# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 182/1446 data_1 _publ_requested_journal ' ChemComm' _publ_contact_author ; Professor Hwu, Shiou-Jyh Department of Chemistry Clemson University Clemson, SC 29634-1905 U.S.A. ; _publ_contact_author_phone '864 656 5031' _publ_contact_author_fax '864 656 6613' _publ_contact_author_email 'shwu@clemson.edu' _audit_creation_method 'manual editing of form.cif' _publ_section_title ; Cs~2~Al~2~P~2~O~9~: an exception to Lowenstein's rule. Synthesis and characterization of a novel layered aluminophosphate containing linear Al-O-Al linkages ; loop_ _publ_author_name _publ_author_address 'Huang, Qun' ; Department of Chemistry Clemson University Clemson, SC 29634-1905 U.S.A. ; 'Hwu, Shiou-Jyh' ; Department of Chemistry Clemson University Clemson, SC 29634-1905 U.S.A. ; #------------------------------------------------------------------------------ _chemical_formula_sum 'Cs2 Al2 P2 O9' _chemical_formula_weight 525.7 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz ' x, y, z' ' -x, -y, -z' _cell_length_a 4.925(2) _cell_length_b 7.121(2) _cell_length_c 8.066(2) _cell_angle_alpha 96.51(2) _cell_angle_beta 107.12(2) _cell_angle_gamma 108.68(2) _cell_volume 249.3(1) _cell_formula_units_Z 1 _cell_measurement_temperature 298 _cell_measurement_reflns_used 50 _cell_measurement_theta_min 17.84 _cell_measurement_theta_max 27.50 _exptl_crystal_description column _exptl_crystal_colour colorless _exptl_crystal_size_max 0.240 _exptl_crystal_size_mid 0.048 _exptl_crystal_size_min 0.052 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 3.502 _exptl_crystal_density_method ? _exptl_crystal_F_000 238 _exptl_absorpt_coefficient_mu 7.835 _exptl_absorpt_correction_type 'Semi-empirical' _exptl_absorpt_correction_T_min 0.6808 _exptl_absorpt_correction_T_max 0.8257 _exptl_crystal_preparation ; The crystal was mounted with epoxy onto the end of a glass fiber. ; #------------------------------------------------------------------------------ _diffrn_special_details ; Data were collected using an \w--2\q scan mode with a speed range of 1.0-14.65\%/min, and corrected for Lorentz and polarization effects. ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nicolet R3mV' _diffrn_measurement_method \w--2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2463 _reflns_number_observed 1110 _reflns_number_total 2463 _reflns_number_unique 1158 _reflns_observed_criterion (F)>4\s(F) _diffrn_reflns_av_R_equivalents 1.00% _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 27.5 _computing_data_collection 'Siemens P3 software 1976' _computing_cell_refinement 'Siemens P3 software 1976' _computing_data_reduction 'SHELXTL-Plus (Sheldrick, 1990)' _computing_structure_solution 'SHELXTL-Plus (Sheldrick, 1990)' _computing_structure_refinement 'SHELXTL-Plus (Sheldrick, 1990)' #------------------------------------------------------------------------------ _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '1/(\s^2^(F)+0.0005F^2^)' _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method 'Larson (1970)' _refine_ls_extinction_coef 0.0008(4) _atom_type_scat_source 'International Tables (Cromer & Waber, 1974)' _refine_ls_number_reflns 1110 _refine_ls_number_parameters 71 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_obs 0.0235 _refine_ls_wR_factor_obs 0.0345 _refine_ls_goodness_of_fit_obs 1.36 _refine_ls_R_factor_all 0.0242 _refine_ls_wR_factor_all 0.348 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 1.60 _refine_diff_density_min -1.04 #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags Cs(1) 0.2283(1) 0.7940(1) 0.6504(1) 0.023(1) Uani d . 1.00 . P(1) -0.3882(2) 0.3504(1) 0.7732(1) 0.009(1) Uani d . 1.00 . Al(1) -0.1493(2) 0.7646(1) 0.0330(1) 0.010(1) Uani d . 1.00 . O(1) -0.9036(6) 0.6995(4) 0.2020(3) 0.017(1) Uani d . 1.00 . O(2) -0.7186(6) 0.4153(4) 0.1697(3) 0.018(1) Uani d . 1.00 . O(3) -0.5261(6) 0.2572(4) 0.9082(3) 0.017(1) Uani d . 1.00 . O(4) -0.6027(6) 0.2676(4) 0.5863(3) 0.022(1) Uani d . 1.00 . O(5) 0 0 0 0.024(1) Uani d . 0.50 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cs(1) 0.022(1) 0.023(1) 0.021(1) 0.008(1) 0.006(1) 0.004(1) P(1) 0.009(1) 0.009(1) 0.010(1) 0.003(1) 0.003(1) 0.001(1) Al(1) 0.011(1) 0.006(1) 0.014(1) 0.003(1) 0.007(1) 0.004(1) O(1) 0.015(1) 0.026(1) 0.020(1) 0.013(1) 0.010(1) 0.011(1) O(2) 0.030(1) 0.009(1) 0.016(1) 0.006(1) 0.008(1) 0.003(1) O(3) 0.015(1) 0.021(1) 0.023(1) 0.009(1) 0.012(1) 0.012(1) O(4) 0.018(1) 0.027(1) 0.013(1) 0.007(1) -0.002(1) -0.001(1) O(5) 0.027(2) 0.011(2) 0.040(2) 0.007(1) 0.020(2) 0.014(2) #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Cs(1) O(1) 3.427(3) . 1_655 Cs(1) O(1) 3.808(2) . 2_576 Cs(1) O(2) 3.297(3) . 2_466 Cs(1) O(2) 3.300(3) . 2_566 Cs(1) O(3) 3.328(3) . 1_665 Cs(1) O(3) 3.539(3) . 2_567 Cs(1) O(4) 3.344(3) . 1_665 Cs(1) O(4) 2.969(3) . 2_466 Cs(1) O(4) 3.104(3) . 2_566 Cs(1) O(5) 3.655(1) . 1_566 Cs(1) O(5) 3.705(1) . 1_666 P(1) O(1) 1.551(3) . 2_466 P(1) O(2) 1.547(3) . 2_466 P(1) O(3) 1.548(3) . . P(1) O(4) 1.483(2) . . Al(1) O(1) 1.751(3) . 1_655 Al(1) O(2) 1.762(3) . 2_465 Al(1) O(3) 1.763(3) . 2_466 Al(1) O(5) 1.688(1) . 2_565 #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 O(1) Cs(1) O(1) 99.2(1) 1_655 . 2_576 O(1) Cs(1) O(2) 124.3(1) 1_655 . 2_466 O(1) Cs(1) O(2) 132.3(1) 2_576 . 2_466 O(1) Cs(1) O(2) 106.7(1) 1_655 . 2_566 O(1) Cs(1) O(2) 87.6(1) 2_576 . 2_566 O(2) Cs(1) O(2) 96.6(1) 2_466 . 2_566 O(1) Cs(1) O(3) 124.0(1) 1_655 . 1_665 O(1) Cs(1) O(3) 39.8(1) 2_576 . 1_665 O(2) Cs(1) O(3) 94.6(1) 2_466 . 1_665 O(2) Cs(1) O(3) 106.6(1) 2_566 . 1_665 O(1) Cs(1) O(3) 154.9(1) 1_655 . 2_567 O(1) Cs(1) O(3) 85.3(1) 2_576 . 2_567 O(2) Cs(1) O(3) 64.1(1) 2_466 . 2_567 O(2) Cs(1) O(3) 48.5(1) 2_566 . 2_567 O(3) Cs(1) O(3) 74.4(1) 1_665 . 2_567 O(1) Cs(1) O(4) 79.6(1) 1_655 . 1_665 O(1) Cs(1) O(4) 40.1(1) 2_576 . 1_665 O(2) Cs(1) O(4) 123.8(1) 2_466 . 1_665 O(2) Cs(1) O(4) 126.8(1) 2_566 . 1_665 O(3) Cs(1) O(4) 44.5(1) 1_665 . 1_665 O(3) Cs(1) O(4) 117.0(1) 2_567 . 1_665 O(1) Cs(1) O(4) 63.9(1) 1_655 . 2_466 O(1) Cs(1) O(4) 123.8(1) 2_576 . 2_466 O(2) Cs(1) O(4) 69.4(1) 2_466 . 2_466 O(2) Cs(1) O(4) 147.5(1) 2_566 . 2_466 O(3) Cs(1) O(4) 103.7(1) 1_665 . 2_466 O(3) Cs(1) O(4) 133.0(1) 2_567 . 2_466 O(4) Cs(1) O(4) 83.7(1) 1_665 . 2_466 O(1) Cs(1) O(4) 44.5(1) 1_655 . 2_566 O(1) Cs(1) O(4) 76.9(1) 2_576 . 2_566 O(2) Cs(1) O(4) 147.9(1) 2_466 . 2_566 O(2) Cs(1) O(4) 67.8(1) 2_566 . 2_566 O(3) Cs(1) O(4) 116.4(1) 1_665 . 2_566 O(3) Cs(1) O(4) 114.3(1) 2_567 . 2_566 O(4) Cs(1) O(4) 86.6(1) 1_665 . 2_566 O(4) Cs(1) O(4) 108.4(1) 2_466 . 2_566 O(1) Cs(1) O(5) 144.8(1) 1_655 . 1_566 O(1) Cs(1) O(5) 86.2(1) 2_576 . 1_566 O(2) Cs(1) O(5) 47.3(1) 2_466 . 1_566 O(2) Cs(1) O(5) 108.2(1) 2_566 . 1_566 O(3) Cs(1) O(5) 47.3(1) 1_665 . 1_566 O(3) Cs(1) O(5) 59.7(1) 2_567 . 1_566 O(4) Cs(1) O(5) 82.8(1) 1_665 . 1_566 O(4) Cs(1) O(5) 84.1(1) 2_466 . 1_566 O(4) Cs(1) O(5) 162.7(1) 2_566 . 1_566 O(1) Cs(1) O(5) 124.2(1) 1_655 . 1_666 O(1) Cs(1) O(5) 45.5(1) 2_576 . 1_666 O(2) Cs(1) O(5) 108.8(1) 2_466 . 1_666 O(2) Cs(1) O(5) 46.8(1) 2_566 . 1_666 O(3) Cs(1) O(5) 61.0(1) 1_665 . 1_666 O(3) Cs(1) O(5) 45.7(1) 2_567 . 1_666 O(4) Cs(1) O(5) 85.1(1) 1_665 . 1_666 O(4) Cs(1) O(5) 164.6(1) 2_466 . 1_666 O(4) Cs(1) O(5) 81.4(1) 2_566 . 1_666 O(3) P(1) O(4) 112.8(1) . . . O(3) P(1) O(1) 105.8(2) . . 2_466 O(4) P(1) O(1) 110.5(2) . . 2_466 O(3) P(1) O(2) 107.9(2) . . 2_466 O(4) P(1) O(2) 112.5(2) . . 2_466 O(1) P(1) O(2) 106.9(2) 2_466 . 2_466 O(1) Al(1) O(2) 110.2(2) 1_655 . 1_465 O(1) Al(1) O(3) 106.4(2) 1_655 . 2_466 O(2) Al(1) O(3) 106.2(1) 1_465 . 2_466 O(1) Al(1) O(5) 115.3(1) 1_655 . 1_565 O(2) Al(1) O(5) 108.9(1) 1_465 . 1_565 O(3) Al(1) O(5) 109.4(1) 2_466 . 1_565 P(1) O(1) Al(1) 135.7(2) 2_466 . 1_455 P(1) O(2) Al(1) 135.7(2) 2_466 . 1_465 P(1) O(3) Al(1) 136.9(2) . . 2_466 Al(1) O(5) Al(1) 180.0(1) 1_545 . 2_565 #==END