#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/4/4000411.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_4000411 _journal_name_full 'Chemistry of Materials' _journal_year 2004 _chemical_formula_sum 'C7 H11 Al4 F N2 O16.50 P4' _chemical_formula_moiety 'C7 H11 Al4 F N2 O16.50 P4' _chemical_formula_weight 637.98 _symmetry_space_group_name_H-M 'C2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.759(3) _cell_length_b 13.8214(18) _cell_length_c 14.2237(18) _cell_angle_alpha 90 _cell_angle_beta 98.849(4) _cell_angle_gamma 90 _cell_volume 4226.7(9) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_theta_min 1.83 _cell_measurement_theta_max 29.37 _exptl_crystal_description Needle _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.005 _exptl_crystal_density_diffrn 2.005 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2560 _exptl_absorpt_coefficient_mu 0.62 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.6875 _diffrn_radiation_type Synchrotron _diffrn_radiation_monochromator silicon _diffrn_reflns_av_R_equivalents 0.0519 _diffrn_reflns_av_unetI/netI 0.0991 _diffrn_reflns_number 8454 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 29.37 _diffrn_reflns_theta_full 24 _diffrn_measured_fraction_theta_full 0.895 _diffrn_measured_fraction_theta_max 0.781 _reflns_number_total 5039 _reflns_number_gt 3254 _reflns_threshold_expression >2sigma(I) _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^)+(0.0817P)^2^+2.9573P] 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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 5039 _refine_ls_number_parameters 315 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1118 _refine_ls_R_factor_gt 0.0628 _refine_ls_wR_factor_ref 0.1644 _refine_ls_wR_factor_gt 0.1441 _refine_ls_goodness_of_fit_ref 1.01 _refine_ls_restrained_S_all 1.01 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 0.897 _refine_diff_density_min -0.625 _refine_diff_density_rms 0.138 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0028 0.0015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0056 0.0031 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0164 0.0096 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0605 0.0482 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.097 0.0885 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0101 0.0056 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.05959(6) 0.12051(8) 0.01465(9) 0.0117(3) Uani 1 1 d . . . P2 P 0.17164(6) -0.21536(7) -0.10591(8) 0.0091(2) Uani 1 1 d . . . P3 P 0.26241(6) 0.11092(7) 0.06219(8) 0.0089(2) Uani 1 1 d . . . P4 P 0.15797(6) -0.11435(8) 0.20493(8) 0.0107(3) Uani 1 1 d . . . Al5 Al 0.16167(7) 0.20348(9) -0.09108(9) 0.0091(3) Uani 1 1 d . . . Al6 Al 0.08374(7) -0.10027(9) 0.00792(10) 0.0129(3) Uani 1 1 d . . . Al7 Al 0.24608(7) -0.10860(9) 0.05953(10) 0.0123(3) Uani 1 1 d . . . Al8 Al 0.16015(7) 0.10872(9) 0.19667(10) 0.0114(3) Uani 1 1 d . . . F1 F 0.16788(14) -0.04470(18) 0.0268(2) 0.0178(6) Uani 1 1 d . . . O1 O 0.22897(16) -0.1626(2) -0.0550(2) 0.0126(7) Uani 1 1 d . . . O2 O 0.06186(19) 0.0180(2) -0.0248(3) 0.0226(9) Uani 1 1 d . . . O3 O 0.22339(16) 0.1355(2) -0.0337(2) 0.0124(7) Uani 1 1 d . . . O4 O 0.11318(17) -0.1871(2) -0.0648(2) 0.0150(7) Uani 1 1 d . . . O5 O 0.22535(17) 0.1317(2) 0.1424(2) 0.0150(7) Uani 1 1 d . . . O6 O 0.09876(17) -0.1272(2) 0.1326(2) 0.0138(7) Uani 1 1 d . . . O7 O -0.00718(16) 0.1541(2) 0.0104(2) 0.0141(7) Uani 1 1 d . . . O8 O 0.28447(17) 0.00570(19) 0.0636(2) 0.0126(7) Uani 1 1 d . . . O9 O 0.15195(17) 0.1788(2) -0.2107(2) 0.0161(8) Uani 1 1 d . . . O10 O 0.17882(16) 0.32662(19) -0.0764(2) 0.0117(7) Uani 1 1 d . . . O11 O 0.18042(16) -0.3253(2) -0.0945(2) 0.0113(7) Uani 1 1 d . . . O12 O 0.09318(17) 0.1886(2) -0.0449(3) 0.0189(8) Uani 1 1 d . . . O13 O 0.16196(17) 0.1915(2) 0.2881(2) 0.0149(7) Uani 1 1 d . . . O14 O 0.21551(17) -0.1449(2) 0.1634(2) 0.0179(8) Uani 1 1 d . . . O15 O 0.09222(19) 0.1252(3) 0.1172(3) 0.0253(9) Uani 1 1 d . . . O16 O 0.16478(18) -0.0090(2) 0.2400(2) 0.0163(8) Uani 1 1 d . . . N1 N 0.5645(3) 0.0736(4) 0.8922(4) 0.0364(13) Uani 1 1 d . . . H1 H 0.603 0.0952 0.9014 0.044 Uiso 1 1 calc R . . C2 C 0.5183(3) 0.1371(4) 0.8795(5) 0.0365(16) Uani 1 1 d . . . H2 H 0.5273 0.2044 0.8815 0.044 Uiso 1 1 calc R . . C3 C 0.4587(3) 0.1067(4) 0.8638(5) 0.0327(14) Uani 1 1 d . . . H3 H 0.426 0.1529 0.8536 0.039 Uiso 1 1 calc R . . C4 C 0.4440(3) 0.0056(3) 0.8622(4) 0.0190(11) Uani 1 1 d . . . C5 C 0.4951(3) -0.0583(4) 0.8771(4) 0.0312(14) Uani 1 1 d . . . H5 H 0.4881 -0.1261 0.8772 0.037 Uiso 1 1 calc R . . C6 C 0.5548(3) -0.0236(5) 0.8915(5) 0.0359(15) Uani 1 1 d . . . H6 H 0.5891 -0.067 0.9008 0.043 Uiso 1 1 calc R . . N7 N 0.3847(3) -0.0218(4) 0.8470(4) 0.0334(12) Uani 1 1 d . . . C8 C 0.3332(3) 0.0453(5) 0.8325(5) 0.0443(18) Uani 1 1 d . . . H8A H 0.3378 0.0925 0.8845 0.053 Uiso 1 1 calc R . . H8B H 0.2941 0.0098 0.8312 0.053 Uiso 1 1 calc R . . H8C H 0.3328 0.0791 0.7718 0.053 Uiso 1 1 calc R . . C9 C 0.3698(4) -0.1260(5) 0.8446(6) 0.052(2) Uani 1 1 d . . . H9A H 0.3974 -0.1602 0.8075 0.063 Uiso 1 1 calc R . . H9B H 0.3265 -0.1354 0.8151 0.063 Uiso 1 1 calc R . . H9C H 0.3756 -0.1515 0.9097 0.063 Uiso 1 1 calc R . . OW1 O 0.5 -0.2701(9) 0.75 0.061(4) Uiso 0.6 2 d SP . . OW2 O 0.5 -0.413(3) 0.75 0.053(10) Uiso 0.2 2 d SP . . OW3 O 0.5 0.311(3) 0.75 0.068(12) Uiso 0.2 2 d SP . . 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 0.0147(7) 0.0106(5) 0.0098(5) 0.0013(4) 0.0019(5) 0.0011(4) P2 0.0134(7) 0.0094(5) 0.0052(5) 0.0000(4) 0.0037(5) -0.0005(4) P3 0.0133(7) 0.0063(4) 0.0071(5) 0.0003(4) 0.0013(4) 0.0009(4) P4 0.0157(7) 0.0107(5) 0.0064(5) 0.0000(4) 0.0039(5) -0.0013(4) Al5 0.0152(8) 0.0070(5) 0.0049(6) 0.0007(4) 0.0010(5) -0.0006(5) Al6 0.0218(9) 0.0095(6) 0.0080(6) -0.0010(5) 0.0042(6) 0.0034(5) Al7 0.0231(9) 0.0066(5) 0.0074(6) 0.0003(4) 0.0030(6) -0.0027(5) Al8 0.0183(9) 0.0121(6) 0.0040(6) -0.0018(4) 0.0026(6) 0.0009(5) F1 0.0228(19) 0.0171(13) 0.0136(15) 0.0018(10) 0.0031(13) -0.0001(11) O1 0.015(2) 0.0159(14) 0.0070(15) 0.0005(11) 0.0025(14) -0.0001(12) O2 0.030(3) 0.0119(15) 0.029(2) -0.0002(13) 0.0126(19) -0.0019(14) O3 0.017(2) 0.0120(14) 0.0085(15) 0.0030(11) 0.0011(14) 0.0047(12) O4 0.018(2) 0.0165(15) 0.0125(17) -0.0062(12) 0.0072(15) -0.0031(13) O5 0.017(2) 0.0189(15) 0.0098(16) -0.0042(12) 0.0051(15) 0.0007(13) O6 0.015(2) 0.0184(15) 0.0080(15) 0.0030(11) 0.0031(14) -0.0026(13) O7 0.012(2) 0.0153(15) 0.0158(17) -0.0020(12) 0.0040(14) 0.0011(12) O8 0.018(2) 0.0055(12) 0.0139(16) 0.0007(11) 0.0029(14) -0.0007(12) O9 0.025(2) 0.0169(15) 0.0059(16) -0.0028(11) 0.0006(15) 0.0016(13) O10 0.0131(19) 0.0058(12) 0.0168(17) -0.0001(11) 0.0040(14) -0.0010(12) O11 0.013(2) 0.0091(13) 0.0116(16) 0.0013(11) 0.0013(14) -0.0004(12) O12 0.017(2) 0.0165(15) 0.025(2) 0.0046(13) 0.0095(17) -0.0016(14) O13 0.024(2) 0.0145(14) 0.0061(16) -0.0040(11) 0.0033(15) 0.0016(13) O14 0.017(2) 0.0264(17) 0.0118(17) -0.0026(13) 0.0057(15) 0.0022(14) O15 0.022(2) 0.045(2) 0.0082(17) -0.0031(15) -0.0015(16) 0.0077(17) O16 0.028(2) 0.0136(15) 0.0086(16) -0.0028(11) 0.0080(15) -0.0047(13) N1 0.030(4) 0.053(3) 0.026(3) -0.006(2) 0.005(3) -0.015(3) C2 0.040(5) 0.033(3) 0.037(4) 0.000(2) 0.007(3) -0.010(3) C3 0.039(4) 0.028(3) 0.031(3) -0.006(2) 0.006(3) -0.010(3) C4 0.018(3) 0.021(2) 0.018(3) -0.0033(18) 0.006(2) -0.005(2) C5 0.037(4) 0.031(3) 0.025(3) -0.002(2) 0.001(3) 0.003(3) C6 0.028(4) 0.055(4) 0.025(3) -0.002(3) 0.005(3) 0.006(3) N7 0.029(3) 0.040(3) 0.032(3) -0.003(2) 0.007(3) -0.006(2) C8 0.030(5) 0.067(5) 0.034(4) 0.000(3) 0.002(3) 0.007(3) C9 0.061(6) 0.042(4) 0.058(5) -0.010(3) 0.021(5) -0.032(4)