# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _audit_creation_method SHELXL-97 _publ_contact_author_name 'Piero Sozzani' _publ_contact_author_address ; Dept.Materials Science University of Milano Bicocca Via R. Cozzi 53 I-20125 Milan ITALY ; _publ_contact_author_email piero.sozzani@mater.unimib.it _publ_section_title ; A single crystal imprints macroscopic orientation to xenon atoms ; loop_ _publ_author_name 'P. Sozzani' 'S. Bracco' 'A. Comotti' 'L. Ferretti' 'M. Mauri' 'R. Simonutti' data_compound_1 _database_code_depnum_ccdc_archive 'CCDC 625332' _chemical_name_common tris-o-phenylenedioxyspirocyclotriphosphazene _chemical_formula_sum 'C18 H12 N3 O6 P3' _chemical_formula_weight 459.23 _chemical_melting_point 249 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' O O 0.0106 0.0060 '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 hexagonal _symmetry_space_group_name_H-M 'P 63/m' _symmetry_Int_Tables_number 176 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' _cell_length_a 11.454(5) _cell_length_b 11.454(5) _cell_length_c 10.160(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 1154.4(9) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 266 _cell_measurement_theta_min 3.56 _cell_measurement_theta_max 28.14 _exptl_crystal_description 'hexagonal prism' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.080 _exptl_crystal_size_min 0.080 _exptl_crystal_density_diffrn 1.286 _exptl_crystal_F_000 468 _exptl_absorpt_coefficient_mu 0.293 _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Xcalibur' _diffrn_measurement_method '\w scans' _diffrn_reflns_number 8016 _diffrn_reflns_av_R_equivalents 0.1693 _diffrn_reflns_av_sigmaI/netI 0.1257 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.56 _diffrn_reflns_theta_max 28.14 _reflns_number_total 949 _reflns_number_gt 862 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrysAlis _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _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^)+(0.0001P)^2^+25.1800P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 949 _refine_ls_number_parameters 49 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1920 _refine_ls_R_factor_gt 0.0856 _refine_ls_wR_factor_ref 0.3027 _refine_ls_wR_factor_gt 0.1246 _refine_ls_goodness_of_fit_ref 1.447 _refine_ls_restrained_S_all 1.447 _refine_ls_shift/su_max 0.107 _refine_ls_shift/su_mean 0.032 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 0.5430(4) 0.1836(5) 0.7500 0.0249(11) Uani 1 2 d S . . O1 O 0.4611(9) 0.0830(9) 0.6313(8) 0.037(2) Uani 1 1 d . . . N1 N 0.6895(17) 0.2101(17) 0.7500 0.041(4) Uani 1 2 d S . . C1 C 0.3526(14) -0.0335(13) 0.6821(12) 0.037(3) Uani 1 1 d . . . C2 C 0.2572(15) -0.1399(15) 0.6091(15) 0.052(4) Uani 1 1 d . . . H2 H 0.2593 -0.1400 0.5176 0.067 Uiso 1 1 calc R . . C3 C 0.1570(15) -0.2476(17) 0.6809(14) 0.067(6) Uani 1 1 d . . . H3 H 0.0889 -0.3208 0.6361 0.087 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 0.014(2) 0.023(2) 0.026(2) 0.000 0.000 0.0003(18) O1 0.044(6) 0.039(5) 0.020(4) 0.002(4) 0.004(4) 0.014(4) N1 0.039(10) 0.035(9) 0.052(10) 0.000 0.000 0.021(8) C1 0.054(9) 0.033(7) 0.029(7) 0.005(6) 0.007(7) 0.026(7) C2 0.048(9) 0.044(9) 0.030(7) -0.005(7) -0.003(7) -0.001(7) C3 0.040(9) 0.063(11) 0.040(8) -0.005(8) -0.009(7) -0.018(8) _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 N1 1.548(17) . ? P1 N1 1.598(17) 3_665 ? P1 O1 1.606(9) . ? P1 O1 1.606(9) 10_557 ? O1 C1 1.391(16) . ? N1 P1 1.598(17) 2_655 ? C1 C2 1.377(18) . ? C1 C1 1.38(2) 10_557 ? C2 C3 1.398(19) . ? C3 C3 1.40(3) 10_557 ? 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 P1 N1 118.2(11) . 3_665 ? N1 P1 O1 109.2(6) . . ? N1 P1 O1 110.5(5) 3_665 . ? N1 P1 O1 109.2(6) . 10_557 ? N1 P1 O1 110.5(5) 3_665 10_557 ? O1 P1 O1 97.3(7) . 10_557 ? C1 O1 P1 109.4(7) . . ? P1 N1 P1 121.8(11) . 2_655 ? C2 C1 C1 122.6(8) . 10_557 ? C2 C1 O1 125.6(11) . . ? C1 C1 O1 111.8(6) 10_557 . ? C1 C2 C3 116.0(13) . . ? C3 C3 C2 121.4(8) 10_557 . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 28.14 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 0.525 _refine_diff_density_min -1.126 _refine_diff_density_rms 0.128