Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_k0070 _database_code_CSD 179588 _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Manners, I.' 'Lough, Alan' 'McWilliams, Andrew R.' 'Rivard, Eric' _publ_contact_author_name 'Prof I Manners' _publ_contact_author_address ; Department of Chemistry University of Toronto 80 St. George Street Toronto M5S 1A1 CANADA ; _publ_contact_author_email 'IMANNERS@CHEM.UTORONTO.CA' _publ_section_title ; Reversible skeletal substitution reactions involving gruop 13 heterophosphazenes ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H9 Al Cl5 N3 P2' _chemical_formula_weight 353.30 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' 'N' 'N' 0.0061 0.0033 '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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.6405(6) _cell_length_b 7.8844(5) _cell_length_c 19.1001(12) _cell_angle_alpha 90.00 _cell_angle_beta 102.851(3) _cell_angle_gamma 90.00 _cell_volume 1415.43(15) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 8467 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 27.54 _exptl_crystal_description 'block' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.658 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 1.282 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6280 _exptl_absorpt_correction_T_max 0.6996 _exptl_absorpt_process_details 'Denzo-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 '\f scans and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 'not relevent for area detector data' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3433 _diffrn_reflns_av_R_equivalents 0.022 _diffrn_reflns_av_sigmaI/netI 0.0416 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 27.53 _reflns_number_total 3200 _reflns_number_gt 2664 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2001)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXTL V5.1 (Sheldrick 1999)' _computing_structure_refinement 'SHELXTL V5.1 (Sheldrick 1999)' _computing_molecular_graphics 'SHELXTL V5.1 (Sheldrick 1999)' _computing_publication_material 'SHELXTL V6.1 (Sheldrick 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^+1.6728P] 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 'none' _refine_ls_number_reflns 3200 _refine_ls_number_parameters 131 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0496 _refine_ls_R_factor_gt 0.0365 _refine_ls_wR_factor_ref 0.0840 _refine_ls_wR_factor_gt 0.0795 _refine_ls_goodness_of_fit_ref 1.136 _refine_ls_restrained_S_all 1.136 _refine_ls_shift/su_max 0.000 _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 Cl1 Cl 0.32935(9) 0.75670(10) -0.02380(4) 0.0448(2) Uani 1 1 d . . . Cl2 Cl 0.44247(10) 0.51783(11) 0.10374(5) 0.0577(3) Uani 1 1 d . . . Cl3 Cl -0.11252(10) 0.79636(12) -0.00433(4) 0.0535(2) Uani 1 1 d . . . Cl4 Cl -0.09795(9) 0.55755(11) 0.12493(4) 0.0469(2) Uani 1 1 d . . . Cl5 Cl 0.28673(8) 0.78523(9) 0.28279(3) 0.03563(18) Uani 1 1 d . . . P1 P 0.30559(7) 0.70823(9) 0.07573(4) 0.02876(18) Uani 1 1 d . . . P2 P 0.01887(7) 0.73119(9) 0.08843(4) 0.02800(17) Uani 1 1 d . . . Al1 Al 0.23866(9) 0.94441(10) 0.18836(4) 0.02682(19) Uani 1 1 d . . . N1 N 0.3503(2) 0.8685(3) 0.12485(11) 0.0315(5) Uani 1 1 d . . . N2 N 0.1532(3) 0.6386(3) 0.07427(14) 0.0390(6) Uani 1 1 d . . . N3 N 0.0513(2) 0.8894(3) 0.13972(11) 0.0288(5) Uani 1 1 d . . . C1 C 0.2629(4) 1.1858(4) 0.20877(16) 0.0424(7) Uani 1 1 d . . . H1A H 0.2303 1.2503 0.1643 0.064 Uiso 1 1 calc R . . H1B H 0.3637 1.2101 0.2286 0.064 Uiso 1 1 calc R . . H1C H 0.2071 1.2184 0.2437 0.064 Uiso 1 1 calc R . . C2 C 0.4916(3) 0.9483(5) 0.12799(18) 0.0506(9) Uani 1 1 d . . . H2A H 0.5414 0.8863 0.0965 0.076 Uiso 0.50 1 calc PR . . H2B H 0.5482 0.9445 0.1774 0.076 Uiso 0.50 1 calc PR . . H2C H 0.4783 1.0665 0.1121 0.076 Uiso 0.50 1 calc PR . . H2A* H 0.5038 1.0452 0.1609 0.076 Uiso 0.50 1 calc PR . . H2B* H 0.4971 0.9870 0.0799 0.076 Uiso 0.50 1 calc PR . . H2C* H 0.5670 0.8650 0.1452 0.076 Uiso 0.50 1 calc PR . . C3 C -0.0683(3) 0.9861(4) 0.15782(17) 0.0445(8) Uani 1 1 d . . . H3A H -0.1182 0.9143 0.1861 0.067 Uiso 0.50 1 calc PR . . H3B H -0.1346 1.0210 0.1135 0.067 Uiso 0.50 1 calc PR . . H3C H -0.0309 1.0869 0.1858 0.067 Uiso 0.50 1 calc PR . . H3A* H -0.0709 1.1005 0.1375 0.067 Uiso 0.50 1 calc PR . . H3B* H -0.0546 0.9938 0.2101 0.067 Uiso 0.50 1 calc PR . . H3C* H -0.1582 0.9279 0.1378 0.067 Uiso 0.50 1 calc PR . . 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 Cl1 0.0566(5) 0.0538(5) 0.0277(4) -0.0030(3) 0.0173(3) -0.0021(4) Cl2 0.0544(5) 0.0448(5) 0.0773(6) 0.0164(4) 0.0223(5) 0.0182(4) Cl3 0.0621(5) 0.0595(5) 0.0300(4) 0.0003(4) -0.0093(3) -0.0072(4) Cl4 0.0483(5) 0.0469(5) 0.0503(5) 0.0003(4) 0.0213(4) -0.0179(4) Cl5 0.0376(4) 0.0412(4) 0.0271(3) 0.0062(3) 0.0051(3) 0.0015(3) P1 0.0302(4) 0.0299(4) 0.0287(4) -0.0002(3) 0.0120(3) 0.0005(3) P2 0.0274(4) 0.0324(4) 0.0244(3) -0.0015(3) 0.0064(3) -0.0050(3) Al1 0.0325(4) 0.0260(4) 0.0220(4) -0.0019(3) 0.0061(3) -0.0048(3) N1 0.0296(12) 0.0371(13) 0.0296(12) -0.0032(10) 0.0102(9) -0.0115(11) N2 0.0352(13) 0.0327(13) 0.0531(15) -0.0151(12) 0.0184(11) -0.0085(11) N3 0.0285(11) 0.0319(12) 0.0257(11) -0.0026(9) 0.0055(9) 0.0033(10) C1 0.065(2) 0.0282(15) 0.0363(16) -0.0051(12) 0.0152(14) -0.0122(15) C2 0.0413(18) 0.062(2) 0.0519(19) -0.0119(17) 0.0189(15) -0.0253(17) C3 0.0376(17) 0.0477(19) 0.0481(18) -0.0049(15) 0.0092(14) 0.0135(15) _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 Cl1 P1 2.0016(10) . ? Cl2 P1 1.9917(11) . ? Cl3 P2 2.0023(10) . ? Cl4 P2 1.9944(10) . ? Cl5 Al1 2.1613(10) . ? P1 N2 1.563(2) . ? P1 N1 1.575(2) . ? P2 N2 1.562(2) . ? P2 N3 1.574(2) . ? Al1 N3 1.889(2) . ? Al1 N1 1.889(2) . ? Al1 C1 1.946(3) . ? N1 C2 1.490(3) . ? N3 C3 1.485(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 N2 P1 N1 115.08(12) . . ? N2 P1 Cl2 107.70(11) . . ? N1 P1 Cl2 111.55(10) . . ? N2 P1 Cl1 110.84(10) . . ? N1 P1 Cl1 109.79(9) . . ? Cl2 P1 Cl1 100.96(5) . . ? N2 P2 N3 114.89(12) . . ? N2 P2 Cl4 107.10(10) . . ? N3 P2 Cl4 112.07(9) . . ? N2 P2 Cl3 110.64(11) . . ? N3 P2 Cl3 110.26(9) . . ? Cl4 P2 Cl3 100.96(5) . . ? N3 Al1 N1 103.33(10) . . ? N3 Al1 C1 112.48(13) . . ? N1 Al1 C1 112.23(12) . . ? N3 Al1 Cl5 106.33(8) . . ? N1 Al1 Cl5 107.74(8) . . ? C1 Al1 Cl5 114.00(10) . . ? C2 N1 P1 119.3(2) . . ? C2 N1 Al1 119.13(19) . . ? P1 N1 Al1 121.14(13) . . ? P2 N2 P1 130.18(16) . . ? C3 N3 P2 119.67(19) . . ? C3 N3 Al1 118.31(18) . . ? P2 N3 Al1 121.58(13) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.349 _refine_diff_density_min -0.384 _refine_diff_density_rms 0.067