#------------------------------------------------------------------------------ #$Date: 2014-03-15 13:45:36 +0200 (Sat, 15 Mar 2014) $ #$Revision: 106525 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/10/16/7101659.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7101659 loop_ _publ_author_name 'Comotti, Angiolina' 'Bracco, Silvia' 'Ferretti, Lisa' 'Mauri, Michele' 'Simonutti, Roberto' 'Sozzani, Piero' _publ_section_title ; A single-crystal imprints macroscopic orientation on xenon atoms. ; _journal_issue 4 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 350 _journal_page_last 352 _journal_year 2007 _chemical_formula_sum 'C18 H12 N3 O6 P3' _chemical_formula_weight 459.23 _chemical_melting_point 249 _chemical_name_common tris-o-phenylenedioxyspirocyclotriphosphazene _space_group_IT_number 176 _symmetry_cell_setting hexagonal _symmetry_Int_Tables_number 176 _symmetry_space_group_name_Hall '-P 6c' _symmetry_space_group_name_H-M 'P 63/m' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 2 _cell_length_a 11.454(5) _cell_length_b 11.454(5) _cell_length_c 10.160(5) _cell_measurement_reflns_used 266 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 28.14 _cell_measurement_theta_min 3.56 _cell_volume 1154.4(9) _computing_cell_refinement CrysAlis _computing_data_collection CrysAlis _computing_data_reduction CrysAlis _computing_molecular_graphics Diamond _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.944 _diffrn_measured_fraction_theta_max 0.944 _diffrn_measurement_device_type 'Oxford Xcalibur' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.1693 _diffrn_reflns_av_sigmaI/netI 0.1257 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 8016 _diffrn_reflns_theta_full 28.14 _diffrn_reflns_theta_max 28.14 _diffrn_reflns_theta_min 3.56 _exptl_absorpt_coefficient_mu 0.293 _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.286 _exptl_crystal_description 'hexagonal prism' _exptl_crystal_F_000 468 _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.080 _exptl_crystal_size_min 0.080 _refine_diff_density_max 0.525 _refine_diff_density_min -1.126 _refine_diff_density_rms 0.128 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.447 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 49 _refine_ls_number_reflns 949 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.447 _refine_ls_R_factor_all 0.1920 _refine_ls_R_factor_gt 0.0856 _refine_ls_shift/su_max 0.107 _refine_ls_shift/su_mean 0.032 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+25.1800P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1246 _refine_ls_wR_factor_ref 0.3027 _reflns_number_gt 862 _reflns_number_total 949 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file b612002d.txt _[local]_cod_data_source_block compound_1 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' 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' 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 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) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 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 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 . _cod_database_code 7101659 _journal_paper_doi 10.1039/b612002d