Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 ---------- X-Sun-Charset: us-ascii X-Sun-Content-Lines: 764 data_global #data_CRYSTALS_cif _audit_creation_date 15 05 01 _audit_creation_method CRYSTALS #**************************************************************************** #SUBMISSION DETAILS _publ_contact_author_name 'Dr. Bonhomme' _publ_contact_author_address ; Laboratoire de Chimie de la Matiere Condensee, Universite P. et M. Curie, 4 place Jussieu, 75252 Paris cedex 05, France ; _publ_contact_author_phone ' 33 1 44 27 41 35 ' _publ_contact_author_fax ' 33 1 44 27 47 69 ' _publ_contact_author_email ' bonhomme@ccr.jussieu.fr ' _publ_requested_journal J. Chem. Soc. Dalton Trans' _journal_coden_Cambridge 186 _publ_requested_coeditor_name ' ? ' _publ_contact_letter ; ; #============================================================================= #TITLE AND AUTHOR LIST _publ_section_title ; Cubane Shaped Clusters, Precursors for Aluminophosphate Frameworks: a Solid State Multinuclear NMR Study, in Time and Frequency Domains ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Azais, T.' ; Laboratoire de Chimie de la Matiere Condensee, Universite P. et M. Curie, 4 place Jussieu, 75252 Paris cedex 05, France ; 'Bonhomme, C.' ; Laboratoire de Chimie de la Matiere Condensee, Universite P. et M. Curie, 4 place Jussieu, 75252 Paris cedex 05, France ; 'Bonhomme-Coury, L.' ; Laboratoire Ceramiques et Materiaux Mineraux, Ecole Superieure de Physique et Chimie Industrielles de la Ville de Paris, 10 rue Vauquelin, 75231 Paris cedex 05, France ; 'Vaissermann, J.' ; Laboratoire de Chimie Inorganique et Materiaux Moleculaires, Universite P. et M. Curie, 4 place Jussieu, 75252 Paris cedex 05, France ; #============================================================================== #========================================================================== _computing_data_collection 'CAD-4 software (Enraf-Nonius, 1989)' _computing_cell_refinement 'CAD-4 software (Enraf-Nonius, 1989)' _computing_data_reduction ; RC93 (Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. 1994) ; _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_molecular_graphics ; CAMERON (Watkin, Prout & Pearce, 1996) ; # _computing_structure_solution 'SHELXS86 (Sheldrick, 1986)' #========================================================================== # Compound 1 data_1 _database_code_CSD 165094 #========================================================================== _chemical_melting_point ? _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device 'Enraf-nonius CAD4 ' _refine_ls_matrix_type 'full' _refine_ls_weighting_scheme ; Chebychev polynomial (Carruthers & Watkin, 1979) ; _atom_sites_solution_primary 'Direct_Methods' _atom_sites_solution_hydrogens 'Geometric' _refine_ls_hydrogen_treatment ; H atoms placed geometrically after each cycle ; #**************************************************************************** _chemical_name_systematic ; # IUPAC name, in full ? ; _cell_length_a 15.379(8) _cell_angle_alpha 90 _cell_length_b 15.379(8) _cell_angle_beta 90 _cell_length_c 14.410(3) _cell_angle_gamma 90 _cell_volume 3408(3) _symmetry_cell_setting 'Tetragonal ' _symmetry_space_group_name_H-M 'I -4 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' 'x+1/2,y+1/2,z+1/2' 'y,-x,-z' 'y+1/2,-x+1/2,-z+1/2' '-x,-y,z' '-x+1/2,-y+1/2,z+1/2' '-y,x,-z' '-y+1/2,x+1/2,-z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' 'Al ' 0.0560 0.0520 6.4202 3.0387 1.9002 0.7426 1.5936 31.5472 1.9646 85.0886 1.1151 'International_Tables_Vol_IV_Table_2.2B' 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International_Tables_Vol_IV_Table_2.2B' 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C32 H100 Al4 Cl4 O32 P4' _chemical_formula_moiety ' (C24 H76 Al4 O28 P4) 4+, 4 (Cl 1-),4(C2 H6 O1)' _chemical_compound_source ; ? ; _chemical_formula_weight 1370.8 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.9 _cell_measurement_theta_max 12.2 _cell_measurement_temperature 233 K _cell_formula_units_Z 2 _exptl_crystal_description 'block ' _exptl_crystal_colour 'colourless ' _exptl_crystal_size_min 0.25 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_max 0.35 _exptl_crystal_density_diffrn 1.34 _exptl_crystal_density_meas ? _exptl_crystal_F_000 1418.72 _exptl_absorpt_coefficient_mu 0.39 _exptl_absorpt_correction_type 'none' _diffrn_standards_interval_time 3600 s _diffrn_standards_number 2 _diffrn_standards_decay_% 9.75 _diffrn_ambient_temperature 233 K _diffrn_reflns_number 1698 _reflns_number_total 1574 _diffrn_reflns_av_R_equivalents 0.06 _reflns_number_observed 1179 _diffrn_reflns_theta_min 1 _diffrn_reflns_theta_max 25 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _reflns_observed_criterion >3.00\s(I) _refine_diff_density_min -0.43 _refine_diff_density_max 0.51 _refine_ls_number_reflns 1179 _refine_ls_number_parameters ? _refine_ls_R_factor_obs 0.0623 _refine_ls_wR_factor_obs 0.0749 _refine_ls_goodness_of_fit_obs 1.10 _refine_ls_shift/esd_max 0.634155 _refine_ls_structure_factor_coef 'F' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method 2\q/\w loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type AL1 0.5608(2) 0.1456(1) 0.1310(2) 0.0248 1.0000 Uani P1 0.3708(1) 0.0501(1) 0.1497(1) 0.0233 1.0000 Uani O1 0.2994(4) 0.0840(4) 0.0787(5) 0.0347 1.0000 Uani O2 0.4543(3) 0.0972(3) 0.1302(5) 0.0308 1.0000 Uani O3 0.5694(4) 0.1643(4) 0.2548(4) 0.0335 1.0000 Uani O4 0.6256(3) 0.0456(4) 0.1300(4) 0.0293 1.0000 Uani O5 0.5655(4) 0.1414(4) -0.0054(4) 0.0359 1.0000 Uani O6 0.5019(4) 0.2585(4) 0.1148(5) 0.0369 1.0000 Uani O7 0.6689(4) 0.2116(4) 0.1163(4) 0.0339 1.0000 Uani O8 0.6970(6) 0.0403(7) -0.0723(7) 0.0723 1.0000 Uani C1 0.506(1) 0.166(2) -0.0725(9) 0.0746 1.0000 Uani C2 0.523(1) 0.3421(8) 0.157(2) 0.0895 1.0000 Uani C3 0.7463(9) 0.202(1) 0.170(1) 0.0712 1.0000 Uani C4 0.776(2) 0.072(1) -0.096(2) 0.1102 1.0000 Uani C12 0.518(2) 0.137(3) -0.165(1) 0.1489 1.0000 Uani C22 0.549(3) 0.412(2) 0.093(3) 0.2540 1.0000 Uani C32 0.803(2) 0.264(2) 0.183(2) 0.1198 1.0000 Uani C42 0.849(2) 0.025(3) -0.109(3) 0.1789 1.0000 Uani CL1 0.7199(2) 0.3116(2) -0.0607(2) 0.0457 1.0000 Uani H11 0.5035 0.2312 -0.0739 0.0800 1.0000 Uiso H12 0.4467 0.1439 -0.0520 0.0800 1.0000 Uiso H121 0.4708 0.1589 -0.2057 0.1500 1.0000 Uiso H122 0.5757 0.1591 -0.1879 0.1500 1.0000 Uiso H123 0.5188 0.0718 -0.1660 0.1500 1.0000 Uiso H21 0.5724 0.3329 0.2018 0.0900 1.0000 Uiso H22 0.4708 0.3625 0.1929 0.0900 1.0000 Uiso H221 0.5612 0.4654 0.1272 0.2600 1.0000 Uiso H222 0.6007 0.3920 0.0569 0.2600 1.0000 Uiso H223 0.4990 0.4216 0.0480 0.2600 1.0000 Uiso H31 0.7790 0.1533 0.1410 0.0800 1.0000 Uiso H32 0.7263 0.1847 0.2334 0.0800 1.0000 Uiso H321 0.8509 0.2413 0.2230 0.1200 1.0000 Uiso H322 0.8267 0.2825 0.1218 0.1200 1.0000 Uiso H323 0.7739 0.3140 0.2143 0.1200 1.0000 Uiso H41 0.7905 0.1159 -0.0483 0.1100 1.0000 Uiso H42 0.7666 0.1014 -0.1576 0.1100 1.0000 Uiso H421 0.8977 0.0653 -0.1262 0.1800 1.0000 Uiso H422 0.8642 -0.0044 -0.0486 0.1800 1.0000 Uiso H423 0.8402 -0.0189 -0.1579 0.1800 1.0000 Uiso 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 AL1 0.024(1) 0.025(1) 0.027(1) 0.0049(9) 0.002(1) -0.0004(9) P1 0.024(1) 0.025(1) 0.022(1) 0.0002(8) -0.0016(8) 0.0033(7) O1 0.031(3) 0.045(4) 0.038(4) 0.006(3) -0.015(3) -0.000(2) O2 0.027(3) 0.026(3) 0.045(4) 0.009(3) 0.002(3) -0.003(2) O3 0.040(3) 0.041(3) 0.025(3) 0.007(3) 0.006(3) -0.003(3) O4 0.027(3) 0.031(3) 0.039(3) 0.007(3) 0.014(3) 0.001(2) O5 0.038(4) 0.047(4) 0.027(3) 0.007(3) 0.004(3) 0.005(3) O6 0.041(3) 0.031(3) 0.041(4) 0.005(3) -0.004(3) 0.001(2) O7 0.032(3) 0.038(3) 0.034(4) 0.008(3) -0.000(2) -0.003(2) O8 0.079(6) 0.095(7) 0.066(5) 0.025(5) 0.022(5) 0.028(5) C1 0.11(1) 0.19(2) 0.030(6) -0.01(1) -0.018(8) 0.07(1) C2 0.066(8) 0.036(7) 0.31(4) 0.01(1) -0.01(2) 0.005(6) C3 0.054(8) 0.15(2) 0.07(1) 0.04(1) -0.026(7) -0.042(9) C4 0.15(2) 0.09(1) 0.17(2) 0.06(1) 0.08(2) 0.03(1) C12 0.19(3) 0.37(5) 0.09(2) 0.00(2) -0.08(2) 0.08(3) C22 0.43(8) 0.24(5) 0.22(5) -0.04(4) -0.00(5) 0.17(5) C32 0.13(2) 0.18(2) 0.11(2) 0.02(1) -0.04(1) -0.06(2) C42 0.08(2) 0.26(4) 0.29(5) 0.05(4) 0.01(2) -0.01(2) CL1 0.048(1) 0.049(1) 0.052(2) 0.014(1) 0.008(1) -0.016(1) _refine_ls_extinction_coef 66 _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag AL1 . O2 . 1.799(5) yes AL1 . O3 . 1.812(7) yes AL1 . O4 . 1.833(6) yes AL1 . O5 . 1.969(6) yes AL1 . O6 . 1.973(6) yes AL1 . O7 . 1.959(6) yes P1 . O1 . 1.589(6) yes P1 . O2 . 1.500(6) yes P1 . O3 8_545 1.507(6) yes P1 . O4 5_655 1.499(6) yes O5 . C1 . 1.39(1) yes O6 . C2 . 1.46(1) yes O7 . C3 . 1.43(1) yes O8 . C4 . 1.36(2) yes C1 . C12 . 1.42(2) yes C1 . H11 . 1.00(2) no C1 . H12 . 1.01(2) no C2 . C22 . 1.47(2) yes C2 . H21 . 1.00(2) no C2 . H22 . 1.01(2) no C3 . C32 . 1.30(2) yes C3 . H31 . 0.99(2) no C3 . H32 . 1.00(2) no C4 . C42 . 1.35(3) yes C4 . H41 . 0.99(3) no C4 . H42 . 1.01(2) no C12 . H121 . 0.99(2) no C12 . H122 . 1.00(4) no C12 . H123 . 1.01(4) no C22 . H221 . 0.98(5) no C22 . H222 . 1.00(4) no C22 . H223 . 1.01(5) no C32 . H321 . 1.00(2) no C32 . H322 . 1.00(3) no C32 . H323 . 1.00(3) no C42 . H421 . 1.00(3) no C42 . H422 . 1.01(4) no C42 . H423 . 0.98(5) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O2 . AL1 . O3 . 98.0(3) no O2 . AL1 . O4 . 98.5(2) no O3 . AL1 . O4 . 95.8(3) no O2 . AL1 . O5 . 90.8(3) no O3 . AL1 . O5 . 170.3(3) no O4 . AL1 . O5 . 86.8(3) no O2 . AL1 . O6 . 86.9(3) no O3 . AL1 . O6 . 90.6(3) no O4 . AL1 . O6 . 170.9(3) no O5 . AL1 . O6 . 85.8(3) no O2 . AL1 . O7 . 170.4(3) no O3 . AL1 . O7 . 87.8(3) no O4 . AL1 . O7 . 88.4(3) no O5 . AL1 . O7 . 83.0(3) no O6 . AL1 . O7 . 85.4(3) no O1 . P1 . O2 . 108.1(3) no O1 . P1 . O3 8_545 106.0(4) no O2 . P1 . O3 8_545 112.5(4) no O1 . P1 . O4 5_655 103.1(3) no O2 . P1 . O4 5_655 114.0(3) no O3 8_545 P1 . O4 5_655 112.4(4) no AL1 . O2 . P1 . 167.8(5) no AL1 . O3 . P1 4_555 145.8(4) no AL1 . O4 . P1 5_655 147.4(4) no AL1 . O5 . C1 . 131.4(7) no AL1 . O6 . C2 . 128.4(8) no AL1 . O7 . C3 . 126.4(7) no O5 . C1 . C12 . 118.5(15) no O5 . C1 . H11 . 108.1(16) no C12 . C1 . H11 . 107.2(24) no O5 . C1 . H12 . 107.3(15) no C12 . C1 . H12 . 107.0(25) no H11 . C1 . H12 . 108.4(14) no O6 . C2 . C22 . 115.7(30) no O6 . C2 . H21 . 108.2(11) no C22 . C2 . H21 . 107.8(25) no O6 . C2 . H22 . 108.0(12) no C22 . C2 . H22 . 108.1(20) no H21 . C2 . H22 . 108.9(28) no O7 . C3 . C32 . 123.7(18) no O7 . C3 . H31 . 106.2(13) no C32 . C3 . H31 . 105.9(19) no O7 . C3 . H32 . 105.4(11) no C32 . C3 . H32 . 105.0(18) no H31 . C3 . H32 . 110.3(17) no O8 . C4 . C42 . 126.0(24) no O8 . C4 . H41 . 105.5(18) no C42 . C4 . H41 . 106.5(32) no O8 . C4 . H42 . 104.3(24) no C42 . C4 . H42 . 104.0(26) no H41 . C4 . H42 . 110.1(18) no C1 . C12 . H121 . 110.3(22) no C1 . C12 . H122 . 109.0(29) no H121 . C12 . H122 . 110.3(33) no C1 . C12 . H123 . 108.8(29) no H121 . C12 . H123 . 109.4(33) no H122 . C12 . H123 . 108.9(25) no C2 . C22 . H221 . 110.2(32) no C2 . C22 . H222 . 108.9(29) no H221 . C22 . H222 . 110.9(50) no C2 . C22 . H223 . 108.3(41) no H221 . C22 . H223 . 109.8(33) no H222 . C22 . H223 . 108.6(41) no C3 . C32 . H321 . 109.1(24) no C3 . C32 . H322 . 109.4(21) no H321 . C32 . H322 . 109.4(24) no C3 . C32 . H323 . 110.0(24) no H321 . C32 . H323 . 109.4(22) no H322 . C32 . H323 . 109.5(26) no C4 . C42 . H421 . 108.5(35) no C4 . C42 . H422 . 107.9(36) no H421 . C42 . H422 . 108.6(33) no C4 . C42 . H423 . 110.6(31) no H421 . C42 . H423 . 110.9(40) no H422 . C42 . H423 . 110.1(37) no #===End #========================================================================== data_2 _database_code_CSD 165095 # Compound 2 #========================================================================== _chemical_melting_point ? _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device 'Enraf-nonius CAD4 ' _refine_ls_matrix_type 'full' _refine_ls_weighting_scheme ; Chebychev polynomial (Carruthers & Watkin, 1979) ; _atom_sites_solution_primary 'Direct_Methods' _atom_sites_solution_hydrogens 'Geometric' _refine_ls_hydrogen_treatment ; H atoms placed geometrically after each cycle ; #**************************************************************************** _chemical_name_systematic ; # IUPAC name, in full ? ; _cell_length_a 15.425(4) _cell_angle_alpha 90 _cell_length_b 15.425(6) _cell_angle_beta 90 _cell_length_c 14.712(4) _cell_angle_gamma 90 _cell_volume 3500(2) _symmetry_cell_setting 'Tetragonal' _symmetry_space_group_name_H-M 'I -4 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' 'x+1/2,y+1/2,z+1/2' 'y,-x,-z' 'y+1/2,-x+1/2,-z+1/2' '-x,-y,z' '-x+1/2,-y+1/2,z+1/2' '-y,x,-z' '-y+1/2,x+1/2,-z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' 'Br ' -0.3740 2.4560 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 'International_Tables_Vol_IV_Table_2.2B' 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International_Tables_Vol_IV_Table_2.2B' 'Al ' 0.0560 0.0520 6.4202 3.0387 1.9002 0.7426 1.5936 31.5472 1.9646 85.0886 1.1151 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C32 H100 Al4 Br4 O32 P4 ' _chemical_formula_moiety ' (C24 H76 Al4 O28 P4) 4+, 4 (Br 1-),4(C2 H6 O1) ' _chemical_compound_source ; ? ; _chemical_formula_weight 1548.4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14 _cell_measurement_theta_max 14.2 _cell_measurement_temperature 163 _cell_formula_units_Z 2 _exptl_crystal_description 'block' _exptl_crystal_colour 'colourless ' _exptl_crystal_size_min 0.2 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_max 0.4 _exptl_crystal_density_diffrn 1.45 _exptl_crystal_density_meas ? _exptl_crystal_F_000 1558.61 _exptl_absorpt_coefficient_mu 2.49 _exptl_absorpt_correction_type 'none' _diffrn_standards_interval_time 3600 _diffrn_standards_number 2 _diffrn_standards_decay_% 12.13 _diffrn_ambient_temperature 163 _diffrn_reflns_number 1743 _reflns_number_total 1616 _diffrn_reflns_av_R_equivalents 0.06 _reflns_number_observed 1347 _diffrn_reflns_theta_min 1 _diffrn_reflns_theta_max 25 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _reflns_observed_criterion >3.00\s(I) _refine_diff_density_min -0.71 _refine_diff_density_max 0.69 _refine_ls_number_reflns 1347 _refine_ls_number_parameters 173 _refine_ls_R_factor_obs 0.0589 _refine_ls_wR_factor_obs 0.0726 _refine_ls_goodness_of_fit_obs 1.0369 _refine_ls_shift/esd_max 0.343220 _refine_ls_structure_factor_coef 'F' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method 2\q/\w loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type AL1 0.1452(2) 0.9393(2) 0.3830(2) 0.0161 1.0000 Uani P1 -0.0515(2) 0.8706(2) 0.4033(2) 0.0146 1.0000 Uani O1 -0.0818(5) 0.8008(5) 0.3313(6) 0.0251 1.0000 Uani O2 0.0443(4) 0.8779(4) 0.3848(5) 0.0196 1.0000 Uani O4 0.1666(5) 0.9292(5) 0.5042(5) 0.0217 1.0000 Uani O3 0.0995(5) 1.0470(5) 0.3848(5) 0.0209 1.0000 Uani O5 0.1365(5) 0.9377(5) 0.2506(5) 0.0209 1.0000 Uani O6 0.2599(5) 0.9933(5) 0.3649(6) 0.0232 1.0000 Uani O7 0.2082(5) 0.8321(5) 0.3658(5) 0.0130 1.0000 Uani O8 0.0392(8) 0.8105(7) 0.1853(7) 0.0303 1.0000 Uani C1 0.152(2) 1.003(1) 0.187(1) 0.0456 1.0000 Uani C2 0.341(1) 0.970(1) 0.409(3) 0.0586 1.0000 Uani C3 0.192(1) 0.7504(8) 0.412(1) 0.0349 1.0000 Uani C4 0.062(1) 0.734(2) 0.143(2) 0.0685 1.0000 Uani C12 0.140(2) 0.986(1) 0.095(1) 0.0682 1.0000 Uani C22 0.410(3) 0.951(3) 0.354(2) 0.1445 1.0000 Uani C32 0.270(2) 0.699(1) 0.423(1) 0.0687 1.0000 Uani C42 0.041(4) 0.653(2) 0.173(5) 0.1796 1.0000 Uani BR1 0.30524(8) 0.78832(7) 0.17677(8) 0.0280 1.0000 Uani H11 0.1138 1.0526 0.2024 0.0500 1.0000 Uiso H12 0.2144 1.0204 0.1940 0.0500 1.0000 Uiso H121 0.1545 1.0398 0.0596 0.0700 1.0000 Uiso H122 0.0784 0.9701 0.0844 0.0700 1.0000 Uiso H123 0.1789 0.9379 0.0759 0.0700 1.0000 Uiso H21 0.3585 1.0204 0.4481 0.0600 1.0000 Uiso H22 0.3300 0.9185 0.4479 0.0600 1.0000 Uiso H221 0.4613 0.9367 0.3923 0.1400 1.0000 Uiso H222 0.4234 1.0025 0.3150 0.1400 1.0000 Uiso H223 0.3948 0.9006 0.3147 0.1400 1.0000 Uiso H31 0.1677 0.7631 0.4739 0.0400 1.0000 Uiso H32 0.1490 0.7162 0.3764 0.0400 1.0000 Uiso H321 0.2560 0.6439 0.4551 0.0700 1.0000 Uiso H322 0.3137 0.7326 0.4592 0.0700 1.0000 Uiso H323 0.2949 0.6857 0.3616 0.0700 1.0000 Uiso H41 0.1268 0.7349 0.1400 0.0700 1.0000 Uiso H42 0.0375 0.7382 0.0804 0.0700 1.0000 Uiso H421 0.0650 0.6083 0.1306 0.1900 1.0000 Uiso H422 0.0655 0.6434 0.2353 0.1900 1.0000 Uiso H423 -0.0238 0.6467 0.1757 0.1900 1.0000 Uiso 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 AL1 0.013(1) 0.018(1) 0.018(1) -0.000(1) 0.003(1) 0.001(1) P1 0.013(1) 0.013(1) 0.018(1) -0.001(1) -0.002(1) -0.0015(9) O1 0.026(4) 0.030(4) 0.022(4) -0.006(4) 0.000(3) -0.004(3) O2 0.017(4) 0.018(3) 0.029(4) 0.004(3) 0.007(3) 0.003(3) O4 0.025(4) 0.026(4) 0.018(4) -0.007(3) 0.003(3) 0.002(3) O3 0.026(4) 0.021(4) 0.018(4) -0.002(3) 0.002(3) 0.004(3) O5 0.024(4) 0.025(4) 0.016(3) 0.003(3) -0.003(3) 0.001(3) O6 0.014(4) 0.023(4) 0.045(5) 0.002(4) 0.006(4) -0.004(3) O7 0.031(4) 0.018(3) 0.008(3) 0.004(3) 0.011(3) 0.007(3) O8 0.083(8) 0.068(7) 0.028(5) -0.036(5) 0.030(5) -0.036(6) C1 0.18(2) 0.05(1) 0.032(9) 0.019(8) 0.01(1) -0.06(1) C2 0.021(7) 0.042(9) 0.25(4) 0.01(2) 0.00(1) -0.008(6) C3 0.060(8) 0.023(6) 0.038(7) 0.011(5) 0.014(7) 0.005(6) C4 0.07(1) 0.12(2) 0.08(2) -0.06(1) 0.03(1) -0.04(1) C12 0.11(2) 0.07(1) 0.05(1) 0.012(9) 0.00(1) -0.01(1) C22 0.39(8) 0.27(6) 0.04(2) -0.05(2) -0.00(3) -0.12(5) C32 0.11(2) 0.08(1) 0.05(1) 0.01(1) 0.00(1) 0.05(1) C42 0.25(5) 0.07(2) 0.40(9) -0.01(4) 0.14(6) -0.01(3) BR1 0.0355(7) 0.0311(7) 0.0302(6) -0.0045(5) 0.0104(5) 0.0141(5) _refine_ls_extinction_coef 34.4 _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag AL1 . O2 . 1.822(7) yes AL1 . O4 . 1.820(8) yes AL1 . O3 . 1.804(8) yes AL1 . O5 . 1.953(7) yes AL1 . O6 . 1.974(8) yes AL1 . O7 . 1.935(7) yes P1 . O1 . 1.581(8) yes P1 . O2 . 1.507(7) yes P1 . O4 3_466 1.507(8) yes P1 . O3 5_575 1.497(7) yes O5 . C1 . 1.40(2) yes O6 . C2 . 1.46(2) yes O7 . C3 . 1.46(1) yes O8 . C4 . 1.38(2) yes C1 . C12 . 1.38(2) yes C1 . H11 . 1.00(3) no C1 . H12 . 1.00(2) no C2 . C22 . 1.37(3) yes C2 . H21 . 1.00(3) no C2 . H22 . 1.00(3) no C3 . C32 . 1.45(2) yes C3 . H31 . 1.00(1) no C3 . H32 . 1.00(2) no C4 . C42 . 1.37(3) yes C4 . H41 . 1.00(2) no C4 . H42 . 1.00(3) no C12 . H121 . 1.00(2) no C12 . H122 . 1.00(2) no C12 . H123 . 1.00(2) no C22 . H221 . 1.00(5) no C22 . H222 . 1.00(5) no C22 . H223 . 1.00(4) no C32 . H321 . 1.00(2) no C32 . H322 . 1.00(3) no C32 . H323 . 1.00(2) no C42 . H421 . 1.00(5) no C42 . H422 . 1.01(8) no C42 . H423 . 1.00(5) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O2 . AL1 . O4 . 95.5(4) no O2 . AL1 . O3 . 98.3(3) no O4 . AL1 . O3 . 97.7(4) no O2 . AL1 . O5 . 87.1(4) no O4 . AL1 . O5 . 171.4(4) no O3 . AL1 . O5 . 89.9(3) no O2 . AL1 . O6 . 170.8(4) no O4 . AL1 . O6 . 90.3(4) no O3 . AL1 . O6 . 87.9(3) no O5 . AL1 . O6 . 86.1(4) no O2 . AL1 . O7 . 89.3(3) no O4 . AL1 . O7 . 88.0(3) no O3 . AL1 . O7 . 170.0(3) no O5 . AL1 . O7 . 83.9(3) no O6 . AL1 . O7 . 83.8(3) no O1 . P1 . O2 . 102.8(4) no O1 . P1 . O4 3_466 106.7(4) no O2 . P1 . O4 3_466 112.6(4) no O1 . P1 . O3 5_575 108.1(4) no O2 . P1 . O3 5_575 112.9(4) no O4 3_466 P1 . O3 5_575 112.9(4) no AL1 . O2 . P1 . 151.6(5) no AL1 . O4 . P1 7_666 143.1(5) no AL1 . O3 . P1 5_575 168.0(5) no AL1 . O5 . C1 . 130.6(9) no AL1 . O6 . C2 . 127.5(11) no AL1 . O7 . C3 . 126.3(7) no O5 . C1 . C12 . 119.9(15) no O5 . C1 . H11 . 106.7(16) no C12 . C1 . H11 . 106.8(22) no O5 . C1 . H12 . 106.8(19) no C12 . C1 . H12 . 106.7(19) no H11 . C1 . H12 . 109.7(15) no O6 . C2 . C22 . 116.7(38) no O6 . C2 . H21 . 107.5(14) no C22 . C2 . H21 . 107.5(21) no O6 . C2 . H22 . 107.6(12) no C22 . C2 . H22 . 107.4(28) no H21 . C2 . H22 . 110.0(37) no O7 . C3 . C32 . 112.4(14) no O7 . C3 . H31 . 108.7(10) no C32 . C3 . H31 . 108.8(15) no O7 . C3 . H32 . 108.7(12) no C32 . C3 . H32 . 108.7(15) no H31 . C3 . H32 . 109.5(14) no O8 . C4 . C42 . 125.3(28) no O8 . C4 . H41 . 105.5(16) no C42 . C4 . H41 . 105.3(34) no O8 . C4 . H42 . 105.5(23) no C42 . C4 . H42 . 105.1(37) no H41 . C4 . H42 . 109.7(18) no C1 . C12 . H121 . 109.2(18) no C1 . C12 . H122 . 109.5(20) no H121 . C12 . H122 . 109.4(20) no C1 . C12 . H123 . 109.6(21) no H121 . C12 . H123 . 109.5(20) no H122 . C12 . H123 . 109.7(19) no C2 . C22 . H221 . 109.0(26) no C2 . C22 . H222 . 109.5(49) no H221 . C22 . H222 . 109.3(41) no C2 . C22 . H223 . 109.7(40) no H221 . C22 . H223 . 109.4(54) no H222 . C22 . H223 . 109.8(28) no C3 . C32 . H321 . 109.6(21) no C3 . C32 . H322 . 109.4(18) no H321 . C32 . H322 . 109.4(18) no C3 . C32 . H323 . 109.5(16) no H321 . C32 . H323 . 109.6(20) no H322 . C32 . H323 . 109.2(25) no C4 . C42 . H421 . 109.7(45) no C4 . C42 . H422 . 109.4(47) no H421 . C42 . H422 . 109.1(48) no C4 . C42 . H423 . 109.8(41) no H421 . C42 . H423 . 109.7(57) no #===End