# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address 'Bellussi, Giuseppe' ; Eni S.p.A., Refining & Marketing Division, Via F. Martiano 26 San Doanto Milaese I-27100 Milano Italy ; 'Millini, Roberto' ; Eni S.p.A., Refining & Marketing Division, Via F. Martiano 26 San Doanto Milaese I-27100 Milano Italy ; 'Montanari, Erica' ; Eni S.p.A., Refining & Marketing Division, Via F. Martiano 26 San Doanto Milaese I-27100 Milano Italy ; 'Carati, Angela' ; Eni S.p.A., Refining & Marketing Division, Via F. Martiano 26 San Doanto Milaese I-27100 Milano Italy ; 'Rizzo, Caterina.' ; Eni S.p.A., Refining & Marketing Division, Via F. Martiano 26 San Doanto Milaese I-27100 Milano Italy ; "Parker, jr, Wallace O'Neil" ; Eni S.p.A., Refining & Marketing Division, Via F. Martiano 26 San Doanto Milaese I-27100 Milano Italy ; 'Cruciani, Giuseppe' ; Department of Physicas and Earth Sciences, University of Ferrara, Via Sarags\`iat 1, I-44100 Ferrara Italy ; 'de Angelis, Alberto' ; Eni S.p.A., Refining & Marketing Division, Via F. Martiano 26 San Doanto Milaese I-27100 Milano Italy ; 'Bonoldi, Lucia' ; Eni S.p.A., Refining & Marketing Division, Via F. Martiano 26 San Doanto Milaese I-27100 Milano Italy ; 'Zanardi, Stefano' ; Eni S.p.A., Refining & Marketing Division, Via F. Martiano 26 San Doanto Milaese I-27100 Milano Italy ; _publ_contact_author_address ; Eni S.p.A. Refining & Marketing Division Research Center of San Donato Milanese Milano Italy ; _publ_contact_author_email giuseppe.bellussi@eni.com _publ_contact_author_fax ? _publ_contact_author_phone +390252036555 #TrackingRef '- ECS-14_chem_com.cif' #============================================================================= # this information describes the project, paper etc. for the CIF # # Acta Cryst. Section C papers and editorial correspondence is generated # # from the information in this section # # # # (from) CIF submission form for Rietveld refinements (Acta Cryst. C) # # Version 14 December 1998 # #============================================================================= _publ_contact_author_name 'Giuseppe Bellussi' _publ_contact_letter ; ? ; _publ_requested_category ? _publ_requested_coeditor_name ? # TITLE AND AUTHOR LIST _publ_section_title ; A highly crystalline microporous hybrid organic-inorganic aluminosilicate resembling the AFI-type zeolite ; data_ECS-14 _database_code_depnum_ccdc_archive 'CCDC 884850' #SAMPLE PREPARATION DATA # (In the unusual case where multiple samples are used in a single # Rietveld study, this information should be moved into the phase # blocks) # The following three fields describe the preparation of the material. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure 0.0001 _pd_prep_temperature 298 _refine_ls_shift/su_max 0.06 _refine_ls_shift/su_mean 0.01 _computing_structure_refinement GSAS _refine_ls_number_parameters 123 _refine_ls_goodness_of_fit_all 3.0 _refine_ls_number_restraints 26 _refine_ls_matrix_type full # CHEMICAL, STRUCTURAL AND CRYSTAL DATA _pd_char_particle_morphology ? _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural H10.2Na13.8Si24Al24(C6H4)12O9662H2O _chemical_formula_analytical Na19.2B1.0Si29.3Al24(C6H4)14.2O91.2.48H2O _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products _symmetry_space_group_name_Hall ? _exptl_crystal_F_000 ? _exptl_crystal_density_diffrn ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _pd_char_colour white _cell_measurement_temperature 298 _cell_special_details ; ? ; _geom_special_details ? # The following item identifies the program(s) used (if appropriate). _computing_structure_solution ? #============================================================================== # Phase information from GSAS _cell_length_a 14.21306(3) _cell_length_b 14.21306 _cell_length_c 27.2081(1) _cell_angle_alpha 90.000 _cell_angle_beta 90.000 _cell_angle_gamma 120.000 _cell_volume 4759.97(3) _symmetry_space_group_name_H-M 'P 6/m c c' _diffrn_radiation_type synchrotron _diffrn_source 'ESRF station ID-31' _diffrn_radiation_probe x-ray _diffrn_radiation_polarisn_ratio 1.0 _diffrn_radiation_wavelength 0.4959 _diffrn_ambient_temperature 298 _pd_proc_ls_prof_R_factor 0.0460 _pd_proc_ls_prof_wR_factor 0.0640 _pd_proc_ls_prof_wR_expected 0.0216 _refine_ls_R_Fsqd_factor 0.14085 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 x-y,+x,+z 3 -y,x-y,+z 4 -x,-y,+z 5 y-x,-x,+z 6 +y,y-x,+z 7 y-x,+y,+z+1/2 8 -x,y-x,+z+1/2 9 -y,-x,+z+1/2 10 x-y,-y,+z+1/2 11 +x,x-y,+z+1/2 12 +y,+x,+z+1/2 -1 -x,-y,-z -2 y-x,-x,-z -3 +y,y-x,-z -4 +x,+y,-z -5 x-y,+x,-z -6 -y,x-y,-z -7 x-y,-y,-z+1/2 -8 +x,x-y,-z+1/2 -9 +y,+x,-z+1/2 -10 y-x,+y,-z+1/2 -11 -x,y-x,-z+1/2 -12 -y,-x,-z+1/2 loop_ _atom_type_symbol _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source Si 24.0 0.000 0.000 6.29150 2.43860 3.03530 32.3337 1.98910 0.67850 1.54100 81.6937 1.14070 International_Tables_Vol_C Al 24.0 0.000 0.000 6.42020 3.03870 1.90020 0.74260 1.59360 31.5472 1.96460 85.0886 1.11510 International_Tables_Vol_C Na 13.811 0.000 0.000 4.76260 3.28500 3.17360 8.84220 1.26740 0.31360 1.11280 129.424 0.67600 International_Tables_Vol_C O 158.019 0.000 0.000 3.04850 13.2771 2.28680 5.70110 1.54630 0.32390 0.86700 32.9089 0.25080 International_Tables_Vol_C C 72.0 0.000 0.000 2.31000 20.8439 1.02000 10.2075 1.58860 0.56870 0.86500 51.6512 0.21560 International_Tables_Vol_C # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_Wyckoff_symbol _atom_site_thermal_displace_type _atom_site_u_iso_or_equiv Si1 Si 0.6771(1) 0.1261(1) 0.12150(5) 1.000 24 m Uiso 0.0267(4) Al1 Al 0.4559(1) 0.1174(1) 0.15994(5) 1.000 24 m Uiso 0.0363(5) Na1 Na 0.6667 0.3333 0.1708(2) 1.000 8 h Uiso 0.0579(13) Na2 Na 0.5000 0.0000 0.2500 0.70(5) 6 f Uiso 0.1381(32) Na3 Na 1.0000 0.0000 0.2500 0.79(1) 2 a Uiso 0.221(17) O1 O 0.7912(2) 0.2120(2) 0.1495(1) 1.000 24 m Uiso 0.051(5) O2 O 0.3525(2) -0.0061(2) 0.1384(1) 1.000 24 m Uiso 0.051(5) O3 O 0.5876(2) 0.1548(2) 0.1380(1) 1.000 24 m Uiso 0.051(5) O4 O 0.4646(2) 0.1027(2) 0.2217(1) 1.000 24 m Uiso 0.051(5) C1 C 0.6880(3) 0.1369(3) 0.0519(1) 1.000 24 m Uiso 0.045(10) C3 C 0.6411(3) 0.0369(2) 0.0257(1) 1.000 24 m Uiso 0.045(10) C5 C 0.7384(3) 0.2351(2) 0.0248(1) 1.000 24 m Uiso 0.045(10) W1 O 0.7980(2) -0.0538(3) 0.0990(1) 0.78(4) 24 m Uiso 0.112(15) W4 O 0.7891(3) 0.0867(2) 0.2308(2) 0.56(3) 24 m Uiso 0.170(22) W5 O 0.8506(6) -0.0030(11) 0.1892(2) 0.61(5) 24 m Uiso 0.241(23) W6 O 0.0000 0.0000 -0.013(4) 0.20(1) 4 e Uiso 0.291(31) W7 O 0.1962(3) 0.0814(5) 0.0000 0.87(4) 12 l Uiso 0.111(44) W9 O 0.5886(9) 0.290(6) 0.2530(32) 0.14(2) 24 m Uiso 0.087(24) # If you change Z, be sure to change all 3 of the following _chemical_formula_sum 'C9 Al3 Na1.726 O19.675 Si3' _chemical_formula_weight 627.7 _cell_formula_units_Z 8 # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Si1 Na1 . . 3.3059(25) no Si1 O1 . . 1.6498(26) no Si1 O2 . 4_655 1.6061(38) no Si1 O3 . . 1.5826(40) no Si1 C1 . . 1.8989(30) no Al1 Na1 . . 3.0479(15) no Al1 O1 . 5_665 1.6326(41) no Al1 O2 . . 1.7330(29) no Al1 O3 . . 1.7746(35) no Al1 O4 . . 1.7050(31) no Al1 Na2 . . 3.1980(19) no Na1 Si1 . . 3.3059(25) no Na1 Si1 . 3_655 3.3065(21) no Na1 Si1 . 5_665 3.3071(24) no Na1 Al1 . . 3.0479(15) no Na1 Al1 . 3_655 3.0472(22) no Na1 Al1 . 5_665 3.0486(23) no Na1 O1 . . 3.0802(35) no Na1 O1 . 3_655 3.0814(26) no Na1 O1 . 5_665 3.0814(25) no Na1 O3 . . 2.3761(31) no Na1 O3 . 3_655 2.3762(31) no Na1 O3 . 5_665 2.3773(39) no Na1 W9 . . 2.4351(802) no Na1 W9 . 3_655 2.4346(850) no Na1 W9 . 5_665 2.4351(856) no Na1 W9 . . 2.4351(802) no Na1 W9 . . 2.4351(802) no Na1 W9 . . 2.4351(802) no O1 Si1 . . 1.6498(26) no O1 Al1 . 3_655 1.6326(26) no O1 Na1 . . 3.0802(35) no O2 Si1 . 4_655 1.6061(38) no O2 Al1 . . 1.7330(29) no O3 Si1 . . 1.5826(40) no O3 Al1 . . 1.7746(35) no O3 Na1 . . 2.3761(31) no C1 Si1 . . 1.8989(30) no C1 C3 . . 1.4235(46) no C1 C5 . . 1.4157(45) no O4 Al1 . . 1.7050(31) no O4 Na2 . . 1.9260(33) no C3 C1 . . 1.4235(46) no C3 C3 . . 0.0000 no C5 C1 . . 1.4157(45) no C5 C5 . . 0.0000 no Na2 Al1 . . 3.1980(19) no Na2 Al1 . 4_655 3.1980(19) no Na2 Al1 . . 3.1980(19) no Na2 Al1 . . 3.1980(19) no Na2 O4 . . 1.9260(33) no Na2 O4 . 4_655 1.9260(33) no Na2 O4 . . 1.9260(33) no Na2 O4 . . 1.9260(33) no W4 W4 . . 0.0000 no Na3 W5 . . 2.6754(95) no Na3 W5 . 2_545 2.6754(78) no Na3 W5 . 3_645 2.6754(132) no Na3 W5 . 4_755 2.6754(95) no Na3 W5 . 5_765 2.6754(78) no Na3 W5 . 6_665 2.6754(132) no Na3 W5 . . 2.6754(95) no Na3 W5 . . 2.6754(95) no Na3 W5 . . 2.6754(95) no Na3 W5 . . 2.6754(95) no Na3 W5 . . 2.6754(95) no Na3 W5 . . 2.6754(95) no W5 Na3 . . 2.6754(95) no W5 W5 . 2_545 2.1024(230) no W5 W5 . 6_665 2.1024(128) no W6 W6 . . 0.0000 no W9 Na1 . . 2.4351(802) no W9 Na1 . . 2.4351(802) no W9 W9 . 3_655 1.6677(565) no W9 W9 . 5_665 1.6677(673) no W9 W9 . . 0.0000 no W9 W9 . . 0.0000 no W9 W9 . . 0.0000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 Si1 O2 . . 4_655 106.95(16) no O1 Si1 O3 . . . 107.32(18) no O1 Si1 C1 . . . 112.99(17) no O2 Si1 O3 4_655 . . 112.03(18) no O2 Si1 C1 4_655 . . 109.82(18) no O3 Si1 C1 . . . 107.78(18) no Na1 Al1 O1 . . 5_665 75.69(13) no Na1 Al1 O2 . . . 164.04(15) no Na1 Al1 O3 . . . 51.10(12) no Na1 Al1 O4 . . . 86.13(13) no Na1 Al1 Na2 . . . 95.76(7) no O1 Al1 O2 5_665 . . 107.83(16) no O1 Al1 O3 5_665 . . 113.52(19) no O1 Al1 O4 5_665 . . 109.78(17) no O1 Al1 Na2 5_665 . . 139.97(14) no O2 Al1 O3 . . . 115.02(18) no O2 Al1 O4 . . . 106.59(17) no O2 Al1 Na2 . . . 91.06(13) no O3 Al1 O4 . . . 103.76(17) no O3 Al1 Na2 . . . 87.81(12) no O4 Al1 Na2 . . . 30.2(1) no Al1 Na1 Al1 . . 3_655 119.09(9) no Al1 Na1 Al1 . . 5_665 119.05(9) no Al1 Na1 O3 . . . 35.54(9) no Al1 Na1 O3 . . 3_655 141.48(13) no Al1 Na1 O3 . . 5_665 85.53(11) no Al1 Na1 W9 . . . 74.94(167) no Al1 Na1 W9 . . 3_655 96.08(167) no Al1 Na1 W9 . . 5_665 114.90(167) no Al1 Na1 W9 . . . 74.94(167) no Al1 Na1 W9 . . . 74.94(167) no Al1 Na1 W9 . . . 74.94(167) no Al1 Na1 Al1 3_655 . 5_665 119.07(9) no Al1 Na1 O3 3_655 . . 85.56(11) no Al1 Na1 O3 3_655 . 3_655 35.55(9) no Al1 Na1 O3 3_655 . 5_665 141.46(13) no Al1 Na1 W9 3_655 . . 114.93(167) no Al1 Na1 W9 3_655 . 3_655 74.96(167) no Al1 Na1 W9 3_655 . 5_665 96.09(167) no Al1 Na1 W9 3_655 . . 114.93(167) no Al1 Na1 W9 3_655 . . 114.93(167) no Al1 Na1 W9 3_655 . . 114.93(167) no Al1 Na1 O3 5_665 . . 141.44(13) no Al1 Na1 O3 5_665 . 3_655 85.53(11) no Al1 Na1 O3 5_665 . 5_665 35.53(9) no Al1 Na1 W9 5_665 . . 96.05(167) no Al1 Na1 W9 5_665 . 3_655 114.90(167) no Al1 Na1 W9 5_665 . 5_665 74.92(167) no Al1 Na1 W9 5_665 . . 96.05(167) no Al1 Na1 W9 5_665 . . 96.05(167) no Al1 Na1 W9 5_665 . . 96.05(167) no O3 Na1 O3 . . 3_655 106.77(14) no O3 Na1 O3 . . 5_665 106.73(14) no O3 Na1 W9 . . . 99.37(167) no O3 Na1 W9 . . 3_655 99.30(167) no O3 Na1 W9 . . 5_665 135.38(167) no O3 Na1 W9 . . . 99.37(167) no O3 Na1 W9 . . . 99.37(167) no O3 Na1 W9 . . . 99.37(167) no O3 Na1 O3 3_655 . 5_665 106.73(14) no O3 Na1 W9 3_655 . . 135.38(167) no O3 Na1 W9 3_655 . 3_655 99.38(167) no O3 Na1 W9 3_655 . 5_665 99.29(167) no O3 Na1 W9 3_655 . . 135.38(167) no O3 Na1 W9 3_655 . . 135.38(167) no O3 Na1 W9 3_655 . . 135.38(167) no O3 Na1 W9 5_665 . . 99.26(167) no O3 Na1 W9 5_665 . 3_655 135.34(167) no O3 Na1 W9 5_665 . 5_665 99.34(167) no O3 Na1 W9 5_665 . . 99.26(167) no O3 Na1 W9 5_665 . . 99.26(167) no O3 Na1 W9 5_665 . . 99.26(167) no W9 Na1 W9 . . 3_655 40.05(235) no W9 Na1 W9 . . 5_665 40.05(235) no W9 Na1 W9 3_655 . 5_665 40.05(235) no W9 Na1 W9 3_655 . . 40.05(235) no W9 Na1 W9 3_655 . . 40.05(235) no W9 Na1 W9 3_655 . . 40.05(235) no W9 Na1 W9 5_665 . . 40.05(235) no W9 Na1 W9 5_665 . . 40.05(235) no W9 Na1 W9 5_665 . . 40.05(235) no Si1 O1 Al1 . . 3_655 147.33(19) no Si1 O2 Al1 4_655 . . 144.23(21) no Si1 O3 Al1 . . . 151.84(24) no Si1 O3 Na1 . . . 111.68(17) no Al1 O3 Na1 . . . 93.36(15) no Si1 C1 C3 . . . 116.18(21) no Si1 C1 C5 . . . 125.42(22) no C3 C1 C5 . . . 118.40(31) no Al1 O4 Na2 . . . 123.35(17) no Al1 Na2 Al1 . . 4_655 79.97(5) no Al1 Na2 O4 . . . 26.45(9) no Al1 Na2 O4 . . 4_655 106.40(9) no Al1 Na2 O4 . . . 26.45(9) no Al1 Na2 O4 . . . 26.45(9) no Al1 Na2 Al1 4_655 . . 79.97(5) no Al1 Na2 Al1 4_655 . . 79.97(5) no Al1 Na2 O4 4_655 . . 106.40(9) no Al1 Na2 O4 4_655 . 4_655 26.45(9) no Al1 Na2 O4 4_655 . . 106.40(9) no Al1 Na2 O4 4_655 . . 106.40(9) no Al1 Na2 O4 . . . 26.45(9) no Al1 Na2 O4 . . 4_655 106.40(9) no Al1 Na2 O4 . . . 26.45(9) no Al1 Na2 O4 . . . 26.45(9) no Al1 Na2 O4 . . . 26.45(9) no Al1 Na2 O4 . . 4_655 106.40(9) no Al1 Na2 O4 . . . 26.45(9) no Al1 Na2 O4 . . . 26.45(9) no O4 Na2 O4 . . 4_655 132.83(12) no O4 Na2 O4 4_655 . . 132.83(12) no O4 Na2 O4 4_655 . . 132.83(12) no W5 Na3 W5 . . 2_545 46.27(32) no W5 Na3 W5 . . 3_645 85.77(32) no W5 Na3 W5 . . 4_755 103.60(32) no W5 Na3 W5 . . 5_765 85.77(32) no W5 Na3 W5 . . 6_665 46.27(32) no W5 Na3 W5 2_545 . 3_645 46.27(32) no W5 Na3 W5 2_545 . 4_755 85.77(32) no W5 Na3 W5 2_545 . 5_765 103.60(32) no W5 Na3 W5 2_545 . 6_665 85.77(32) no W5 Na3 W5 2_545 . . 46.27(32) no W5 Na3 W5 2_545 . . 46.27(32) no W5 Na3 W5 2_545 . . 46.27(32) no W5 Na3 W5 2_545 . . 46.27(32) no W5 Na3 W5 2_545 . . 46.27(32) no W5 Na3 W5 2_545 . . 46.27(32) no W5 Na3 W5 3_645 . 4_755 46.27(32) no W5 Na3 W5 3_645 . 5_765 85.77(32) no W5 Na3 W5 3_645 . 6_665 103.60(32) no W5 Na3 W5 3_645 . . 85.77(32) no W5 Na3 W5 3_645 . . 85.77(32) no W5 Na3 W5 3_645 . . 85.77(32) no W5 Na3 W5 3_645 . . 85.77(32) no W5 Na3 W5 3_645 . . 85.77(32) no W5 Na3 W5 3_645 . . 85.77(32) no W5 Na3 W5 4_755 . 5_765 46.27(32) no W5 Na3 W5 4_755 . 6_665 85.77(32) no W5 Na3 W5 4_755 . . 103.60(32) no W5 Na3 W5 4_755 . . 103.60(32) no W5 Na3 W5 4_755 . . 103.60(32) no W5 Na3 W5 4_755 . . 103.60(32) no W5 Na3 W5 4_755 . . 103.60(32) no W5 Na3 W5 4_755 . . 103.60(32) no W5 Na3 W5 5_765 . 6_665 46.27(32) no W5 Na3 W5 5_765 . . 85.77(32) no W5 Na3 W5 5_765 . . 85.77(32) no W5 Na3 W5 5_765 . . 85.77(32) no W5 Na3 W5 5_765 . . 85.77(32) no W5 Na3 W5 5_765 . . 85.77(32) no W5 Na3 W5 5_765 . . 85.77(32) no W5 Na3 W5 6_665 . . 46.27(32) no W5 Na3 W5 6_665 . . 46.27(32) no W5 Na3 W5 6_665 . . 46.27(32) no W5 Na3 W5 6_665 . . 46.27(32) no W5 Na3 W5 6_665 . . 46.27(32) no W5 Na3 W5 6_665 . . 46.27(32) no Na1 W9 W9 . . 3_655 69.96(344) no Na1 W9 W9 . . 5_665 69.98(344) no Na1 W9 W9 . . 3_655 69.96(344) no Na1 W9 W9 . . 5_665 69.98(344) no W9 W9 W9 3_655 . 5_665 60.00(319) no