 123.2(3) . . ? P1 Li2 P2 73.55(12) . . ? C2 C1 C6 117.7(3) . . ? C2 C1 P1 124.8(2) . . ? C6 C1 P1 117.4(2) . . ? C3 C2 C1 122.8(3) . . ? C4 C3 C2 119.4(4) . . ? C3 C4 C5 120.6(5) . . ? C4 C5 C6 121.6(3) . . ? C5 C6 C1 117.9(3) . . ? C5 C6 P2 125.3(2) . . ? C1 C6 P2 116.8(2) . . ? N1 C9 C10 111.7(3) . . ? N2 C10 C9 112.2(3) . . ? N3 C15 C16 111.0(2) . . ? N4 C16 C15 111.6(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.175 _refine_diff_density_min -0.180 _refine_diff_density_rms 0.042 # Attachment 'compound6Li2.cif' data_dw0824 _database_code_depnum_ccdc_archive 'CCDC 691463' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H54 Li2 N6 P4' _chemical_formula_sum 'C30 H54 Li2 N6 P4' _chemical_formula_weight 636.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 15.2198(3) _cell_length_b 15.4779(3) _cell_length_c 16.4017(4) _cell_angle_alpha 90.00 _cell_angle_beta 107.777(1) _cell_angle_gamma 90.00 _cell_volume 3679.27(14) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 10939 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.149 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 0.233 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.924 _exptl_absorpt_correction_T_max 0.988 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 'Nonius Kappa CCD' _diffrn_measurement_method 'phi\omega scans' _diffrn_reflns_number 21578 _diffrn_reflns_av_R_equivalents 0.0533 _diffrn_reflns_av_sigmaI/netI 0.0665 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.02 _reflns_number_total 6433 _reflns_number_gt 4712 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _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^)+(0.0110P)^2^+3.0662P] 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_extinction_coef ? _refine_ls_number_reflns 6433 _refine_ls_number_parameters 389 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0841 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.1051 _refine_ls_wR_factor_gt 0.0917 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.64390(5) 0.76107(5) 0.21924(5) 0.03600(19) Uani 1 1 d . . . P2 P 0.58997(5) 0.83477(4) 0.30607(5) 0.03278(18) Uani 1 1 d . . . P3 P 0.45495(5) 0.86483(4) 0.21437(4) 0.03223(18) Uani 1 1 d . . . P4 P 0.37259(5) 0.82545(4) 0.29553(5) 0.03250(18) Uani 1 1 d . . . N1 N 0.85932(16) 0.86550(15) 0.20401(15) 0.0401(6) Uani 1 1 d . . . N2 N 0.73101(17) 1.00753(14) 0.18479(15) 0.0412(6) Uani 1 1 d . . . N3 N 0.65591(15) 0.91222(14) 0.02297(14) 0.0357(5) Uani 1 1 d . . . Li1 Li 0.7152(3) 0.8761(3) 0.1529(3) 0.0337(10) Uani 1 1 d . . . N4 N 0.40286(15) 1.08216(13) 0.37728(14) 0.0352(5) Uani 1 1 d . . . N5 N 0.21989(15) 1.02352(14) 0.28166(14) 0.0356(5) Uani 1 1 d . . . N6 N 0.24938(16) 0.93041(15) 0.44257(15) 0.0391(6) Uani 1 1 d . . . Li2 Li 0.3335(3) 0.9612(3) 0.3638(3) 0.0345(10) Uani 1 1 d . . . C1 C 0.53314(19) 0.72980(16) 0.14387(16) 0.0317(6) Uani 1 1 d . . . C2 C 0.45100(18) 0.77403(16) 0.14034(16) 0.0304(6) Uani 1 1 d . . . C3 C 0.3701(2) 0.75588(17) 0.07478(17) 0.0372(7) Uani 1 1 d . . . H3A H 0.3156 0.7873 0.0718 0.045 Uiso 1 1 calc R . . C4 C 0.3673(2) 0.69309(18) 0.01381(18) 0.0433(7) Uani 1 1 d . . . H4A H 0.3119 0.6821 -0.0311 0.052 Uiso 1 1 calc R . . C5 C 0.4469(2) 0.64661(18) 0.01974(18) 0.0450(8) Uani 1 1 d . . . H5A H 0.4454 0.6021 -0.0205 0.054 Uiso 1 1 calc R . . C6 C 0.5278(2) 0.66413(17) 0.08307(18) 0.0393(7) Uani 1 1 d . . . H6A H 0.5814 0.6312 0.0859 0.047 Uiso 1 1 calc R . . C7 C 0.54982(18) 0.75238(16) 0.36772(16) 0.0291(6) Uani 1 1 d . . . C8 C 0.45603(18) 0.75059(15) 0.36407(16) 0.0287(6) Uani 1 1 d . . . C9 C 0.43046(19) 0.68983(16) 0.41650(17) 0.0345(6) Uani 1 1 d . . . H9A H 0.3675 0.6861 0.4144 0.041 Uiso 1 1 calc R . . C10 C 0.4937(2) 0.63556(18) 0.47076(18) 0.0403(7) Uani 1 1 d . . . H10A H 0.4739 0.5954 0.5053 0.048 Uiso 1 1 calc R . . C11 C 0.5854(2) 0.63929(18) 0.47504(18) 0.0430(7) Uani 1 1 d . . . H11A H 0.6292 0.6024 0.5127 0.052 Uiso 1 1 calc R . . C12 C 0.6126(2) 0.69783(17) 0.42343(17) 0.0383(7) Uani 1 1 d . . . H12A H 0.6758 0.7007 0.4263 0.046 Uiso 1 1 calc R . . C13 C 0.9074(2) 0.8097(2) 0.1595(2) 0.0673(10) Uani 1 1 d . . . H13A H 0.9739 0.8120 0.1888 0.101 Uiso 1 1 calc R . . H13B H 0.8948 0.8295 0.1003 0.101 Uiso 1 1 calc R . . H13C H 0.8856 0.7501 0.1597 0.101 Uiso 1 1 calc R . . C14 C 0.8785(2) 0.8345(2) 0.2911(2) 0.0597(9) Uani 1 1 d . . . H14A H 0.9442 0.8419 0.3218 0.090 Uiso 1 1 calc R . . H14B H 0.8623 0.7732 0.2903 0.090 Uiso 1 1 calc R . . H14C H 0.8418 0.8675 0.3201 0.090 Uiso 1 1 calc R . . C15 C 0.8890(2) 0.9553(2) 0.2014(2) 0.0601(9) Uani 1 1 d . . . H15A H 0.8863 0.9701 0.1419 0.072 Uiso 1 1 calc R . . H15B H 0.9539 0.9610 0.2378 0.072 Uiso 1 1 calc R . . C16 C 0.8302(2) 1.0183(2) 0.2318(2) 0.0590(9) Uani 1 1 d . . . H16A H 0.8401 1.0094 0.2938 0.071 Uiso 1 1 calc R . . H16B H 0.8493 1.0780 0.2238 0.071 Uiso 1 1 calc R . . C17 C 0.6727(3) 1.0417(2) 0.2347(2) 0.0595(9) Uani 1 1 d . . . H17A H 0.6865 1.1030 0.2470 0.089 Uiso 1 1 calc R . . H17B H 0.6853 1.0096 0.2886 0.089 Uiso 1 1 calc R . . H17C H 0.6075 1.0350 0.2016 0.089 Uiso 1 1 calc R . . C18 C 0.7059(2) 1.04955(18) 0.10018(19) 0.0440(7) Uani 1 1 d . . . H18A H 0.7604 1.0511 0.0792 0.053 Uiso 1 1 calc R . . H18B H 0.6864 1.1098 0.1053 0.053 Uiso 1 1 calc R . . C19 C 0.6286(2) 1.00132(17) 0.03696(19) 0.0418(7) Uani 1 1 d . . . H19A H 0.5745 0.9993 0.0585 0.050 Uiso 1 1 calc R . . H19B H 0.6102 1.0327 -0.0183 0.050 Uiso 1 1 calc R . . C20 C 0.5730(2) 0.86069(19) -0.01984(19) 0.0464(8) Uani 1 1 d . . . H20A H 0.5407 0.8867 -0.0754 0.070 Uiso 1 1 calc R . . H20B H 0.5319 0.8596 0.0160 0.070 Uiso 1 1 calc R . . H20C H 0.5914 0.8016 -0.0285 0.070 Uiso 1 1 calc R . . C21 C 0.7158(2) 0.9137(2) -0.0323(2) 0.0541(9) Uani 1 1 d . . . H21A H 0.6830 0.9411 -0.0870 0.081 Uiso 1 1 calc R . . H21B H 0.7324 0.8544 -0.0426 0.081 Uiso 1 1 calc R . . H21C H 0.7719 0.9465 -0.0041 0.081 Uiso 1 1 calc R . . C22 C 0.4583(2) 1.0770(2) 0.3183(2) 0.0506(8) Uani 1 1 d . . . H22A H 0.4815 1.1346 0.3108 0.076 Uiso 1 1 calc R . . H22B H 0.4200 1.0551 0.2627 0.076 Uiso 1 1 calc R . . H22C H 0.5105 1.0378 0.3419 0.076 Uiso 1 1 calc R . . C23 C 0.4630(2) 1.1127(2) 0.4612(2) 0.0528(8) Uani 1 1 d . . . H23A H 0.4853 1.1711 0.4550 0.079 Uiso 1 1 calc R . . H23B H 0.5158 1.0736 0.4819 0.079 Uiso 1 1 calc R . . H23C H 0.4279 1.1139 0.5024 0.079 Uiso 1 1 calc R . . C24 C 0.3264(2) 1.14308(17) 0.34595(19) 0.0436(7) Uani 1 1 d . . . H24A H 0.3508 1.1987 0.3322 0.052 Uiso 1 1 calc R . . H24B H 0.2981 1.1540 0.3919 0.052 Uiso 1 1 calc R . . C25 C 0.2526(2) 1.11034(18) 0.26693(19) 0.0454(8) Uani 1 1 d . . . H25A H 0.1999 1.1510 0.2519 0.054 Uiso 1 1 calc R . . H25B H 0.2780 1.1079 0.2182 0.054 Uiso 1 1 calc R . . C26 C 0.1774(2) 0.9792(2) 0.19966(18) 0.0502(8) Uani 1 1 d . . . H26A H 0.1252 1.0134 0.1648 0.075 Uiso 1 1 calc R . . H26B H 0.1556 0.9221 0.2105 0.075 Uiso 1 1 calc R . . H26C H 0.2232 0.9728 0.1691 0.075 Uiso 1 1 calc R . . C27 C 0.1546(2) 1.0290(2) 0.33201(19) 0.0451(8) Uani 1 1 d . . . H27A H 0.0914 1.0386 0.2930 0.054 Uiso 1 1 calc R . . H27B H 0.1712 1.0786 0.3719 0.054 Uiso 1 1 calc R . . C28 C 0.1568(2) 0.9468(2) 0.3822(2) 0.0475(8) Uani 1 1 d . . . H28A H 0.1116 0.9512 0.4145 0.057 Uiso 1 1 calc R . . H28B H 0.1385 0.8976 0.3421 0.057 Uiso 1 1 calc R . . C29 C 0.2569(2) 0.8396(2) 0.4701(2) 0.0617(10) Uani 1 1 d . . . H29A H 0.2111 0.8275 0.4995 0.093 Uiso 1 1 calc R . . H29B H 0.3189 0.8288 0.5091 0.093 Uiso 1 1 calc R . . H29C H 0.2457 0.8020 0.4199 0.093 Uiso 1 1 calc R . . C30 C 0.2668(2) 0.9863(2) 0.51796(19) 0.0536(8) Uani 1 1 d . . . H30A H 0.2201 0.9753 0.5467 0.080 Uiso 1 1 calc R . . H30B H 0.2637 1.0469 0.5001 0.080 Uiso 1 1 calc R . . H30C H 0.3282 0.9739 0.5575 0.080 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 P1 0.0352(4) 0.0367(4) 0.0399(4) 0.0043(3) 0.0170(3) -0.0018(3) P2 0.0357(4) 0.0302(4) 0.0321(4) 0.0001(3) 0.0099(3) -0.0069(3) P3 0.0400(4) 0.0255(3) 0.0313(4) 0.0014(3) 0.0110(3) 0.0002(3) P4 0.0352(4) 0.0297(4) 0.0341(4) -0.0018(3) 0.0129(3) 0.0024(3) N1 0.0374(13) 0.0413(14) 0.0411(15) 0.0021(11) 0.0109(11) -0.0026(11) N2 0.0495(15) 0.0368(13) 0.0392(15) -0.0031(11) 0.0165(12) -0.0039(12) N3 0.0387(13) 0.0377(13) 0.0357(14) 0.0030(10) 0.0185(11) 0.0047(11) Li1 0.035(2) 0.038(2) 0.030(2) 0.0025(19) 0.011(2) 0.001(2) N4 0.0371(13) 0.0313(12) 0.0361(14) -0.0075(10) 0.0097(11) -0.0024(11) N5 0.0368(13) 0.0355(13) 0.0315(13) -0.0014(10) 0.0058(10) 0.0024(11) N6 0.0420(14) 0.0414(13) 0.0373(14) 0.0020(11) 0.0171(11) 0.0004(12) Li2 0.037(3) 0.034(2) 0.034(3) -0.0003(19) 0.013(2) 0.000(2) C1 0.0438(16) 0.0279(14) 0.0278(15) 0.0045(11) 0.0174(13) -0.0019(13) C2 0.0390(16) 0.0289(14) 0.0264(15) 0.0024(11) 0.0146(12) -0.0031(12) C3 0.0394(16) 0.0382(16) 0.0349(16) 0.0032(13) 0.0127(13) -0.0026(13) C4 0.0530(19) 0.0467(18) 0.0280(16) -0.0018(13) 0.0092(14) -0.0102(16) C5 0.070(2) 0.0363(16) 0.0334(17) -0.0051(13) 0.0233(16) -0.0091(16) C6 0.0534(19) 0.0339(15) 0.0388(17) 0.0014(13) 0.0260(15) 0.0022(14) C7 0.0345(15) 0.0262(13) 0.0266(14) -0.0014(11) 0.0093(12) -0.0006(12) C8 0.0358(15) 0.0256(13) 0.0248(14) -0.0059(11) 0.0094(12) -0.0032(12) C9 0.0378(16) 0.0314(15) 0.0383(17) -0.0057(12) 0.0174(13) -0.0052(13) C10 0.061(2) 0.0331(15) 0.0343(17) 0.0022(12) 0.0261(15) -0.0013(15) C11 0.056(2) 0.0394(16) 0.0357(17) 0.0115(13) 0.0174(15) 0.0138(15) C12 0.0381(16) 0.0433(16) 0.0343(16) 0.0000(13) 0.0123(13) 0.0066(14) C13 0.056(2) 0.081(3) 0.069(3) 0.001(2) 0.0243(19) 0.016(2) C14 0.059(2) 0.072(2) 0.041(2) 0.0074(17) 0.0037(16) -0.0073(19) C15 0.0405(19) 0.058(2) 0.074(3) 0.0056(18) 0.0070(18) -0.0120(17) C16 0.064(2) 0.0401(18) 0.065(2) -0.0083(16) 0.0084(19) -0.0158(18) C17 0.086(3) 0.0467(19) 0.057(2) -0.0099(16) 0.038(2) -0.0039(19) C18 0.056(2) 0.0299(15) 0.054(2) 0.0035(14) 0.0290(16) -0.0011(15) C19 0.0479(18) 0.0383(16) 0.0433(18) 0.0096(13) 0.0202(15) 0.0068(14) C20 0.0495(19) 0.0446(17) 0.0420(18) 0.0023(14) 0.0093(15) 0.0023(15) C21 0.064(2) 0.061(2) 0.047(2) -0.0026(16) 0.0323(17) 0.0021(18) C22 0.057(2) 0.0448(18) 0.057(2) -0.0097(15) 0.0286(17) -0.0133(16) C23 0.052(2) 0.0536(19) 0.048(2) -0.0150(15) 0.0066(16) -0.0104(16) C24 0.0506(19) 0.0289(15) 0.051(2) -0.0020(13) 0.0153(15) 0.0004(14) C25 0.0529(19) 0.0338(16) 0.0434(19) 0.0071(13) 0.0056(15) 0.0079(15) C26 0.059(2) 0.0481(18) 0.0353(18) -0.0038(14) 0.0023(15) -0.0045(16) C27 0.0320(16) 0.0541(19) 0.0447(19) -0.0065(15) 0.0052(14) 0.0062(15) C28 0.0394(18) 0.057(2) 0.050(2) -0.0080(16) 0.0190(15) -0.0084(15) C29 0.072(2) 0.052(2) 0.073(3) 0.0174(18) 0.041(2) 0.0035(19) C30 0.0471(19) 0.072(2) 0.0421(19) -0.0023(16) 0.0144(15) 0.0078(17) _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 P1 C1 1.825(3) . ? P1 P2 2.1718(11) . ? P1 Li1 2.501(4) . ? P2 C7 1.844(3) . ? P2 P3 2.1941(13) . ? P3 C2 1.846(3) . ? P3 P4 2.1757(11) . ? P4 C8 1.830(3) . ? P4 Li2 2.536(4) . ? N1 C14 1.450(4) . ? N1 C13 1.463(4) . ? N1 C15 1.467(4) . ? N1 Li1 2.102(5) . ? N2 C18 1.473(4) . ? N2 C17 1.477(4) . ? N2 C16 1.480(4) . ? N2 Li1 2.096(5) . ? N3 C21 1.468(3) . ? N3 C20 1.476(4) . ? N3 C19 1.478(3) . ? N3 Li1 2.120(5) . ? N4 C24 1.464(3) . ? N4 C22 1.468(4) . ? N4 C23 1.480(4) . ? N4 Li2 2.128(5) . ? N5 C26 1.472(3) . ? N5 C27 1.476(4) . ? N5 C25 1.478(3) . ? N5 Li2 2.076(5) . ? N6 C30 1.465(4) . ? N6 C29 1.470(4) . ? N6 C28 1.475(4) . ? N6 Li2 2.132(5) . ? C1 C6 1.409(4) . ? C1 C2 1.411(4) . ? C2 C3 1.394(4) . ? C3 C4 1.386(4) . ? C4 C5 1.387(4) . ? C5 C6 1.375(4) . ? C7 C12 1.389(4) . ? C7 C8 1.410(4) . ? C8 C9 1.407(3) . ? C9 C10 1.378(4) . ? C10 C11 1.377(4) . ? C11 C12 1.387(4) . ? C15 C16 1.508(5) . ? C18 C19 1.507(4) . ? C24 C25 1.520(4) . ? C27 C28 1.510(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 C1 P1 P2 97.33(9) . . ? C1 P1 Li1 109.14(13) . . ? P2 P1 Li1 102.28(11) . . ? C7 P2 P1 104.55(9) . . ? C7 P2 P3 97.16(9) . . ? P1 P2 P3 97.14(4) . . ? C2 P3 P4 106.26(8) . . ? C2 P3 P2 97.18(9) . . ? P4 P3 P2 96.62(4) . . ? C8 P4 P3 97.57(9) . . ? C8 P4 Li2 117.77(13) . . ? P3 P4 Li2 107.15(11) . . ? C14 N1 C13 108.4(3) . . ? C14 N1 C15 111.8(3) . . ? C13 N1 C15 109.9(3) . . ? C14 N1 Li1 106.9(2) . . ? C13 N1 Li1 117.8(2) . . ? C15 N1 Li1 102.0(2) . . ? C18 N2 C17 109.7(2) . . ? C18 N2 C16 111.8(2) . . ? C17 N2 C16 111.1(3) . . ? C18 N2 Li1 102.5(2) . . ? C17 N2 Li1 116.3(2) . . ? C16 N2 Li1 105.1(2) . . ? C21 N3 C20 108.4(2) . . ? C21 N3 C19 109.8(2) . . ? C20 N3 C19 109.8(2) . . ? C21 N3 Li1 118.1(2) . . ? C20 N3 Li1 112.0(2) . . ? C19 N3 Li1 98.3(2) . . ? N2 Li1 N1 87.13(19) . . ? N2 Li1 N3 88.62(18) . . ? N1 Li1 N3 119.6(2) . . ? N2 Li1 P1 127.9(2) . . ? N1 Li1 P1 108.04(19) . . ? N3 Li1 P1 121.1(2) . . ? C24 N4 C22 111.1(2) . . ? C24 N4 C23 108.7(2) . . ? C22 N4 C23 108.3(2) . . ? C24 N4 Li2 102.4(2) . . ? C22 N4 Li2 104.5(2) . . ? C23 N4 Li2 121.7(2) . . ? C26 N5 C27 110.8(2) . . ? C26 N5 C25 110.5(2) . . ? C27 N5 C25 110.9(2) . . ? C26 N5 Li2 115.0(2) . . ? C27 N5 Li2 103.5(2) . . ? C25 N5 Li2 105.9(2) . . ? C30 N6 C29 109.1(2) . . ? C30 N6 C28 110.8(2) . . ? C29 N6 C28 109.8(2) . . ? C30 N6 Li2 113.1(2) . . ? C29 N6 Li2 113.3(2) . . ? C28 N6 Li2 100.5(2) . . ? N5 Li2 N4 86.97(18) . . ? N5 Li2 N6 87.83(19) . . ? N4 Li2 N6 120.3(2) . . ? N5 Li2 P4 111.07(19) . . ? N4 Li2 P4 126.8(2) . . ? N6 Li2 P4 110.35(19) . . ? C6 C1 C2 117.6(2) . . ? C6 C1 P1 120.8(2) . . ? C2 C1 P1 121.51(19) . . ? C3 C2 C1 119.8(2) . . ? C3 C2 P3 120.3(2) . . ? C1 C2 P3 119.5(2) . . ? C4 C3 C2 121.6(3) . . ? C3 C4 C5 118.6(3) . . ? C6 C5 C4 120.9(3) . . ? C5 C6 C1 121.4(3) . . ? C12 C7 C8 120.0(2) . . ? C12 C7 P2 120.3(2) . . ? C8 C7 P2 119.40(19) . . ? C9 C8 C7 116.9(2) . . ? C9 C8 P4 121.9(2) . . ? C7 C8 P4 121.15(19) . . ? C10 C9 C8 122.2(3) . . ? C11 C10 C9 120.3(3) . . ? C10 C11 C12 118.9(3) . . ? C11 C12 C7 121.7(3) . . ? N1 C15 C16 112.6(3) . . ? N2 C16 C15 111.6(3) . . ? N2 C18 C19 110.7(2) . . ? N3 C19 C18 111.8(2) . . ? N4 C24 C25 112.7(2) . . ? N5 C25 C24 111.2(2) . . ? N5 C27 C28 110.5(2) . . ? N6 C28 C27 111.6(2) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.244 _refine_diff_density_min -0.264 _refine_diff_density_rms 0.051