Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address 'Mervi Kontturi' ; Department of Chemistry University of Joensuu P.O. Box 111 FIN-80101, Joensuu Finland ; 'Sirpa Peraniemi' ; Department of Chemistry University of Joensuu P.O. Box 111 FIN-80101, Joensuu Finland ; 'Tuula T. Pakkanen' ; Department of Chemistry University of Joensuu P.O. Box 111 FIN-80101, Joensuu Finland ; 'Eija Vuokila-Laine' ; Department of Chemistry University of Joensuu P.O. Box 111 FIN-80101, Joensuu Finland ; 'Jouko J. Vepsalainen' ; Department of Chemistry University of Kuopio P.O. Box 1627 FIN-70211, Kuopio Finland ; 'Markku Ahlgren' ; Department of Chemistry University of Joensuu P.O. Box 111 FIN-80101, Joensuu Finland ; _publ_contact_author_name 'Dr Mervi Konttuir' _publ_contact_author_address ; Department of Chemistry University of Joensuu P.O Box 111 Joensuu FIN-80101 FINLAND ; _publ_contact_author_phone '358 13 2513377' _publ_contact_author_fax '358 13 2513390' _publ_contact_author_email 'Mervi.Kontturi@joensuu.fi' _publ_requested_journal 'Dalton Transactions' _publ_requested_coeditor_name ? _publ_contact_letter ? _publ_section_title ; A Structural Study of Bisphosphonate Metal Complexes. Alkaline Earth Metal Complexes of (dichloromethylene)bisphosphonic acid P,P'-diethyl ester. ; _publ_section_abstract ; A dipiperidinium salt and four alkaline earth metal complexes of the (dichloromethylene)bisphosphosphonic acid P,P'-diethyl ester: (C5H10NH2)2Cl2C(PO3Et)2 (1), [MgCl2C(PO3Et)2(H2O)3]n (2), [(H2O)3Ca{Cl2C(PO3Et)2}2Ca(H2O)3] (3), [(H2O)3Sr{Cl2C(PO3Et)2}2Sr(H2O)3] (4) and [(H2O)2Ba{Cl2C(PO3Et)2}2Ba(H2O)2]n (5) were prepared and characterised. The crystal structures were determined with the single crystal X-ray diffraction technique. The asymmetric unit of compound 1 contains two piperidinium cations and one (dichloromethylene)bisphosphosphonic acid P,P'-diethyl ester anion, which are bound to each other by hydrogen bonding via amine-N+H2. Compound 2 is polymeric, having two independent magnesium atoms with octahedral geometry. Calcium and strontium complexes 3 and 4 are isomorphous and dimeric with seven co-ordinated metal atoms connected by two Cl2C(PO3Et)22- ligands. In the asymmetric unit of complex 5, two adjacent barium atoms are joined by two Cl2C(PO3Et)22- ligands. The dimeric units are bridged through the oxygen atoms of Cl2C(PO3Et)22- and aqua ligands, forming polymeric chains. Compounds were characterised by infrared spectroscopy, thermogravimetry and 31P CP/MAS NMR spectroscopy. ; _publ_section_comment ; ? ; _publ_section_references ; ? ; data_Structure_1 _database_code_CSD 163497 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '(C5H10NH2)2Cl2C[PO3(C2H5)]2' _chemical_formula_sum 'C15 H34 Cl2 N2 O6 P2' _chemical_formula_weight 471.28 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'triclinic' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4317(2) _cell_length_b 11.2372(3) _cell_length_c 11.9292(4) _cell_angle_alpha 105.774(1) _cell_angle_beta 98.221(2) _cell_angle_gamma 106.067(2) _cell_volume 1136.17(5) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 3.12 _cell_measurement_theta_max 29.10 _exptl_crystal_description 'irregular' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 1.355(14) _exptl_crystal_density_diffrn 1.378 _exptl_crystal_density_method 'flotation' _exptl_crystal_F_000 500 _exptl_absorpt_coefficient_mu 0.458 _exptl_absorpt_correction_type 'semiempirical' _exptl_absorpt_correction_T_min 0.8379 _exptl_absorpt_correction_T_max 0.9556 _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19610 _diffrn_reflns_av_R_equivalents 0.0150 _diffrn_reflns_av_sigmaI/netI 0.0290 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 29.10 _reflns_number_total 5368 _reflns_number_gt 4663 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'collect (Nonius, 1999)' _computing_cell_refinement 'Denzo, Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo, Scalepack' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+0.7000P] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0010(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5368 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0396 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0752 _refine_ls_wR_factor_gt 0.0718 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.01141(4) 0.42884(4) 0.10648(3) 0.02347(9) Uani 1 d . . . Cl2 Cl 0.22410(5) 0.28562(4) 0.09079(3) 0.02498(10) Uani 1 d . . . P1 P 0.06513(4) 0.30361(4) 0.29109(3) 0.01642(9) Uani 1 d . . . P2 P 0.31308(4) 0.54780(4) 0.27850(3) 0.01655(9) Uani 1 d . . . O11 O 0.02972(14) 0.40293(11) 0.38351(9) 0.0244(2) Uani 1 d . . . O12 O 0.16202(12) 0.22895(10) 0.32607(9) 0.0209(2) Uani 1 d . . . O13 O -0.09456(12) 0.20562(10) 0.20646(10) 0.0226(2) Uani 1 d . . . O21 O 0.24626(12) 0.65028(10) 0.32901(9) 0.0207(2) Uani 1 d . . . O22 O 0.42005(13) 0.51458(10) 0.35998(9) 0.0226(2) Uani 1 d . . . O23 O 0.39762(12) 0.58226(11) 0.17896(10) 0.0221(2) Uani 1 d . . . N1 N -0.00918(15) 0.65725(12) 0.40957(11) 0.0195(3) Uani 1 d . . . H1A H 0.0582 0.6335 0.3669 0.023 Uiso 1 calc R . . H1B H -0.0037 0.6268 0.4737 0.023 Uiso 1 calc R . . N2 N 0.46168(14) 0.28426(12) 0.42607(11) 0.0188(2) Uani 1 d . . . H2A H 0.4873 0.3543 0.4954 0.023 Uiso 1 calc R . . H2B H 0.3727 0.2808 0.3799 0.023 Uiso 1 calc R . . C1 C 0.15414(16) 0.39170(14) 0.19374(12) 0.0163(3) Uani 1 d . . . C2 C -0.1163(2) 0.07824(16) 0.12302(17) 0.0317(4) Uani 1 d . . . H2C H -0.1809 0.0090 0.1480 0.038 Uiso 1 calc R . . H2D H -0.0170 0.0647 0.1225 0.038 Uiso 1 calc R . . C3 C -0.1907(3) 0.0694(2) -0.00020(19) 0.0486(6) Uani 1 d . . . H3A H -0.2877 0.0852 0.0012 0.073 Uiso 1 calc R . . H3B H -0.2088 -0.0181 -0.0562 0.073 Uiso 1 calc R . . H3C H -0.1243 0.1355 -0.0260 0.073 Uiso 1 calc R . . C4 C 0.3431(2) 0.6451(2) 0.10002(19) 0.0403(5) Uani 1 d . . . H4A H 0.3136 0.7181 0.1463 0.048 Uiso 1 calc R . . H4B H 0.2524 0.5814 0.0384 0.048 Uiso 1 calc R . . C5 C 0.4634(2) 0.6958(2) 0.04160(19) 0.0406(5) Uani 1 d . . . H5A H 0.5515 0.7614 0.1027 0.061 Uiso 1 calc R . . H5B H 0.4250 0.7363 -0.0138 0.061 Uiso 1 calc R . . H5C H 0.4936 0.6235 -0.0029 0.061 Uiso 1 calc R . . C11 C -0.16552(19) 0.59407(16) 0.33156(16) 0.0260(3) Uani 1 d . . . H11A H -0.2395 0.6075 0.3806 0.031 Uiso 1 calc R . . H11B H -0.1858 0.4986 0.2978 0.031 Uiso 1 calc R . . C12 C -0.1879(2) 0.64840(19) 0.23038(16) 0.0346(4) Uani 1 d . . . H12A H -0.2959 0.6106 0.1864 0.042 Uiso 1 calc R . . H12B H -0.1263 0.6222 0.1738 0.042 Uiso 1 calc R . . C13 C -0.1426(2) 0.79684(19) 0.27593(17) 0.0361(4) Uani 1 d . . . H13A H -0.1509 0.8300 0.2072 0.043 Uiso 1 calc R . . H13B H -0.2120 0.8233 0.3248 0.043 Uiso 1 calc R . . C14 C 0.0192(2) 0.85562(17) 0.35114(17) 0.0320(4) Uani 1 d . . . H14A H 0.0470 0.9522 0.3827 0.038 Uiso 1 calc R . . H14B H 0.0891 0.8344 0.3004 0.038 Uiso 1 calc R . . C15 C 0.0366(2) 0.80283(15) 0.45498(15) 0.0263(3) Uani 1 d . . . H15A H 0.1435 0.8402 0.5013 0.032 Uiso 1 calc R . . H15B H -0.0276 0.8296 0.5091 0.032 Uiso 1 calc R . . C21 C 0.43599(19) 0.16151(16) 0.45705(15) 0.0258(3) Uani 1 d . . . H21A H 0.3500 0.1491 0.4965 0.031 Uiso 1 calc R . . H21B H 0.5276 0.1686 0.5141 0.031 Uiso 1 calc R . . C22 C 0.4014(2) 0.04414(16) 0.34527(16) 0.0310(4) Uani 1 d . . . H22A H 0.3045 0.0321 0.2917 0.037 Uiso 1 calc R . . H22B H 0.3898 -0.0358 0.3681 0.037 Uiso 1 calc R . . C23 C 0.5278(2) 0.06288(18) 0.27881(17) 0.0355(4) Uani 1 d . . . H23A H 0.6228 0.0663 0.3293 0.043 Uiso 1 calc R . . H23B H 0.5004 -0.0123 0.2040 0.043 Uiso 1 calc R . . C24 C 0.5528(2) 0.18912(19) 0.24890(15) 0.0317(4) Uani 1 d . . . H24A H 0.6398 0.2033 0.2107 0.038 Uiso 1 calc R . . H24B H 0.4616 0.1811 0.1909 0.038 Uiso 1 calc R . . C25 C 0.58388(18) 0.30574(16) 0.35959(15) 0.0243(3) Uani 1 d . . . H25A H 0.6825 0.3212 0.4128 0.029 Uiso 1 calc R . . H25B H 0.5909 0.3847 0.3360 0.029 Uiso 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 Cl1 0.0210(2) 0.0297(2) 0.02084(17) 0.01261(14) -0.00225(13) 0.00957(14) Cl2 0.0281(2) 0.02662(19) 0.02136(18) 0.00370(14) 0.01177(14) 0.01197(15) P1 0.0166(2) 0.02122(18) 0.01557(17) 0.00823(14) 0.00477(13) 0.00985(14) P2 0.0147(2) 0.01985(18) 0.01599(17) 0.00616(14) 0.00184(13) 0.00764(13) O11 0.0370(7) 0.0285(6) 0.0189(5) 0.0123(4) 0.0140(4) 0.0195(5) O12 0.0187(6) 0.0238(5) 0.0237(5) 0.0113(4) 0.0025(4) 0.0103(4) O13 0.0150(6) 0.0241(6) 0.0302(6) 0.0096(5) 0.0044(4) 0.0084(4) O21 0.0204(6) 0.0211(5) 0.0215(5) 0.0055(4) 0.0047(4) 0.0098(4) O22 0.0220(6) 0.0236(5) 0.0201(5) 0.0058(4) -0.0030(4) 0.0096(4) O23 0.0183(6) 0.0280(6) 0.0264(5) 0.0142(5) 0.0078(4) 0.0111(4) N1 0.0238(7) 0.0220(6) 0.0202(6) 0.0114(5) 0.0096(5) 0.0125(5) N2 0.0150(6) 0.0208(6) 0.0206(6) 0.0070(5) 0.0018(4) 0.0069(5) C1 0.0164(7) 0.0220(7) 0.0126(6) 0.0053(5) 0.0024(5) 0.0103(5) C2 0.0227(9) 0.0188(8) 0.0468(10) 0.0064(7) -0.0029(7) 0.0063(6) C3 0.0485(14) 0.0361(11) 0.0437(12) -0.0069(9) -0.0151(9) 0.0197(9) C4 0.0324(11) 0.0671(14) 0.0495(11) 0.0441(11) 0.0209(8) 0.0290(9) C5 0.0436(12) 0.0552(12) 0.0465(11) 0.0348(10) 0.0249(9) 0.0272(10) C11 0.0177(8) 0.0236(8) 0.0389(9) 0.0120(7) 0.0098(6) 0.0071(6) C12 0.0316(11) 0.0398(10) 0.0325(9) 0.0101(8) -0.0029(7) 0.0187(8) C13 0.0456(12) 0.0410(10) 0.0390(10) 0.0244(8) 0.0132(8) 0.0279(9) C14 0.0402(11) 0.0226(8) 0.0448(10) 0.0191(7) 0.0228(8) 0.0142(7) C15 0.0304(9) 0.0212(8) 0.0263(8) 0.0041(6) 0.0065(6) 0.0105(6) C21 0.0239(9) 0.0275(8) 0.0284(8) 0.0155(7) 0.0027(6) 0.0078(6) C22 0.0268(9) 0.0200(8) 0.0395(10) 0.0089(7) -0.0044(7) 0.0045(6) C23 0.0291(10) 0.0322(9) 0.0359(10) -0.0046(7) -0.0033(7) 0.0168(7) C24 0.0206(9) 0.0502(11) 0.0266(8) 0.0107(8) 0.0067(6) 0.0165(7) C25 0.0126(8) 0.0283(8) 0.0348(9) 0.0144(7) 0.0066(6) 0.0066(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 C1 1.7934(14) . ? Cl2 C1 1.7989(14) . ? P1 O11 1.4884(11) . ? P1 O12 1.4897(11) . ? P1 O13 1.5947(11) . ? P1 C1 1.8646(15) . ? P2 O21 1.4898(11) . ? P2 O22 1.4925(11) . ? P2 O23 1.5955(11) . ? P2 C1 1.8690(15) . ? O13 C2 1.444(2) . ? O23 C4 1.440(2) . ? N1 C11 1.488(2) . ? N1 C15 1.4887(19) . ? N1 H1A 0.9200 . ? N1 H1B 0.9200 . ? N2 C21 1.4886(19) . ? N2 C25 1.4923(19) . ? N2 H2A 0.9200 . ? N2 H2B 0.9200 . ? C2 C3 1.500(3) . ? C2 H2C 0.9900 . ? C2 H2D 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.477(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C11 C12 1.508(2) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.519(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.516(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.519(2) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C21 C22 1.518(2) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.522(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.520(3) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.511(2) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? 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 _geom_angle_publ_flag O11 P1 O12 120.96(6) . . ? O11 P1 O13 105.90(7) . . ? O12 P1 O13 110.41(6) . . ? O11 P1 C1 105.81(6) . . ? O12 P1 C1 108.45(6) . . ? O13 P1 C1 103.98(6) . . ? O21 P2 O22 119.92(6) . . ? O21 P2 O23 110.34(6) . . ? O22 P2 O23 106.65(6) . . ? O21 P2 C1 108.22(6) . . ? O22 P2 C1 106.46(6) . . ? O23 P2 C1 104.08(6) . . ? C2 O13 P1 124.25(10) . . ? C4 O23 P2 122.32(11) . . ? C11 N1 C15 112.82(12) . . ? C11 N1 H1A 109.0 . . ? C15 N1 H1A 109.0 . . ? C11 N1 H1B 109.0 . . ? C15 N1 H1B 109.0 . . ? H1A N1 H1B 107.8 . . ? C21 N2 C25 112.75(12) . . ? C21 N2 H2A 109.0 . . ? C25 N2 H2A 109.0 . . ? C21 N2 H2B 109.0 . . ? C25 N2 H2B 109.0 . . ? H2A N2 H2B 107.8 . . ? Cl1 C1 Cl2 107.38(7) . . ? Cl1 C1 P1 108.79(8) . . ? Cl2 C1 P1 109.28(7) . . ? Cl1 C1 P2 108.41(7) . . ? Cl2 C1 P2 108.88(8) . . ? P1 C1 P2 113.90(7) . . ? O13 C2 C3 109.50(14) . . ? O13 C2 H2C 109.8 . . ? C3 C2 H2C 109.8 . . ? O13 C2 H2D 109.8 . . ? C3 C2 H2D 109.8 . . ? H2C C2 H2D 108.2 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O23 C4 C5 109.69(15) . . ? O23 C4 H4A 109.7 . . ? C5 C4 H4A 109.7 . . ? O23 C4 H4B 109.7 . . ? C5 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C11 C12 112.21(13) . . ? N1 C11 H11A 109.2 . . ? C12 C11 H11A 109.2 . . ? N1 C11 H11B 109.2 . . ? C12 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? C11 C12 C13 111.66(15) . . ? C11 C12 H12A 109.3 . . ? C13 C12 H12A 109.3 . . ? C11 C12 H12B 109.3 . . ? C13 C12 H12B 109.3 . . ? H12A C12 H12B 107.9 . . ? C14 C13 C12 109.83(14) . . ? C14 C13 H13A 109.7 . . ? C12 C13 H13A 109.7 . . ? C14 C13 H13B 109.7 . . ? C12 C13 H13B 109.7 . . ? H13A C13 H13B 108.2 . . ? C13 C14 C15 110.88(14) . . ? C13 C14 H14A 109.5 . . ? C15 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? N1 C15 C14 110.30(13) . . ? N1 C15 H15A 109.6 . . ? C14 C15 H15A 109.6 . . ? N1 C15 H15B 109.6 . . ? C14 C15 H15B 109.6 . . ? H15A C15 H15B 108.1 . . ? N2 C21 C22 110.62(13) . . ? N2 C21 H21A 109.5 . . ? C22 C21 H21A 109.5 . . ? N2 C21 H21B 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 108.1 . . ? C21 C22 C23 110.99(14) . . ? C21 C22 H22A 109.4 . . ? C23 C22 H22A 109.4 . . ? C21 C22 H22B 109.4 . . ? C23 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? C24 C23 C22 110.10(14) . . ? C24 C23 H23A 109.6 . . ? C22 C23 H23A 109.6 . . ? C24 C23 H23B 109.6 . . ? C22 C23 H23B 109.6 . . ? H23A C23 H23B 108.2 . . ? C25 C24 C23 111.59(14) . . ? C25 C24 H24A 109.3 . . ? C23 C24 H24A 109.3 . . ? C25 C24 H24B 109.3 . . ? C23 C24 H24B 109.3 . . ? H24A C24 H24B 108.0 . . ? N2 C25 C24 111.31(13) . . ? N2 C25 H25A 109.4 . . ? C24 C25 H25A 109.4 . . ? N2 C25 H25B 109.4 . . ? C24 C25 H25B 109.4 . . ? H25A C25 H25B 108.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O11 P1 O13 C2 -164.66(12) . . . . ? O12 P1 O13 C2 -32.07(14) . . . . ? C1 P1 O13 C2 84.07(13) . . . . ? O21 P2 O23 C4 -34.94(16) . . . . ? O22 P2 O23 C4 -166.71(14) . . . . ? C1 P2 O23 C4 80.96(15) . . . . ? O11 P1 C1 Cl1 -70.56(9) . . . . ? O12 P1 C1 Cl1 158.29(7) . . . . ? O13 P1 C1 Cl1 40.78(8) . . . . ? O11 P1 C1 Cl2 172.49(7) . . . . ? O12 P1 C1 Cl2 41.34(9) . . . . ? O13 P1 C1 Cl2 -76.18(8) . . . . ? O11 P1 C1 P2 50.48(9) . . . . ? O12 P1 C1 P2 -80.67(9) . . . . ? O13 P1 C1 P2 161.82(7) . . . . ? O21 P2 C1 Cl1 43.49(9) . . . . ? O22 P2 C1 Cl1 173.64(7) . . . . ? O23 P2 C1 Cl1 -73.89(8) . . . . ? O21 P2 C1 Cl2 160.01(7) . . . . ? O22 P2 C1 Cl2 -69.83(8) . . . . ? O23 P2 C1 Cl2 42.64(8) . . . . ? O21 P2 C1 P1 -77.76(8) . . . . ? O22 P2 C1 P1 52.40(9) . . . . ? O23 P2 C1 P1 164.86(7) . . . . ? P1 O13 C2 C3 -124.66(15) . . . . ? P2 O23 C4 C5 164.89(14) . . . . ? C15 N1 C11 C12 53.34(17) . . . . ? N1 C11 C12 C13 -52.9(2) . . . . ? C11 C12 C13 C14 54.9(2) . . . . ? C12 C13 C14 C15 -57.37(19) . . . . ? C11 N1 C15 C14 -55.19(17) . . . . ? C13 C14 C15 N1 57.44(18) . . . . ? C25 N2 C21 C22 -55.75(17) . . . . ? N2 C21 C22 C23 56.32(18) . . . . ? C21 C22 C23 C24 -56.14(18) . . . . ? C22 C23 C24 C25 55.16(18) . . . . ? C21 N2 C25 C24 54.82(17) . . . . ? C23 C24 C25 N2 -54.28(18) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A O21 0.92 1.86 2.7312(17) 156.1 . N1 H1B O11 0.92 2.58 2.9204(16) 102.6 . N1 H1B O11 0.92 1.86 2.7494(16) 162.2 2_566 N2 H2B O12 0.92 1.87 2.7308(17) 155.1 . N2 H2B O22 0.92 2.62 3.0096(16) 106.0 . N2 H2A O22 0.92 1.84 2.7425(16) 166.6 2_666 _diffrn_measured_fraction_theta_max 0.880 _diffrn_reflns_theta_full 29.10 _diffrn_measured_fraction_theta_full 0.880 _refine_diff_density_max 0.413 _refine_diff_density_min -0.352 _refine_diff_density_rms 0.051 #===END data_Structure_2 _database_code_CSD 163498 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[MgCl2C(PO3Et)2(H2O)3]n' _chemical_formula_sum 'C5 H16 Cl2 Mg O9 P2' _chemical_formula_weight 377.33 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mg' 'Mg' 0.0486 0.0363 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'triclinic' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.3862(7) _cell_length_b 8.3578(7) _cell_length_c 11.8701(11) _cell_angle_alpha 94.151(6) _cell_angle_beta 97.755(5) _cell_angle_gamma 93.418(7) _cell_volume 722.38(11) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.79 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'plate' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 1.704(14) _exptl_crystal_density_diffrn 1.735 _exptl_crystal_density_method 'flotation' _exptl_crystal_F_000 388 _exptl_absorpt_coefficient_mu 0.748 _exptl_absorpt_correction_type 'semiempirical' _exptl_absorpt_correction_T_min 0.8351 _exptl_absorpt_correction_T_max 0.9779 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11038 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3041 _reflns_number_gt 2631 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'collect (Nonius, 1999)' _computing_cell_refinement 'Denzo, Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo, Scalepack' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0200P)^2^+0.8000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom and difmap' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0108(19) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3041 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0477 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.0872 _refine_ls_wR_factor_gt 0.0840 _refine_ls_goodness_of_fit_ref 1.174 _refine_ls_restrained_S_all 1.174 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Cl1 Cl 0.26984(8) 0.20308(7) 0.85353(5) 0.02113(16) Uani 1 1 d . . . Cl2 Cl 0.59171(8) 0.40530(8) 0.82710(5) 0.02192(16) Uani 1 1 d . . . Mg1 Mg 0.5000 0.5000 0.5000 0.0153(2) Uani 1 2 d S . . Mg2 Mg 0.0000 0.0000 0.5000 0.0159(2) Uani 1 2 d S . . P1 P 0.22893(8) 0.47493(7) 0.70577(5) 0.01486(16) Uani 1 1 d . . . P2 P 0.42423(8) 0.18011(7) 0.63137(5) 0.01438(15) Uani 1 1 d . . . O1 O 0.2643(2) 0.4041(2) 0.38570(15) 0.0187(4) Uani 1 1 d . . . O2 O -0.0548(2) 0.2368(2) 0.46584(14) 0.0194(4) Uani 1 1 d . . . O3 O 0.0851(2) -0.0437(2) 0.34121(15) 0.0218(4) Uani 1 1 d . . . O11 O 0.3232(2) 0.5530(2) 0.61815(14) 0.0170(4) Uani 1 1 d . . . O12 O 0.0389(2) 0.3992(2) 0.67271(14) 0.0182(4) Uani 1 1 d . . . O13 O 0.2391(2) 0.6038(2) 0.81065(15) 0.0194(4) Uani 1 1 d . . . O21 O 0.5335(2) 0.28048(19) 0.56264(14) 0.0166(4) Uani 1 1 d . . . O22 O 0.2461(2) 0.0984(2) 0.57656(14) 0.0182(4) Uani 1 1 d . . . O23 O 0.5554(2) 0.0570(2) 0.68852(14) 0.0175(4) Uani 1 1 d . . . C1 C 0.3774(3) 0.3155(3) 0.7546(2) 0.0167(5) Uani 1 1 d . . . C13 C 0.1111(4) 0.6056(3) 0.8930(2) 0.0255(6) Uani 1 1 d . . . H13A H 0.1493 0.5349 0.9540 0.031 Uiso 1 1 calc R . . H13B H -0.0130 0.5663 0.8553 0.031 Uiso 1 1 calc R . . C14 C 0.1101(4) 0.7761(4) 0.9425(3) 0.0347(7) Uani 1 1 d . . . H14A H 0.2331 0.8131 0.9805 0.052 Uiso 1 1 calc R . . H14B H 0.0232 0.7814 0.9979 0.052 Uiso 1 1 calc R . . H14C H 0.0733 0.8450 0.8812 0.052 Uiso 1 1 calc R . . C23 C 0.4896(3) -0.0975(3) 0.7266(2) 0.0203(5) Uani 1 1 d . . . H23A H 0.5051 -0.1867 0.6699 0.024 Uiso 1 1 calc R . . H23B H 0.3581 -0.0963 0.7346 0.024 Uiso 1 1 calc R . . C24 C 0.5996(4) -0.1204(3) 0.8391(2) 0.0293(6) Uani 1 1 d . . . H24A H 0.7300 -0.1169 0.8310 0.044 Uiso 1 1 calc R . . H24B H 0.5621 -0.2248 0.8645 0.044 Uiso 1 1 calc R . . H24C H 0.5785 -0.0345 0.8956 0.044 Uiso 1 1 calc R . . H1A H 0.1912 0.4748 0.3608 0.030 Uiso 1 1 d . . . H1B H 0.1787 0.3303 0.4043 0.030 Uiso 1 1 d . . . H2A H -0.0283 0.2967 0.5297 0.030 Uiso 1 1 d . . . H2B H -0.1624 0.2739 0.4351 0.030 Uiso 1 1 d . . . H3A H 0.1983 -0.0529 0.3404 0.030 Uiso 1 1 d . . . H3B H 0.0250 -0.1326 0.3094 0.030 Uiso 1 1 d . . . 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 Cl1 0.0229(3) 0.0194(3) 0.0231(3) 0.0061(2) 0.0075(2) 0.0028(3) Cl2 0.0166(3) 0.0222(3) 0.0251(3) 0.0008(2) -0.0025(2) 0.0000(2) Mg1 0.0133(5) 0.0130(6) 0.0200(6) 0.0024(4) 0.0032(4) 0.0013(5) Mg2 0.0120(5) 0.0141(6) 0.0217(6) 0.0029(4) 0.0023(4) 0.0010(5) P1 0.0124(3) 0.0131(3) 0.0194(3) 0.0015(2) 0.0029(2) 0.0015(2) P2 0.0109(3) 0.0127(3) 0.0199(3) 0.0029(2) 0.0021(2) 0.0014(2) O1 0.0133(8) 0.0168(9) 0.0257(9) 0.0032(7) 0.0015(6) 0.0002(7) O2 0.0166(8) 0.0162(9) 0.0246(9) 0.0016(7) -0.0006(7) 0.0035(7) O3 0.0134(8) 0.0259(10) 0.0260(9) 0.0008(7) 0.0043(7) -0.0002(7) O11 0.0155(8) 0.0154(9) 0.0216(9) 0.0043(6) 0.0053(7) 0.0042(7) O12 0.0125(8) 0.0172(9) 0.0244(9) 0.0010(6) 0.0015(6) 0.0013(7) O13 0.0174(8) 0.0172(9) 0.0239(9) -0.0018(7) 0.0072(7) -0.0013(7) O21 0.0138(8) 0.0148(9) 0.0222(9) 0.0046(6) 0.0050(6) 0.0014(7) O22 0.0126(8) 0.0175(9) 0.0239(9) 0.0007(7) 0.0011(6) 0.0009(7) O23 0.0130(8) 0.0140(9) 0.0266(9) 0.0070(6) 0.0036(7) 0.0009(7) C1 0.0126(10) 0.0161(12) 0.0215(12) 0.0038(9) 0.0033(9) -0.0013(10) C13 0.0244(13) 0.0285(15) 0.0246(13) -0.0019(11) 0.0107(10) -0.0024(12) C14 0.0347(16) 0.0304(16) 0.0405(17) -0.0091(12) 0.0157(13) 0.0042(13) C23 0.0210(12) 0.0108(12) 0.0295(13) 0.0061(9) 0.0035(10) -0.0009(10) C24 0.0271(14) 0.0259(15) 0.0341(15) 0.0126(11) -0.0026(11) -0.0021(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 C1 1.793(2) . ? Cl2 C1 1.791(2) . ? Mg1 O21 2.0451(16) . ? Mg1 O21 2.0451(16) 2_666 ? Mg1 O11 2.0834(16) 2_666 ? Mg1 O11 2.0834(16) . ? Mg1 O1 2.1338(17) 2_666 ? Mg1 O1 2.1338(17) . ? Mg2 O22 2.0187(16) 2_556 ? Mg2 O22 2.0187(16) . ? Mg2 O3 2.0806(18) . ? Mg2 O3 2.0806(17) 2_556 ? Mg2 O2 2.1006(17) 2_556 ? Mg2 O2 2.1006(17) . ? P1 O11 1.4941(17) . ? P1 O12 1.4945(17) . ? P1 O13 1.5769(18) . ? P1 C1 1.852(2) . ? P2 O21 1.4889(17) . ? P2 O22 1.4891(17) . ? P2 O23 1.5812(17) . ? P2 C1 1.866(3) . ? O1 H1A 0.87 . ? O1 H1B 0.92 . ? O2 H2A 0.87 . ? O2 H2B 0.91 . ? O3 H3A 0.85 . ? O3 H3B 0.88 . ? O13 C13 1.449(3) . ? O23 C23 1.475(3) . ? C13 C14 1.502(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C23 C24 1.498(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? 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 _geom_angle_publ_flag O21 Mg1 O21 180.0 . 2_666 ? O21 Mg1 O11 90.06(6) . 2_666 ? O21 Mg1 O11 89.94(6) 2_666 2_666 ? O21 Mg1 O11 89.94(6) . . ? O21 Mg1 O11 90.06(6) 2_666 . ? O11 Mg1 O11 180.000(1) 2_666 . ? O21 Mg1 O1 89.16(7) . 2_666 ? O21 Mg1 O1 90.84(7) 2_666 2_666 ? O11 Mg1 O1 87.24(7) 2_666 2_666 ? O11 Mg1 O1 92.76(7) . 2_666 ? O21 Mg1 O1 90.84(7) . . ? O21 Mg1 O1 89.16(7) 2_666 . ? O11 Mg1 O1 92.76(7) 2_666 . ? O11 Mg1 O1 87.24(7) . . ? O1 Mg1 O1 180.0 2_666 . ? O22 Mg2 O22 180.0 2_556 . ? O22 Mg2 O3 85.35(7) 2_556 . ? O22 Mg2 O3 94.65(7) . . ? O22 Mg2 O3 94.65(7) 2_556 2_556 ? O22 Mg2 O3 85.35(7) . 2_556 ? O3 Mg2 O3 180.0 . 2_556 ? O22 Mg2 O2 84.96(7) 2_556 2_556 ? O22 Mg2 O2 95.04(7) . 2_556 ? O3 Mg2 O2 88.61(7) . 2_556 ? O3 Mg2 O2 91.39(7) 2_556 2_556 ? O22 Mg2 O2 95.04(7) 2_556 . ? O22 Mg2 O2 84.96(7) . . ? O3 Mg2 O2 91.39(7) . . ? O3 Mg2 O2 88.61(7) 2_556 . ? O2 Mg2 O2 180.0 2_556 . ? O11 P1 O12 119.23(10) . . ? O11 P1 O13 106.56(10) . . ? O12 P1 O13 111.28(10) . . ? O11 P1 C1 105.16(10) . . ? O12 P1 C1 107.61(10) . . ? O13 P1 C1 106.13(10) . . ? O21 P2 O22 119.15(10) . . ? O21 P2 O23 107.38(9) . . ? O22 P2 O23 111.53(10) . . ? O21 P2 C1 106.30(10) . . ? O22 P2 C1 107.58(10) . . ? O23 P2 C1 103.72(10) . . ? Mg1 O1 H1A 115 . . ? Mg1 O1 H1B 124 . . ? H1A O1 H1B 99 . . ? Mg2 O2 H2A 108 . . ? Mg2 O2 H2B 128 . . ? H2A O2 H2B 102 . . ? Mg2 O3 H3A 117 . . ? Mg2 O3 H3B 107 . . ? H3A O3 H3B 109 . . ? P1 O11 Mg1 140.29(10) . . ? C13 O13 P1 124.48(16) . . ? P2 O21 Mg1 133.02(10) . . ? P2 O22 Mg2 176.77(11) . . ? C23 O23 P2 123.64(15) . . ? Cl2 C1 Cl1 107.98(12) . . ? Cl2 C1 P1 109.58(13) . . ? Cl1 C1 P1 109.35(12) . . ? Cl2 C1 P2 108.27(12) . . ? Cl1 C1 P2 110.63(13) . . ? P1 C1 P2 110.98(12) . . ? O13 C13 C14 107.6(2) . . ? O13 C13 H13A 110.2 . . ? C14 C13 H13A 110.2 . . ? O13 C13 H13B 110.2 . . ? C14 C13 H13B 110.2 . . ? H13A C13 H13B 108.5 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O23 C23 C24 108.0(2) . . ? O23 C23 H23A 110.1 . . ? C24 C23 H23A 110.1 . . ? O23 C23 H23B 110.1 . . ? C24 C23 H23B 110.1 . . ? H23A C23 H23B 108.4 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O12 P1 O11 Mg1 -93.07(17) . . . . ? O13 P1 O11 Mg1 140.03(15) . . . . ? C1 P1 O11 Mg1 27.64(19) . . . . ? O21 Mg1 O11 P1 -7.02(17) . . . . ? O21 Mg1 O11 P1 172.98(17) 2_666 . . . ? O11 Mg1 O11 P1 -167(100) 2_666 . . . ? O1 Mg1 O11 P1 -96.17(17) 2_666 . . . ? O1 Mg1 O11 P1 83.83(17) . . . . ? O11 P1 O13 C13 155.00(19) . . . . ? O12 P1 O13 C13 23.5(2) . . . . ? C1 P1 O13 C13 -93.3(2) . . . . ? O22 P2 O21 Mg1 72.06(16) . . . . ? O23 P2 O21 Mg1 -160.00(12) . . . . ? C1 P2 O21 Mg1 -49.49(16) . . . . ? O21 Mg1 O21 P2 37(100) 2_666 . . . ? O11 Mg1 O21 P2 -160.33(14) 2_666 . . . ? O11 Mg1 O21 P2 19.67(14) . . . . ? O1 Mg1 O21 P2 112.43(14) 2_666 . . . ? O1 Mg1 O21 P2 -67.57(14) . . . . ? O21 P2 O22 Mg2 -57(2) . . . . ? O23 P2 O22 Mg2 177(100) . . . . ? C1 P2 O22 Mg2 64(2) . . . . ? O22 Mg2 O22 P2 -34(100) 2_556 . . . ? O3 Mg2 O22 P2 92(2) . . . . ? O3 Mg2 O22 P2 -88(2) 2_556 . . . ? O2 Mg2 O22 P2 -179(100) 2_556 . . . ? O2 Mg2 O22 P2 1(2) . . . . ? O21 P2 O23 C23 -156.50(17) . . . . ? O22 P2 O23 C23 -24.3(2) . . . . ? C1 P2 O23 C23 91.23(19) . . . . ? O11 P1 C1 Cl2 65.84(14) . . . . ? O12 P1 C1 Cl2 -166.07(11) . . . . ? O13 P1 C1 Cl2 -46.85(14) . . . . ? O11 P1 C1 Cl1 -175.99(11) . . . . ? O12 P1 C1 Cl1 -47.90(15) . . . . ? O13 P1 C1 Cl1 71.32(14) . . . . ? O11 P1 C1 P2 -53.67(14) . . . . ? O12 P1 C1 P2 74.41(14) . . . . ? O13 P1 C1 P2 -166.36(11) . . . . ? O21 P2 C1 Cl2 -54.91(14) . . . . ? O22 P2 C1 Cl2 176.41(11) . . . . ? O23 P2 C1 Cl2 58.14(14) . . . . ? O21 P2 C1 Cl1 -173.05(11) . . . . ? O22 P2 C1 Cl1 58.27(14) . . . . ? O23 P2 C1 Cl1 -59.99(14) . . . . ? O21 P2 C1 P1 65.38(14) . . . . ? O22 P2 C1 P1 -63.29(14) . . . . ? O23 P2 C1 P1 178.44(11) . . . . ? P1 O13 C13 C14 -154.18(19) . . . . ? P2 O23 C23 C24 -138.54(19) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1B O2 0.92 2.09 2.969(2) 160 . O1 H1A O12 0.87 2.06 2.895(2) 162 2_566 O2 H2A O12 0.87 1.84 2.702(2) 172 . O2 H2B O11 0.91 2.01 2.854(2) 154 2_566 O3 H3A O23 0.85 1.90 2.733(2) 169 2_656 O3 H3B O12 0.88 2.28 3.043(3) 145 2_556 _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.918 _refine_diff_density_max 0.491 _refine_diff_density_min -0.446 _refine_diff_density_rms 0.079 #===END data_Structure_3 _database_code_CSD 163499 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(H2O)3Ca{Cl2C(PO3Et)2}2Ca(H2O)3]' _chemical_formula_sum 'C10 H32 Ca2 Cl4 O18 P4' _chemical_formula_weight 786.20 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' '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ca' 'Ca' 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'orthorhombic' _symmetry_space_group_name_H-M 'Cmca' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z+1/2' '-x+1/2, y+1, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' 'x, -y-1/2, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z-1/2' 'x+1/2, -y, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 24.0044(4) _cell_length_b 15.5269(2) _cell_length_c 7.9701(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2970.57(7) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 3.00 _cell_measurement_theta_max 29.10 _exptl_crystal_description 'cubic' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 1.700(11) _exptl_crystal_density_diffrn 1.758 _exptl_crystal_density_method 'flotation' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 1.030 _exptl_absorpt_correction_type 'semiempirical' _exptl_absorpt_correction_T_min 0.8204 _exptl_absorpt_correction_T_max 0.8204 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25221 _diffrn_reflns_av_R_equivalents 0.0280 _diffrn_reflns_av_sigmaI/netI 0.0170 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 29.10 _reflns_number_total 2020 _reflns_number_gt 1803 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'collect (Nonius, 1999)' _computing_cell_refinement 'Denzo, Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo, Scalepack' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0400P)^2^+6.0000P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2020 _refine_ls_number_parameters 101 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0362 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0831 _refine_ls_wR_factor_gt 0.0802 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Ca1 Ca 0.5000 0.60690(3) 0.20713(5) 0.01509(11) Uani 1 2 d S . . P P 0.404044(17) 0.43263(3) 0.13803(5) 0.01714(12) Uani 1 1 d . . . Cl Cl 0.31629(2) 0.43234(3) -0.12531(7) 0.03599(14) Uani 1 1 d . . . O1 O 0.5000 0.60416(18) 0.5087(3) 0.0601(8) Uani 1 2 d S . . O2A O 0.43024(14) 0.7063(2) 0.3110(5) 0.0528(13) Uani 0.664(8) 1 d P . . O2B O 0.5410(3) 0.7486(4) 0.2300(8) 0.050(3) Uani 0.336(8) 1 d P . . O11 O 0.43416(5) 0.49249(8) 0.25283(17) 0.0255(3) Uani 1 1 d . . . O12 O 0.43690(5) 0.37515(8) 0.02477(16) 0.0262(3) Uani 1 1 d . . . O13 O 0.36224(5) 0.37230(8) 0.23591(16) 0.0237(3) Uani 1 1 d . . . C1 C 0.35990(9) 0.5000 0.0000 0.0189(4) Uani 1 2 d S . . C11 C 0.33763(9) 0.39242(12) 0.3977(3) 0.0318(4) Uani 1 1 d . . . H11A H 0.3095 0.4377 0.3854 0.038 Uiso 1 1 calc R . . H11B H 0.3664 0.4128 0.4756 0.038 Uiso 1 1 calc R . . C12 C 0.31165(13) 0.31266(16) 0.4625(3) 0.0552(7) Uani 1 1 d . . . H12A H 0.2848 0.2914 0.3815 0.066 Uiso 1 1 calc R . . H12B H 0.2929 0.3249 0.5676 0.066 Uiso 1 1 calc R . . H12C H 0.3402 0.2695 0.4808 0.066 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 Ca1 0.0187(2) 0.01194(19) 0.0146(2) -0.00089(15) 0.000 0.000 P 0.0173(2) 0.0165(2) 0.0176(2) 0.00288(14) 0.00245(14) -0.00074(14) Cl 0.0320(3) 0.0322(3) 0.0437(3) 0.0021(2) -0.0150(2) -0.01335(18) O1 0.101(2) 0.0586(16) 0.0210(10) -0.0065(11) 0.000 0.000 O2A 0.058(2) 0.0491(19) 0.0515(19) -0.0221(17) -0.0178(16) 0.0328(16) O2B 0.076(5) 0.035(3) 0.039(3) -0.020(3) 0.024(3) -0.034(3) O11 0.0276(6) 0.0258(6) 0.0230(6) 0.0064(5) -0.0046(5) -0.0092(5) O12 0.0283(6) 0.0264(6) 0.0238(6) 0.0071(5) 0.0084(5) 0.0105(5) O13 0.0296(6) 0.0191(5) 0.0223(6) -0.0012(5) 0.0087(5) -0.0065(5) C1 0.0169(9) 0.0168(9) 0.0232(11) -0.0017(8) 0.000 0.000 C11 0.0408(11) 0.0257(9) 0.0290(9) -0.0025(7) 0.0174(8) -0.0051(8) C12 0.0786(18) 0.0394(12) 0.0476(14) -0.0015(11) 0.0343(14) -0.0213(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ca1 O1 2.404(2) . ? Ca1 O11 2.4056(12) . ? Ca1 O11 2.4056(12) 12_655 ? Ca1 O12 2.4059(12) 4_565 ? Ca1 O12 2.4059(12) 9_665 ? Ca1 O2B 2.416(5) 12_655 ? Ca1 O2B 2.416(5) . ? Ca1 O2A 2.423(2) 12_655 ? Ca1 O2A 2.423(2) . ? P O11 1.4912(13) . ? P O12 1.4944(13) . ? P O13 1.5790(12) . ? P C1 1.8514(13) . ? Cl C1 1.7880(13) . ? O2A O2B 1.151(8) 12_655 ? O2B O2A 1.151(7) 12_655 ? O12 Ca1 2.4059(12) 9_665 ? O13 C11 1.452(2) . ? C1 Cl 1.7879(13) 4_565 ? C1 P 1.8514(13) 4_565 ? C11 C12 1.480(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? 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 _geom_angle_publ_flag O1 Ca1 O11 80.53(6) . . ? O1 Ca1 O11 80.53(6) . 12_655 ? O11 Ca1 O11 82.15(6) . 12_655 ? O1 Ca1 O12 140.37(3) . 4_565 ? O11 Ca1 O12 77.77(4) . 4_565 ? O11 Ca1 O12 127.99(5) 12_655 4_565 ? O1 Ca1 O12 140.37(3) . 9_665 ? O11 Ca1 O12 127.99(5) . 9_665 ? O11 Ca1 O12 77.77(4) 12_655 9_665 ? O12 Ca1 O12 78.04(6) 4_565 9_665 ? O1 Ca1 O2B 86.60(16) . 12_655 ? O11 Ca1 O2B 113.2(2) . 12_655 ? O11 Ca1 O2B 158.16(14) 12_655 12_655 ? O12 Ca1 O2B 72.32(11) 4_565 12_655 ? O12 Ca1 O2B 102.1(2) 9_665 12_655 ? O1 Ca1 O2B 86.60(16) . . ? O11 Ca1 O2B 158.16(14) . . ? O11 Ca1 O2B 113.2(2) 12_655 . ? O12 Ca1 O2B 102.1(2) 4_565 . ? O12 Ca1 O2B 72.32(11) 9_665 . ? O2B Ca1 O2B 48.0(4) 12_655 . ? O1 Ca1 O2A 70.72(10) . 12_655 ? O11 Ca1 O2A 150.78(10) . 12_655 ? O11 Ca1 O2A 87.96(12) 12_655 12_655 ? O12 Ca1 O2A 128.60(12) 4_565 12_655 ? O12 Ca1 O2A 75.73(7) 9_665 12_655 ? O2B Ca1 O2A 71.1(2) 12_655 12_655 ? O2B Ca1 O2A 27.53(18) . 12_655 ? O1 Ca1 O2A 70.72(10) . . ? O11 Ca1 O2A 87.96(12) . . ? O11 Ca1 O2A 150.78(10) 12_655 . ? O12 Ca1 O2A 75.73(7) 4_565 . ? O12 Ca1 O2A 128.60(12) 9_665 . ? O2B Ca1 O2A 27.53(18) 12_655 . ? O2B Ca1 O2A 71.1(2) . . ? O2A Ca1 O2A 87.45(17) 12_655 . ? O11 P O12 119.15(8) . . ? O11 P O13 112.01(7) . . ? O12 P O13 106.23(7) . . ? O11 P C1 106.85(6) . . ? O12 P C1 106.29(6) . . ? O13 P C1 105.37(8) . . ? O2B O2A Ca1 75.9(3) 12_655 . ? O2A O2B Ca1 76.6(3) 12_655 . ? P O11 Ca1 133.31(8) . . ? P O12 Ca1 136.65(7) . 9_665 ? C11 O13 P 124.72(11) . . ? Cl C1 Cl 108.34(12) 4_565 . ? Cl C1 P 109.58(2) 4_565 . ? Cl C1 P 109.57(2) . . ? Cl C1 P 109.57(2) 4_565 4_565 ? Cl C1 P 109.58(2) . 4_565 ? P C1 P 110.16(11) . 4_565 ? O13 C11 C12 107.52(16) . . ? O13 C11 H11A 110.2 . . ? C12 C11 H11A 110.2 . . ? O13 C11 H11B 110.2 . . ? C12 C11 H11B 110.2 . . ? H11A C11 H11B 108.5 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Ca1 O2A O2B 122.4(3) . . . 12_655 ? O11 Ca1 O2A O2B -157.0(3) . . . 12_655 ? O11 Ca1 O2A O2B 133.1(3) 12_655 . . 12_655 ? O12 Ca1 O2A O2B -79.1(3) 4_565 . . 12_655 ? O12 Ca1 O2A O2B -17.5(3) 9_665 . . 12_655 ? O2B Ca1 O2A O2B 29.3(3) . . . 12_655 ? O2A Ca1 O2A O2B 51.9(3) 12_655 . . 12_655 ? O1 Ca1 O2B O2A 53.0(3) . . . 12_655 ? O11 Ca1 O2B O2A 106.8(6) . . . 12_655 ? O11 Ca1 O2B O2A -25.2(3) 12_655 . . 12_655 ? O12 Ca1 O2B O2A -166.1(2) 4_565 . . 12_655 ? O12 Ca1 O2B O2A -93.0(3) 9_665 . . 12_655 ? O2B Ca1 O2B O2A 141.5(3) 12_655 . . 12_655 ? O2A Ca1 O2B O2A 123.8(3) . . . 12_655 ? O12 P O11 Ca1 58.59(12) . . . . ? O13 P O11 Ca1 -176.61(9) . . . . ? C1 P O11 Ca1 -61.71(12) . . . . ? O1 Ca1 O11 P -175.21(11) . . . . ? O11 Ca1 O11 P -93.57(10) 12_655 . . . ? O12 Ca1 O11 P 38.17(10) 4_565 . . . ? O12 Ca1 O11 P -25.84(13) 9_665 . . . ? O2B Ca1 O11 P 102.66(17) 12_655 . . . ? O2B Ca1 O11 P 130.1(6) . . . . ? O2A Ca1 O11 P -164.9(2) 12_655 . . . ? O2A Ca1 O11 P 114.00(13) . . . . ? O11 P O12 Ca1 -64.28(13) . . . 9_665 ? O13 P O12 Ca1 168.19(10) . . . 9_665 ? C1 P O12 Ca1 56.31(13) . . . 9_665 ? O11 P O13 C11 24.19(17) . . . . ? O12 P O13 C11 155.86(15) . . . . ? C1 P O13 C11 -91.62(15) . . . . ? O11 P C1 Cl -54.60(10) . . . 4_565 ? O12 P C1 Cl 177.18(8) . . . 4_565 ? O13 P C1 Cl 64.70(9) . . . 4_565 ? O11 P C1 Cl -173.34(8) . . . . ? O12 P C1 Cl 58.44(10) . . . . ? O13 P C1 Cl -54.04(9) . . . . ? O11 P C1 P 66.03(6) . . . 4_565 ? O12 P C1 P -62.20(6) . . . 4_565 ? O13 P C1 P -174.68(5) . . . 4_565 ? P O13 C11 C12 -167.54(18) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 29.10 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.931 _refine_diff_density_min -0.496 _refine_diff_density_rms 0.072 #===END data_Structure_4 _database_code_CSD 163500 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(H2O)3Sr{Cl2C(PO3Et)2}2Sr(H2O)3]' _chemical_formula_sum 'C10 H32 Cl4 O18 P4 Sr2' _chemical_formula_weight 881.28 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' '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sr' 'Sr' -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'orthorhombic' _symmetry_space_group_name_H-M 'Cmca' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z+1/2' '-x+1/2, y+1, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' 'x, -y-1/2, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z-1/2' 'x+1/2, -y, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 24.0676(9) _cell_length_b 15.7465(6) _cell_length_c 8.0360(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3045.49(18) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 3.62 _cell_measurement_theta_max 27.65 _exptl_crystal_description 'cubic' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 1.859(8) _exptl_crystal_density_diffrn 1.922 _exptl_crystal_density_method 'flotation' _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 4.133 _exptl_absorpt_correction_type 'semiempirical' _exptl_absorpt_correction_T_min 0.4919 _exptl_absorpt_correction_T_max 0.6826 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41374 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.0195 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.62 _diffrn_reflns_theta_max 27.65 _reflns_number_total 1733 _reflns_number_gt 1624 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'collect (Nonius, 1999)' _computing_cell_refinement 'Denzo, Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo, Scalepack' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0300P)^2^+10.0000P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1733 _refine_ls_number_parameters 100 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0295 _refine_ls_R_factor_gt 0.0273 _refine_ls_wR_factor_ref 0.0708 _refine_ls_wR_factor_gt 0.0691 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Sr Sr 0.5000 0.608242(17) 0.21093(3) 0.01690(10) Uani 1 2 d S . . P P 0.39987(3) 0.43265(4) 0.13685(8) 0.02069(15) Uani 1 1 d . . . Cl Cl 0.31368(3) 0.43425(5) -0.12473(10) 0.0423(2) Uani 1 1 d . . . O1 O 0.5000 0.6029(3) 0.5258(4) 0.0653(12) Uani 1 2 d S . . O2A O 0.42649(19) 0.7112(3) 0.3184(5) 0.0559(11) Uani 0.65 1 d P . . O2B O 0.5424(3) 0.7553(4) 0.2330(9) 0.0509(19) Uani 0.35 1 d P . . O11 O 0.43008(8) 0.48997(12) 0.2518(3) 0.0314(4) Uani 1 1 d . . . O12 O 0.43242(9) 0.37587(12) 0.0262(2) 0.0322(4) Uani 1 1 d . . . O13 O 0.35724(8) 0.37453(11) 0.2311(2) 0.0275(4) Uani 1 1 d . . . C1 C 0.35709(14) 0.5000 0.0000 0.0215(6) Uani 1 2 d S . . C11 C 0.33440(15) 0.39261(17) 0.3933(4) 0.0368(7) Uani 1 1 d . . . H11A H 0.3057 0.4365 0.3846 0.044 Uiso 1 1 calc R . . H11B H 0.3637 0.4132 0.4678 0.044 Uiso 1 1 calc R . . C12 C 0.3104(2) 0.3140(2) 0.4587(5) 0.0672(13) Uani 1 1 d . . . H12A H 0.2859 0.2893 0.3760 0.081 Uiso 1 1 calc R . . H12B H 0.2894 0.3264 0.5589 0.081 Uiso 1 1 calc R . . H12C H 0.3400 0.2743 0.4846 0.081 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 Sr 0.02297(16) 0.01477(15) 0.01296(17) -0.00085(9) 0.000 0.000 P 0.0221(3) 0.0225(3) 0.0175(3) 0.0044(2) 0.0029(2) -0.0012(2) Cl 0.0396(4) 0.0396(4) 0.0477(5) 0.0034(3) -0.0187(3) -0.0155(3) O1 0.100(3) 0.078(3) 0.0188(18) -0.0017(15) 0.000 0.000 O2A 0.061(3) 0.051(2) 0.056(2) -0.0264(19) -0.018(2) 0.032(2) O2B 0.080(5) 0.033(3) 0.041(4) -0.017(3) 0.019(4) -0.032(4) O11 0.0359(10) 0.0331(10) 0.0253(9) 0.0096(8) -0.0076(8) -0.0118(8) O12 0.0380(11) 0.0334(9) 0.0250(10) 0.0108(7) 0.0112(8) 0.0145(8) O13 0.0350(10) 0.0238(8) 0.0238(9) -0.0007(7) 0.0102(7) -0.0076(7) C1 0.0204(15) 0.0197(15) 0.0243(17) -0.0019(12) 0.000 0.000 C11 0.0508(18) 0.0314(14) 0.0282(15) -0.0009(10) 0.0190(13) -0.0034(12) C12 0.099(3) 0.050(2) 0.052(2) 0.0025(17) 0.042(2) -0.021(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sr O12 2.5176(19) 4_565 ? Sr O12 2.5176(19) 9_665 ? Sr O1 2.531(4) . ? Sr O11 2.5315(18) . ? Sr O11 2.5315(18) 12_655 ? Sr O2B 2.536(6) 12_655 ? Sr O2B 2.536(6) . ? Sr O2A 2.550(4) 12_655 ? Sr O2A 2.550(4) . ? Sr P 3.7158(7) . ? Sr P 3.7158(7) 12_655 ? Sr P 3.7462(6) 4_565 ? P O11 1.482(2) . ? P O12 1.4848(19) . ? P O13 1.5694(18) . ? P C1 1.8423(19) . ? P Sr 3.7462(6) 9_665 ? Cl C1 1.780(2) . ? O2A O2B 1.231(9) 12_655 ? O2B O2A 1.231(9) 12_655 ? O12 Sr 2.5176(18) 9_665 ? O13 C11 1.443(3) . ? C1 Cl 1.780(2) 4_565 ? C1 P 1.8423(19) 4_565 ? C11 C12 1.463(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? 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 _geom_angle_publ_flag O12 Sr O12 80.49(10) 4_565 9_665 ? O12 Sr O1 139.44(5) 4_565 . ? O12 Sr O1 139.44(5) 9_665 . ? O12 Sr O11 75.04(6) 4_565 . ? O12 Sr O11 126.93(7) 9_665 . ? O1 Sr O11 81.13(8) . . ? O12 Sr O11 126.93(7) 4_565 12_655 ? O12 Sr O11 75.04(6) 9_665 12_655 ? O1 Sr O11 81.13(8) . 12_655 ? O11 Sr O11 83.33(9) . 12_655 ? O12 Sr O2B 72.69(16) 4_565 12_655 ? O12 Sr O2B 102.8(2) 9_665 12_655 ? O1 Sr O2B 87.73(19) . 12_655 ? O11 Sr O2B 113.3(2) . 12_655 ? O11 Sr O2B 158.40(18) 12_655 12_655 ? O12 Sr O2B 102.8(2) 4_565 . ? O12 Sr O2B 72.69(16) 9_665 . ? O1 Sr O2B 87.73(19) . . ? O11 Sr O2B 158.40(18) . . ? O11 Sr O2B 113.3(2) 12_655 . ? O2B Sr O2B 47.4(4) 12_655 . ? O12 Sr O2A 129.89(13) 4_565 12_655 ? O12 Sr O2A 75.22(10) 9_665 12_655 ? O1 Sr O2A 71.50(12) . 12_655 ? O11 Sr O2A 152.24(11) . 12_655 ? O11 Sr O2A 87.85(13) 12_655 12_655 ? O2B Sr O2A 71.0(2) 12_655 12_655 ? O2B Sr O2A 28.0(2) . 12_655 ? O12 Sr O2A 75.22(10) 4_565 . ? O12 Sr O2A 129.89(13) 9_665 . ? O1 Sr O2A 71.50(12) . . ? O11 Sr O2A 87.85(13) . . ? O11 Sr O2A 152.24(11) 12_655 . ? O2B Sr O2A 28.0(2) 12_655 . ? O2B Sr O2A 71.0(2) . . ? O2A Sr O2A 87.9(2) 12_655 . ? O12 Sr P 62.21(4) 4_565 . ? O12 Sr P 111.82(5) 9_665 . ? O1 Sr P 97.78(7) . . ? O11 Sr P 16.71(5) . . ? O11 Sr P 84.52(5) 12_655 . ? O2B Sr P 115.45(19) 12_655 . ? O2B Sr P 162.0(2) . . ? O2A Sr P 167.74(12) 12_655 . ? O2A Sr P 94.43(11) . . ? O12 Sr P 111.82(5) 4_565 12_655 ? O12 Sr P 62.21(4) 9_665 12_655 ? O1 Sr P 97.78(7) . 12_655 ? O11 Sr P 84.52(5) . 12_655 ? O11 Sr P 16.71(5) 12_655 12_655 ? O2B Sr P 162.0(2) 12_655 12_655 ? O2B Sr P 115.45(19) . 12_655 ? O2A Sr P 94.43(11) 12_655 12_655 ? O2A Sr P 167.74(12) . 12_655 ? P Sr P 80.87(2) . 12_655 ? O12 Sr P 15.60(4) 4_565 4_565 ? O12 Sr P 82.42(5) 9_665 4_565 ? O1 Sr P 137.72(3) . 4_565 ? O11 Sr P 62.79(5) . 4_565 ? O11 Sr P 113.46(5) 12_655 4_565 ? O2B Sr P 87.16(15) 12_655 4_565 ? O2B Sr P 117.9(2) . 4_565 ? O2A Sr P 143.92(12) 12_655 4_565 ? O2A Sr P 85.16(9) . 4_565 ? P Sr P 48.343(17) . 4_565 ? P Sr P 99.777(14) 12_655 4_565 ? O11 P O12 118.77(13) . . ? O11 P O13 112.03(11) . . ? O12 P O13 106.43(11) . . ? O11 P C1 107.20(9) . . ? O12 P C1 106.50(9) . . ? O13 P C1 104.98(12) . . ? O11 P Sr 29.41(8) . . ? O12 P Sr 101.64(9) . . ? O13 P Sr 141.31(7) . . ? C1 P Sr 91.70(7) . . ? O11 P Sr 104.72(9) . 9_665 ? O12 P Sr 27.14(7) . 9_665 ? O13 P Sr 132.86(7) . 9_665 ? C1 P Sr 90.75(7) . 9_665 ? Sr P Sr 80.223(14) . 9_665 ? O2B O2A Sr 75.4(3) 12_655 . ? O2A O2B Sr 76.6(3) 12_655 . ? P O11 Sr 133.88(12) . . ? P O12 Sr 137.26(11) . 9_665 ? C11 O13 P 124.73(17) . . ? Cl C1 Cl 108.12(18) . 4_565 ? Cl C1 P 109.23(3) . . ? Cl C1 P 109.07(3) 4_565 . ? Cl C1 P 109.07(3) . 4_565 ? Cl C1 P 109.23(3) 4_565 4_565 ? P C1 P 112.05(17) . 4_565 ? O13 C11 C12 107.9(2) . . ? O13 C11 H11A 110.1 . . ? C12 C11 H11A 110.1 . . ? O13 C11 H11B 110.1 . . ? C12 C11 H11B 110.1 . . ? H11A C11 H11B 108.4 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O12 Sr P O11 -137.82(18) 4_565 . . . ? O12 Sr P O11 156.53(17) 9_665 . . . ? O1 Sr P O11 4.81(17) . . . . ? O11 Sr P O11 85.05(17) 12_655 . . . ? O2B Sr P O11 -86.4(3) 12_655 . . . ? O2B Sr P O11 -102.2(5) . . . . ? O2A Sr P O11 33.3(5) 12_655 . . . ? O2A Sr P O11 -67.1(2) . . . . ? P Sr P O11 101.49(16) 12_655 . . . ? P Sr P O11 -146.59(16) 4_565 . . . ? O12 Sr P O12 92.75(7) 4_565 . . . ? O12 Sr P O12 27.10(12) 9_665 . . . ? O1 Sr P O12 -124.62(10) . . . . ? O11 Sr P O12 -129.43(18) . . . . ? O11 Sr P O12 -44.38(9) 12_655 . . . ? O2B Sr P O12 144.2(2) 12_655 . . . ? O2B Sr P O12 128.4(5) . . . . ? O2A Sr P O12 -96.2(5) 12_655 . . . ? O2A Sr P O12 163.47(13) . . . . ? P Sr P O12 -27.94(8) 12_655 . . . ? P Sr P O12 83.98(8) 4_565 . . . ? O12 Sr P O13 -131.27(14) 4_565 . . . ? O12 Sr P O13 163.08(13) 9_665 . . . ? O1 Sr P O13 11.36(14) . . . . ? O11 Sr P O13 6.5(2) . . . . ? O11 Sr P O13 91.60(14) 12_655 . . . ? O2B Sr P O13 -79.8(2) 12_655 . . . ? O2B Sr P O13 -95.6(5) . . . . ? O2A Sr P O13 39.8(5) 12_655 . . . ? O2A Sr P O13 -60.55(17) . . . . ? P Sr P O13 108.04(13) 12_655 . . . ? P Sr P O13 -140.04(13) 4_565 . . . ? O12 Sr P C1 -14.48(8) 4_565 . . . ? O12 Sr P C1 -80.13(7) 9_665 . . . ? O1 Sr P C1 128.15(8) . . . . ? O11 Sr P C1 123.34(18) . . . . ? O11 Sr P C1 -151.61(7) 12_655 . . . ? O2B Sr P C1 37.0(2) 12_655 . . . ? O2B Sr P C1 21.2(5) . . . . ? O2A Sr P C1 156.6(5) 12_655 . . . ? O2A Sr P C1 56.24(12) . . . . ? P Sr P C1 -135.17(6) 12_655 . . . ? P Sr P C1 -23.25(6) 4_565 . . . ? O12 Sr P Sr 75.99(6) 4_565 . . 9_665 ? O12 Sr P Sr 10.34(5) 9_665 . . 9_665 ? O1 Sr P Sr -141.38(6) . . . 9_665 ? O11 Sr P Sr -146.19(16) . . . 9_665 ? O11 Sr P Sr -61.14(5) 12_655 . . 9_665 ? O2B Sr P Sr 127.43(19) 12_655 . . 9_665 ? O2B Sr P Sr 111.6(5) . . . 9_665 ? O2A Sr P Sr -112.9(5) 12_655 . . 9_665 ? O2A Sr P Sr 146.71(10) . . . 9_665 ? P Sr P Sr -44.698(14) 12_655 . . 9_665 ? P Sr P Sr 67.216(19) 4_565 . . 9_665 ? O12 Sr O2A O2B -80.8(4) 4_565 . . 12_655 ? O12 Sr O2A O2B -17.2(4) 9_665 . . 12_655 ? O1 Sr O2A O2B 122.7(4) . . . 12_655 ? O11 Sr O2A O2B -155.9(4) . . . 12_655 ? O11 Sr O2A O2B 132.8(4) 12_655 . . 12_655 ? O2B Sr O2A O2B 28.6(4) . . . 12_655 ? O2A Sr O2A O2B 51.5(4) 12_655 . . 12_655 ? P Sr O2A O2B -140.6(4) . . . 12_655 ? P Sr O2A O2B 152.6(4) 12_655 . . 12_655 ? P Sr O2A O2B -93.1(4) 4_565 . . 12_655 ? O12 Sr O2B O2A -166.6(3) 4_565 . . 12_655 ? O12 Sr O2B O2A -91.0(4) 9_665 . . 12_655 ? O1 Sr O2B O2A 53.0(4) . . . 12_655 ? O11 Sr O2B O2A 111.7(6) . . . 12_655 ? O11 Sr O2B O2A -26.3(4) 12_655 . . 12_655 ? O2B Sr O2B O2A 142.0(3) 12_655 . . 12_655 ? O2A Sr O2B O2A 124.2(4) . . . 12_655 ? P Sr O2B O2A 161.5(3) . . . 12_655 ? P Sr O2B O2A -44.5(4) 12_655 . . 12_655 ? P Sr O2B O2A -162.2(3) 4_565 . . 12_655 ? O12 P O11 Sr 59.66(18) . . . . ? O13 P O11 Sr -175.59(13) . . . . ? C1 P O11 Sr -60.94(18) . . . . ? Sr P O11 Sr 34.54(16) 9_665 . . . ? O12 Sr O11 P 37.94(16) 4_565 . . . ? O12 Sr O11 P -27.55(19) 9_665 . . . ? O1 Sr O11 P -175.18(18) . . . . ? O11 Sr O11 P -93.16(15) 12_655 . . . ? O2B Sr O11 P 101.2(2) 12_655 . . . ? O2B Sr O11 P 125.0(6) . . . . ? O2A Sr O11 P -165.5(2) 12_655 . . . ? O2A Sr O11 P 113.21(18) . . . . ? P Sr O11 P -76.40(16) 12_655 . . . ? P Sr O11 P 27.55(13) 4_565 . . . ? O11 P O12 Sr -64.2(2) . . . 9_665 ? O13 P O12 Sr 168.39(16) . . . 9_665 ? C1 P O12 Sr 56.8(2) . . . 9_665 ? Sr P O12 Sr -38.54(18) . . . 9_665 ? O11 P O13 C11 21.3(3) . . . . ? O12 P O13 C11 152.6(2) . . . . ? C1 P O13 C11 -94.7(2) . . . . ? Sr P O13 C11 17.8(3) . . . . ? Sr P O13 C11 159.8(2) 9_665 . . . ? O11 P C1 Cl -173.28(12) . . . . ? O12 P C1 Cl 58.62(16) . . . . ? O13 P C1 Cl -53.99(13) . . . . ? Sr P C1 Cl 161.29(11) . . . . ? Sr P C1 Cl 81.05(11) 9_665 . . . ? O11 P C1 Cl -55.31(16) . . . 4_565 ? O12 P C1 Cl 176.59(12) . . . 4_565 ? O13 P C1 Cl 63.98(13) . . . 4_565 ? Sr P C1 Cl -80.74(11) . . . 4_565 ? Sr P C1 Cl -160.98(11) 9_665 . . 4_565 ? O11 P C1 P 65.75(9) . . . 4_565 ? O12 P C1 P -62.35(9) . . . 4_565 ? O13 P C1 P -174.96(8) . . . 4_565 ? Sr P C1 P 40.325(9) . . . 4_565 ? Sr P C1 P -39.915(9) 9_665 . . 4_565 ? P O13 C11 C12 -163.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 27.65 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 0.846 _refine_diff_density_min -0.457 _refine_diff_density_rms 0.078 #===END data_Structure_5 _database_code_CSD 163501 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(H2O)2Ba{Cl2C(PO3Et)2}2Ba(H2O)2]n' _chemical_formula_sum 'C10 H28 Ba2 Cl4 O16 P4' _chemical_formula_weight 944.68 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' '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ba' 'Ba' -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 25.0009(10) _cell_length_b 6.9490(4) _cell_length_c 17.3764(15) _cell_angle_alpha 90.00 _cell_angle_beta 93.297(4) _cell_angle_gamma 90.00 _cell_volume 3013.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 25.00 _exptl_crystal_description 'needle' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 2.074(68) _exptl_crystal_density_diffrn 2.082 _exptl_crystal_density_method 'flotation' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 3.226 _exptl_absorpt_correction_type 'semiempirical' _exptl_absorpt_correction_T_min 0.5647 _exptl_absorpt_correction_T_max 0.7386 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33369 _diffrn_reflns_av_R_equivalents 0.0776 _diffrn_reflns_av_sigmaI/netI 0.0658 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5229 _reflns_number_gt 4017 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'collect (Nonius, 1999)' _computing_cell_refinement 'Denzo, Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo, Scalepack' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0300P)^2^+10.0000P] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00081(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5229 _refine_ls_number_parameters 330 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0799 _refine_ls_R_factor_gt 0.0533 _refine_ls_wR_factor_ref 0.1127 _refine_ls_wR_factor_gt 0.1053 _refine_ls_goodness_of_fit_ref 1.351 _refine_ls_restrained_S_all 1.351 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Ba1 Ba 0.23182(2) 0.68001(7) 0.17757(3) 0.02010(17) Uani 1 1 d . . . Ba2 Ba 0.27393(2) 0.25937(7) -0.00682(3) 0.02007(17) Uani 1 1 d . . . Cl1 Cl 0.07612(9) -0.0148(3) 0.15703(13) 0.0309(5) Uani 1 1 d . . . Cl2 Cl 0.08838(9) 0.3292(3) 0.06395(13) 0.0313(5) Uani 1 1 d . . . Cl3 Cl 0.43053(9) 0.9359(3) 0.00630(13) 0.0300(5) Uani 1 1 d . . . Cl4 Cl 0.41659(9) 0.5926(3) 0.09858(12) 0.0286(5) Uani 1 1 d . . . P1 P 0.17920(9) 0.2046(3) 0.16781(13) 0.0215(5) Uani 1 1 d . . . P2 P 0.14323(9) -0.0276(3) 0.02093(13) 0.0223(5) Uani 1 1 d . . . P3 P 0.36467(9) 0.9546(3) 0.14477(13) 0.0222(5) Uani 1 1 d . . . P4 P 0.32494(9) 0.7329(3) -0.00079(13) 0.0204(5) Uani 1 1 d . . . O11 O 0.2162(2) 0.3132(8) 0.1185(3) 0.0227(13) Uani 1 1 d . . . O12 O 0.1996(2) 0.0375(8) 0.2132(3) 0.0255(14) Uani 1 1 d . . . O13 O 0.1558(2) 0.3660(8) 0.2214(3) 0.0245(13) Uani 1 1 d . . . O21 O 0.1767(2) 0.0981(9) -0.0252(3) 0.0286(14) Uani 1 1 d . . . O22 O 0.1665(2) -0.2076(7) 0.0556(3) 0.0235(13) Uani 1 1 d . . . O23 O 0.0893(2) -0.0656(8) -0.0283(3) 0.0272(14) Uani 1 1 d . . . O31 O 0.3321(2) 0.8312(8) 0.1934(3) 0.0238(13) Uani 1 1 d . . . O32 O 0.3410(2) 1.1357(8) 0.1114(3) 0.0233(13) Uani 1 1 d . . . O33 O 0.4202(2) 0.9922(8) 0.1906(3) 0.0250(14) Uani 1 1 d . . . O41 O 0.2870(2) 0.6359(8) 0.0500(3) 0.0239(13) Uani 1 1 d . . . O42 O 0.3072(2) 0.9059(8) -0.0468(3) 0.0228(13) Uani 1 1 d . . . O43 O 0.3445(2) 0.5614(7) -0.0532(3) 0.0212(13) Uani 1 1 d . . . O1 O 0.2288(2) 0.7177(8) 0.3340(3) 0.0317(15) Uani 1 1 d . . . O2 O 0.3218(2) 0.4300(8) 0.2216(3) 0.0295(14) Uani 1 1 d . . . O3 O 0.1876(2) 0.5091(8) -0.0558(3) 0.0249(14) Uani 1 1 d . . . O4 O 0.2704(2) 0.2772(8) -0.1660(3) 0.0305(15) Uani 1 1 d . . . C1 C 0.1224(3) 0.1231(12) 0.1032(5) 0.0228(19) Uani 1 1 d . . . C2 C 0.3837(3) 0.8041(12) 0.0627(5) 0.023(2) Uani 1 1 d . . . C13 C 0.1293(4) 0.3275(13) 0.2919(5) 0.032(2) Uani 1 1 d . . . H13A H 0.1493 0.3899 0.3360 0.038 Uiso 1 1 calc R . . H13B H 0.1286 0.1872 0.3016 0.038 Uiso 1 1 calc R . . C14 C 0.0726(4) 0.4047(16) 0.2847(6) 0.046(3) Uani 1 1 d . . . H14A H 0.0735 0.5450 0.2791 0.069 Uiso 1 1 calc R . . H14B H 0.0540 0.3710 0.3309 0.069 Uiso 1 1 calc R . . H14C H 0.0536 0.3481 0.2393 0.069 Uiso 1 1 calc R . . C23 C 0.0546(4) -0.2296(12) -0.0183(5) 0.030(2) Uani 1 1 d . . . H23A H 0.0187 -0.1845 -0.0053 0.036 Uiso 1 1 calc R . . H23B H 0.0695 -0.3104 0.0247 0.036 Uiso 1 1 calc R . . C24 C 0.0499(4) -0.3473(13) -0.0916(5) 0.031(2) Uani 1 1 d . . . H24A H 0.0307 -0.2727 -0.1324 0.047 Uiso 1 1 calc R . . H24B H 0.0301 -0.4660 -0.0824 0.047 Uiso 1 1 calc R . . H24C H 0.0858 -0.3795 -0.1076 0.047 Uiso 1 1 calc R . . C33 C 0.4526(3) 1.1623(12) 0.1795(5) 0.027(2) Uani 1 1 d . . . H33A H 0.4416 1.2674 0.2137 0.032 Uiso 1 1 calc R . . H33B H 0.4478 1.2070 0.1254 0.032 Uiso 1 1 calc R . . C34 C 0.5094(3) 1.1097(14) 0.1981(6) 0.036(2) Uani 1 1 d . . . H34A H 0.5133 1.0602 0.2509 0.053 Uiso 1 1 calc R . . H34B H 0.5321 1.2237 0.1935 0.053 Uiso 1 1 calc R . . H34C H 0.5204 1.0104 0.1621 0.053 Uiso 1 1 calc R . . C43 C 0.3755(4) 0.5821(13) -0.1205(5) 0.029(2) Uani 1 1 d . . . H43A H 0.3903 0.7139 -0.1227 0.035 Uiso 1 1 calc R . . H43B H 0.3523 0.5598 -0.1678 0.035 Uiso 1 1 calc R . . C44 C 0.4201(4) 0.4377(15) -0.1153(6) 0.050(3) Uani 1 1 d . . . H44A H 0.4418 0.4572 -0.0671 0.075 Uiso 1 1 calc R . . H44B H 0.4426 0.4540 -0.1592 0.075 Uiso 1 1 calc R . . H44C H 0.4050 0.3075 -0.1160 0.075 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 Ba1 0.0274(3) 0.0162(3) 0.0169(3) -0.0005(2) 0.0020(2) 0.0000(2) Ba2 0.0268(3) 0.0166(3) 0.0168(3) 0.0002(2) 0.0018(2) -0.0001(2) Cl1 0.0343(13) 0.0296(12) 0.0296(13) -0.0003(10) 0.0092(10) -0.0087(10) Cl2 0.0318(13) 0.0251(12) 0.0365(14) 0.0020(10) -0.0023(10) 0.0047(10) Cl3 0.0329(13) 0.0311(13) 0.0266(13) -0.0001(10) 0.0075(10) -0.0090(10) Cl4 0.0366(13) 0.0220(11) 0.0271(13) 0.0020(9) 0.0000(10) 0.0071(10) P1 0.0266(13) 0.0164(12) 0.0217(13) 0.0001(9) 0.0027(10) 0.0012(9) P2 0.0253(13) 0.0221(12) 0.0196(13) 0.0023(10) 0.0007(10) -0.0023(10) P3 0.0283(13) 0.0198(12) 0.0183(12) 0.0006(9) -0.0015(10) -0.0015(10) P4 0.0268(13) 0.0176(12) 0.0170(12) -0.0016(9) 0.0020(9) -0.0004(10) O11 0.031(3) 0.022(3) 0.015(3) -0.003(2) 0.001(2) -0.006(3) O12 0.035(4) 0.018(3) 0.023(3) -0.002(3) 0.000(3) 0.005(3) O13 0.035(3) 0.020(3) 0.019(3) 0.002(2) 0.007(3) 0.004(3) O21 0.034(4) 0.032(4) 0.020(3) 0.001(3) 0.005(3) -0.011(3) O22 0.034(3) 0.015(3) 0.022(3) -0.005(2) -0.001(3) 0.005(2) O23 0.025(3) 0.025(3) 0.031(4) 0.000(3) -0.007(3) -0.006(3) O31 0.035(4) 0.021(3) 0.016(3) 0.000(2) 0.005(3) -0.008(3) O32 0.030(3) 0.018(3) 0.021(3) 0.000(2) -0.004(3) 0.003(3) O33 0.030(3) 0.019(3) 0.025(4) 0.005(3) -0.006(3) -0.007(3) O41 0.023(3) 0.026(3) 0.023(3) -0.007(3) 0.003(3) -0.002(3) O42 0.028(3) 0.021(3) 0.019(3) 0.003(3) -0.002(2) 0.002(3) O43 0.030(3) 0.020(3) 0.014(3) 0.006(2) 0.007(2) 0.002(3) O1 0.040(4) 0.028(4) 0.027(4) 0.001(3) 0.001(3) 0.003(3) O2 0.033(4) 0.028(4) 0.028(4) -0.001(3) -0.002(3) 0.001(3) O3 0.029(3) 0.020(3) 0.025(4) 0.002(3) -0.002(3) 0.004(3) O4 0.040(4) 0.028(4) 0.023(4) 0.001(3) -0.001(3) 0.001(3) C1 0.030(5) 0.016(4) 0.022(5) 0.008(4) 0.002(4) 0.001(4) C2 0.028(5) 0.017(4) 0.024(5) 0.002(4) 0.003(4) -0.001(4) C13 0.049(6) 0.033(5) 0.014(5) -0.005(4) 0.014(4) -0.009(5) C14 0.036(6) 0.059(7) 0.045(7) -0.018(6) 0.016(5) 0.002(5) C23 0.036(5) 0.019(5) 0.034(6) 0.007(4) -0.004(4) -0.005(4) C24 0.034(6) 0.024(5) 0.036(6) -0.004(4) 0.001(4) -0.002(4) C33 0.032(5) 0.018(5) 0.030(5) 0.002(4) -0.001(4) -0.009(4) C34 0.027(5) 0.040(6) 0.039(6) 0.004(5) 0.000(4) -0.003(5) C43 0.047(6) 0.031(5) 0.011(5) -0.002(4) 0.013(4) 0.001(5) C44 0.070(8) 0.048(7) 0.036(6) 0.018(5) 0.021(5) 0.019(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ba1 O12 2.694(5) 1_565 ? Ba1 O41 2.695(5) . ? Ba1 O22 2.715(6) 1_565 ? Ba1 O31 2.718(5) . ? Ba1 O1 2.736(6) . ? Ba1 O11 2.767(5) . ? Ba1 O2 2.910(6) . ? Ba1 O13 3.020(5) . ? Ba1 P1 3.556(2) . ? Ba1 Ba2 4.5062(7) . ? Ba2 O21 2.678(5) . ? Ba2 O42 2.698(5) 1_545 ? Ba2 O11 2.707(5) . ? Ba2 O32 2.716(5) 1_545 ? Ba2 O4 2.765(6) . ? Ba2 O41 2.809(5) . ? Ba2 O3 2.861(5) . ? Ba2 O43 2.886(5) . ? Ba2 P4 3.529(2) . ? Cl1 C1 1.804(8) . ? Cl2 C1 1.782(8) . ? Cl3 C2 1.817(8) . ? Cl4 C2 1.779(8) . ? P1 O12 1.478(6) . ? P1 O11 1.499(6) . ? P1 O13 1.590(6) . ? P1 C1 1.847(9) . ? P2 O21 1.478(6) . ? P2 O22 1.492(6) . ? P2 O23 1.577(6) . ? P2 C1 1.870(9) . ? P3 O31 1.480(6) . ? P3 O32 1.493(6) . ? P3 O33 1.583(6) . ? P3 C2 1.853(9) . ? P4 O41 1.493(6) . ? P4 O42 1.496(6) . ? P4 O43 1.593(6) . ? P4 C2 1.853(9) . ? O12 Ba1 2.694(5) 1_545 ? O13 C13 1.451(9) . ? O22 Ba1 2.715(6) 1_545 ? O23 C23 1.449(10) . ? O32 Ba2 2.716(5) 1_565 ? O33 C33 1.452(9) . ? O42 Ba2 2.698(5) 1_565 ? O43 C43 1.447(9) . ? C13 C14 1.514(13) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C23 C24 1.513(12) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C33 C34 1.485(12) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C43 C44 1.499(13) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? 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 _geom_angle_publ_flag O12 Ba1 O41 117.88(17) 1_565 . ? O12 Ba1 O22 74.91(16) 1_565 1_565 ? O41 Ba1 O22 72.80(16) . 1_565 ? O12 Ba1 O31 84.63(17) 1_565 . ? O41 Ba1 O31 67.31(16) . . ? O22 Ba1 O31 118.56(16) 1_565 . ? O12 Ba1 O1 70.00(17) 1_565 . ? O41 Ba1 O1 150.76(17) . . ? O22 Ba1 O1 134.28(16) 1_565 . ? O31 Ba1 O1 86.57(17) . . ? O12 Ba1 O11 153.73(16) 1_565 . ? O41 Ba1 O11 70.03(16) . . ? O22 Ba1 O11 84.82(16) 1_565 . ? O31 Ba1 O11 120.23(16) . . ? O1 Ba1 O11 116.44(17) . . ? O12 Ba1 O2 136.62(17) 1_565 . ? O41 Ba1 O2 73.95(16) . . ? O22 Ba1 O2 142.97(16) 1_565 . ? O31 Ba1 O2 60.60(16) . . ? O1 Ba1 O2 82.02(16) . . ? O11 Ba1 O2 68.79(16) . . ? O12 Ba1 O13 114.06(16) 1_565 . ? O41 Ba1 O13 118.99(15) . . ? O22 Ba1 O13 92.61(16) 1_565 . ? O31 Ba1 O13 147.57(16) . . ? O1 Ba1 O13 76.41(16) . . ? O11 Ba1 O13 49.48(15) . . ? O2 Ba1 O13 89.48(15) . . ? O12 Ba1 P1 138.84(12) 1_565 . ? O41 Ba1 P1 93.48(12) . . ? O22 Ba1 P1 91.47(12) 1_565 . ? O31 Ba1 P1 134.46(12) . . ? O1 Ba1 P1 96.04(13) . . ? O11 Ba1 P1 23.45(11) . . ? O2 Ba1 P1 74.72(12) . . ? O13 Ba1 P1 26.41(10) . . ? O12 Ba1 Ba2 147.83(12) 1_565 . ? O41 Ba1 Ba2 35.89(11) . . ? O22 Ba1 Ba2 77.67(11) 1_565 . ? O31 Ba1 Ba2 94.06(11) . . ? O1 Ba1 Ba2 142.12(12) . . ? O11 Ba1 Ba2 34.17(11) . . ? O2 Ba1 Ba2 65.84(11) . . ? O13 Ba1 Ba2 83.50(10) . . ? P1 Ba1 Ba2 57.62(4) . . ? O21 Ba2 O42 83.09(17) . 1_545 ? O21 Ba2 O11 68.38(16) . . ? O42 Ba2 O11 121.32(16) 1_545 . ? O21 Ba2 O32 118.34(17) . 1_545 ? O42 Ba2 O32 73.76(16) 1_545 1_545 ? O11 Ba2 O32 76.71(16) . 1_545 ? O21 Ba2 O4 85.59(17) . . ? O42 Ba2 O4 77.03(16) 1_545 . ? O11 Ba2 O4 144.18(17) . . ? O32 Ba2 O4 138.88(17) 1_545 . ? O21 Ba2 O41 121.20(16) . . ? O42 Ba2 O41 155.15(16) 1_545 . ? O11 Ba2 O41 69.24(15) . . ? O32 Ba2 O41 88.56(16) 1_545 . ? O4 Ba2 O41 107.81(16) . . ? O21 Ba2 O3 63.53(17) . . ? O42 Ba2 O3 135.60(16) 1_545 . ? O11 Ba2 O3 74.18(16) . . ? O32 Ba2 O3 147.11(16) 1_545 . ? O4 Ba2 O3 72.26(16) . . ? O41 Ba2 O3 67.04(16) . . ? O21 Ba2 O43 146.71(17) . . ? O42 Ba2 O43 112.81(15) 1_545 . ? O11 Ba2 O43 119.14(15) . . ? O32 Ba2 O43 94.60(16) 1_545 . ? O4 Ba2 O43 70.90(16) . . ? O41 Ba2 O43 50.20(15) . . ? O3 Ba2 O43 86.48(15) . . ? O21 Ba2 P4 135.85(14) . . ? O42 Ba2 P4 137.78(12) 1_545 . ? O11 Ba2 P4 93.21(12) . . ? O32 Ba2 P4 93.80(12) 1_545 . ? O4 Ba2 P4 88.76(13) . . ? O41 Ba2 P4 23.97(11) . . ? O3 Ba2 P4 73.04(12) . . ? O43 Ba2 P4 26.41(11) . . ? O21 Ba2 Ba1 96.24(12) . . ? O42 Ba2 Ba1 149.55(11) 1_545 . ? O11 Ba2 Ba1 35.04(11) . . ? O32 Ba2 Ba1 80.04(11) 1_545 . ? O4 Ba2 Ba1 133.38(12) . . ? O41 Ba2 Ba1 34.23(11) . . ? O3 Ba2 Ba1 67.35(11) . . ? O43 Ba2 Ba1 84.15(10) . . ? P4 Ba2 Ba1 58.18(4) . . ? O12 P1 O11 119.7(3) . . ? O12 P1 O13 111.7(3) . . ? O11 P1 O13 103.9(3) . . ? O12 P1 C1 108.2(4) . . ? O11 P1 C1 106.5(3) . . ? O13 P1 C1 106.0(3) . . ? O12 P1 Ba1 126.1(2) . . ? O11 P1 Ba1 47.3(2) . . ? O13 P1 Ba1 57.6(2) . . ? C1 P1 Ba1 125.7(3) . . ? O21 P2 O22 119.7(3) . . ? O21 P2 O23 107.3(3) . . ? O22 P2 O23 112.3(3) . . ? O21 P2 C1 106.0(4) . . ? O22 P2 C1 106.2(3) . . ? O23 P2 C1 104.0(4) . . ? O31 P3 O32 119.5(3) . . ? O31 P3 O33 107.7(3) . . ? O32 P3 O33 111.9(3) . . ? O31 P3 C2 106.6(3) . . ? O32 P3 C2 106.9(4) . . ? O33 P3 C2 102.9(4) . . ? O41 P4 O42 120.0(3) . . ? O41 P4 O43 103.1(3) . . ? O42 P4 O43 112.7(3) . . ? O41 P4 C2 106.1(4) . . ? O42 P4 C2 107.7(3) . . ? O43 P4 C2 106.3(3) . . ? O41 P4 Ba2 49.9(2) . . ? O42 P4 Ba2 129.6(2) . . ? O43 P4 Ba2 53.68(19) . . ? C2 P4 Ba2 122.6(3) . . ? P1 O11 Ba2 139.9(3) . . ? P1 O11 Ba1 109.3(3) . . ? Ba2 O11 Ba1 110.79(18) . . ? P1 O12 Ba1 134.5(3) . 1_545 ? C13 O13 P1 124.5(5) . . ? C13 O13 Ba1 132.1(5) . . ? P1 O13 Ba1 96.0(2) . . ? P2 O21 Ba2 136.1(3) . . ? P2 O22 Ba1 139.4(3) . 1_545 ? C23 O23 P2 124.4(5) . . ? P3 O31 Ba1 134.5(3) . . ? P3 O32 Ba2 140.7(3) . 1_565 ? C33 O33 P3 123.1(5) . . ? P4 O41 Ba1 143.8(3) . . ? P4 O41 Ba2 106.2(3) . . ? Ba1 O41 Ba2 109.88(18) . . ? P4 O42 Ba2 132.8(3) . 1_565 ? C43 O43 P4 125.7(5) . . ? C43 O43 Ba2 131.4(5) . . ? P4 O43 Ba2 99.9(2) . . ? Cl2 C1 Cl1 108.6(4) . . ? Cl2 C1 P1 108.6(4) . . ? Cl1 C1 P1 110.0(4) . . ? Cl2 C1 P2 107.7(4) . . ? Cl1 C1 P2 108.3(4) . . ? P1 C1 P2 113.5(4) . . ? Cl4 C2 Cl3 107.9(4) . . ? Cl4 C2 P3 109.3(4) . . ? Cl3 C2 P3 109.4(4) . . ? Cl4 C2 P4 108.8(4) . . ? Cl3 C2 P4 109.1(4) . . ? P3 C2 P4 112.3(4) . . ? O13 C13 C14 109.6(8) . . ? O13 C13 H13A 109.7 . . ? C14 C13 H13A 109.7 . . ? O13 C13 H13B 109.7 . . ? C14 C13 H13B 109.7 . . ? H13A C13 H13B 108.2 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O23 C23 C24 110.1(7) . . ? O23 C23 H23A 109.6 . . ? C24 C23 H23A 109.6 . . ? O23 C23 H23B 109.6 . . ? C24 C23 H23B 109.6 . . ? H23A C23 H23B 108.2 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O33 C33 C34 107.7(7) . . ? O33 C33 H33A 110.2 . . ? C34 C33 H33A 110.2 . . ? O33 C33 H33B 110.2 . . ? C34 C33 H33B 110.2 . . ? H33A C33 H33B 108.5 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O43 C43 C44 108.4(7) . . ? O43 C43 H43A 110.0 . . ? C44 C43 H43A 110.0 . . ? O43 C43 H43B 110.0 . . ? C44 C43 H43B 110.0 . . ? H43A C43 H43B 108.4 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O12 Ba1 Ba2 O21 -94.3(3) 1_565 . . . ? O41 Ba1 Ba2 O21 -140.0(2) . . . . ? O22 Ba1 Ba2 O21 -62.34(17) 1_565 . . . ? O31 Ba1 Ba2 O21 179.30(17) . . . . ? O1 Ba1 Ba2 O21 89.7(2) . . . . ? O11 Ba1 Ba2 O21 36.7(2) . . . . ? O2 Ba1 Ba2 O21 124.13(18) . . . . ? O13 Ba1 Ba2 O21 31.78(16) . . . . ? P1 Ba1 Ba2 O21 37.43(13) . . . . ? O12 Ba1 Ba2 O42 178.7(3) 1_565 . . 1_545 ? O41 Ba1 Ba2 O42 133.1(3) . . . 1_545 ? O22 Ba1 Ba2 O42 -149.3(3) 1_565 . . 1_545 ? O31 Ba1 Ba2 O42 92.3(3) . . . 1_545 ? O1 Ba1 Ba2 O42 2.7(3) . . . 1_545 ? O11 Ba1 Ba2 O42 -50.3(3) . . . 1_545 ? O2 Ba1 Ba2 O42 37.2(3) . . . 1_545 ? O13 Ba1 Ba2 O42 -55.2(2) . . . 1_545 ? P1 Ba1 Ba2 O42 -49.5(2) . . . 1_545 ? O12 Ba1 Ba2 O11 -131.1(3) 1_565 . . . ? O41 Ba1 Ba2 O11 -176.7(3) . . . . ? O22 Ba1 Ba2 O11 -99.1(2) 1_565 . . . ? O31 Ba1 Ba2 O11 142.6(2) . . . . ? O1 Ba1 Ba2 O11 52.9(3) . . . . ? O2 Ba1 Ba2 O11 87.4(2) . . . . ? O13 Ba1 Ba2 O11 -4.9(2) . . . . ? P1 Ba1 Ba2 O11 0.7(2) . . . . ? O12 Ba1 Ba2 O32 147.9(2) 1_565 . . 1_545 ? O41 Ba1 Ba2 O32 102.3(2) . . . 1_545 ? O22 Ba1 Ba2 O32 179.91(16) 1_565 . . 1_545 ? O31 Ba1 Ba2 O32 61.55(16) . . . 1_545 ? O1 Ba1 Ba2 O32 -28.1(2) . . . 1_545 ? O11 Ba1 Ba2 O32 -81.0(2) . . . 1_545 ? O2 Ba1 Ba2 O32 6.38(17) . . . 1_545 ? O13 Ba1 Ba2 O32 -85.97(16) . . . 1_545 ? P1 Ba1 Ba2 O32 -80.32(12) . . . 1_545 ? O12 Ba1 Ba2 O4 -4.5(3) 1_565 . . . ? O41 Ba1 Ba2 O4 -50.1(3) . . . . ? O22 Ba1 Ba2 O4 27.5(2) 1_565 . . . ? O31 Ba1 Ba2 O4 -90.9(2) . . . . ? O1 Ba1 Ba2 O4 179.5(3) . . . . ? O11 Ba1 Ba2 O4 126.6(3) . . . . ? O2 Ba1 Ba2 O4 -146.0(2) . . . . ? O13 Ba1 Ba2 O4 121.6(2) . . . . ? P1 Ba1 Ba2 O4 127.27(17) . . . . ? O12 Ba1 Ba2 O41 45.6(3) 1_565 . . . ? O22 Ba1 Ba2 O41 77.6(2) 1_565 . . . ? O31 Ba1 Ba2 O41 -40.7(2) . . . . ? O1 Ba1 Ba2 O41 -130.4(3) . . . . ? O11 Ba1 Ba2 O41 176.7(3) . . . . ? O2 Ba1 Ba2 O41 -95.9(2) . . . . ? O13 Ba1 Ba2 O41 171.7(2) . . . . ? P1 Ba1 Ba2 O41 177.4(2) . . . . ? O12 Ba1 Ba2 O3 -36.4(3) 1_565 . . . ? O41 Ba1 Ba2 O3 -82.1(2) . . . . ? O22 Ba1 Ba2 O3 -4.44(17) 1_565 . . . ? O31 Ba1 Ba2 O3 -122.81(17) . . . . ? O1 Ba1 Ba2 O3 147.6(2) . . . . ? O11 Ba1 Ba2 O3 94.6(2) . . . . ? O2 Ba1 Ba2 O3 -177.97(17) . . . . ? O13 Ba1 Ba2 O3 89.68(16) . . . . ? P1 Ba1 Ba2 O3 95.33(13) . . . . ? O12 Ba1 Ba2 O43 52.2(2) 1_565 . . . ? O41 Ba1 Ba2 O43 6.6(2) . . . . ? O22 Ba1 Ba2 O43 84.18(16) 1_565 . . . ? O31 Ba1 Ba2 O43 -34.19(16) . . . . ? O1 Ba1 Ba2 O43 -123.8(2) . . . . ? O11 Ba1 Ba2 O43 -176.8(2) . . . . ? O2 Ba1 Ba2 O43 -89.35(16) . . . . ? O13 Ba1 Ba2 O43 178.30(15) . . . . ? P1 Ba1 Ba2 O43 -176.05(12) . . . . ? O12 Ba1 Ba2 P4 47.1(2) 1_565 . . . ? O41 Ba1 Ba2 P4 1.4(2) . . . . ? O22 Ba1 Ba2 P4 79.07(13) 1_565 . . . ? O31 Ba1 Ba2 P4 -39.30(12) . . . . ? O1 Ba1 Ba2 P4 -128.9(2) . . . . ? O11 Ba1 Ba2 P4 178.1(2) . . . . ? O2 Ba1 Ba2 P4 -94.46(13) . . . . ? O13 Ba1 Ba2 P4 173.19(11) . . . . ? P1 Ba1 Ba2 P4 178.84(6) . . . . ? O12 Ba1 P1 O12 -118.9(4) 1_565 . . . ? O41 Ba1 P1 O12 99.7(3) . . . . ? O22 Ba1 P1 O12 172.6(3) 1_565 . . . ? O31 Ba1 P1 O12 38.5(3) . . . . ? O1 Ba1 P1 O12 -52.6(3) . . . . ? O11 Ba1 P1 O12 99.2(4) . . . . ? O2 Ba1 P1 O12 27.4(3) . . . . ? O13 Ba1 P1 O12 -94.5(4) . . . . ? Ba2 Ba1 P1 O12 98.2(3) . . . . ? O12 Ba1 P1 O11 141.9(3) 1_565 . . . ? O41 Ba1 P1 O11 0.5(3) . . . . ? O22 Ba1 P1 O11 73.4(3) 1_565 . . . ? O31 Ba1 P1 O11 -60.7(3) . . . . ? O1 Ba1 P1 O11 -151.8(3) . . . . ? O2 Ba1 P1 O11 -71.8(3) . . . . ? O13 Ba1 P1 O11 166.3(4) . . . . ? Ba2 Ba1 P1 O11 -1.0(3) . . . . ? O12 Ba1 P1 O13 -24.4(3) 1_565 . . . ? O41 Ba1 P1 O13 -165.8(3) . . . . ? O22 Ba1 P1 O13 -92.9(3) 1_565 . . . ? O31 Ba1 P1 O13 133.0(3) . . . . ? O1 Ba1 P1 O13 41.9(3) . . . . ? O11 Ba1 P1 O13 -166.3(4) . . . . ? O2 Ba1 P1 O13 121.9(3) . . . . ? Ba2 Ba1 P1 O13 -167.3(3) . . . . ? O12 Ba1 P1 C1 62.6(4) 1_565 . . . ? O41 Ba1 P1 C1 -78.8(4) . . . . ? O22 Ba1 P1 C1 -5.9(3) 1_565 . . . ? O31 Ba1 P1 C1 -140.0(4) . . . . ? O1 Ba1 P1 C1 128.9(3) . . . . ? O11 Ba1 P1 C1 -79.3(4) . . . . ? O2 Ba1 P1 C1 -151.1(4) . . . . ? O13 Ba1 P1 C1 87.0(4) . . . . ? Ba2 Ba1 P1 C1 -80.3(3) . . . . ? O21 Ba2 P4 O41 60.9(3) . . . . ? O42 Ba2 P4 O41 -147.7(3) 1_545 . . . ? O11 Ba2 P4 O41 -0.9(3) . . . . ? O32 Ba2 P4 O41 -77.8(3) 1_545 . . . ? O4 Ba2 P4 O41 143.3(3) . . . . ? O3 Ba2 P4 O41 71.5(3) . . . . ? O43 Ba2 P4 O41 -170.5(4) . . . . ? Ba1 Ba2 P4 O41 -2.0(3) . . . . ? O21 Ba2 P4 O42 -37.8(4) . . . . ? O42 Ba2 P4 O42 113.6(4) 1_545 . . . ? O11 Ba2 P4 O42 -99.6(3) . . . . ? O32 Ba2 P4 O42 -176.5(3) 1_545 . . . ? O4 Ba2 P4 O42 44.6(3) . . . . ? O41 Ba2 P4 O42 -98.7(4) . . . . ? O3 Ba2 P4 O42 -27.2(3) . . . . ? O43 Ba2 P4 O42 90.8(4) . . . . ? Ba1 Ba2 P4 O42 -100.7(3) . . . . ? O21 Ba2 P4 O43 -128.6(3) . . . . ? O42 Ba2 P4 O43 22.8(3) 1_545 . . . ? O11 Ba2 P4 O43 169.6(3) . . . . ? O32 Ba2 P4 O43 92.7(3) 1_545 . . . ? O4 Ba2 P4 O43 -46.2(3) . . . . ? O41 Ba2 P4 O43 170.5(4) . . . . ? O3 Ba2 P4 O43 -118.0(3) . . . . ? Ba1 Ba2 P4 O43 168.5(3) . . . . ? O21 Ba2 P4 C2 144.7(3) . . . . ? O42 Ba2 P4 C2 -63.9(4) 1_545 . . . ? O11 Ba2 P4 C2 82.9(3) . . . . ? O32 Ba2 P4 C2 6.0(3) 1_545 . . . ? O4 Ba2 P4 C2 -132.9(3) . . . . ? O41 Ba2 P4 C2 83.8(4) . . . . ? O3 Ba2 P4 C2 155.2(3) . . . . ? O43 Ba2 P4 C2 -86.7(4) . . . . ? Ba1 Ba2 P4 C2 81.8(3) . . . . ? O12 P1 O11 Ba2 64.4(6) . . . . ? O13 P1 O11 Ba2 -170.3(4) . . . . ? C1 P1 O11 Ba2 -58.6(6) . . . . ? Ba1 P1 O11 Ba2 177.8(6) . . . . ? O12 P1 O11 Ba1 -113.4(3) . . . . ? O13 P1 O11 Ba1 11.9(4) . . . . ? C1 P1 O11 Ba1 123.6(3) . . . . ? O21 Ba2 O11 P1 42.0(5) . . . . ? O42 Ba2 O11 P1 -24.9(6) 1_545 . . . ? O32 Ba2 O11 P1 -86.2(5) 1_545 . . . ? O4 Ba2 O11 P1 88.3(6) . . . . ? O41 Ba2 O11 P1 -179.8(5) . . . . ? O3 Ba2 O11 P1 109.3(5) . . . . ? O43 Ba2 O11 P1 -174.1(4) . . . . ? P4 Ba2 O11 P1 -179.4(5) . . . . ? Ba1 Ba2 O11 P1 -177.8(6) . . . . ? O21 Ba2 O11 Ba1 -140.3(2) . . . . ? O42 Ba2 O11 Ba1 152.86(17) 1_545 . . . ? O32 Ba2 O11 Ba1 91.6(2) 1_545 . . . ? O4 Ba2 O11 Ba1 -93.9(3) . . . . ? O41 Ba2 O11 Ba1 -1.99(17) . . . . ? O3 Ba2 O11 Ba1 -73.0(2) . . . . ? O43 Ba2 O11 Ba1 3.7(3) . . . . ? P4 Ba2 O11 Ba1 -1.59(18) . . . . ? O12 Ba1 O11 P1 -66.6(5) 1_565 . . . ? O41 Ba1 O11 P1 -179.4(3) . . . . ? O22 Ba1 O11 P1 -105.9(3) 1_565 . . . ? O31 Ba1 O11 P1 133.9(3) . . . . ? O1 Ba1 O11 P1 31.7(4) . . . . ? O2 Ba1 O11 P1 100.6(3) . . . . ? O13 Ba1 O11 P1 -8.0(2) . . . . ? Ba2 Ba1 O11 P1 178.5(4) . . . . ? O12 Ba1 O11 Ba2 114.9(3) 1_565 . . . ? O41 Ba1 O11 Ba2 2.07(18) . . . . ? O22 Ba1 O11 Ba2 75.6(2) 1_565 . . . ? O31 Ba1 O11 Ba2 -44.6(3) . . . . ? O1 Ba1 O11 Ba2 -146.82(19) . . . . ? O2 Ba1 O11 Ba2 -77.9(2) . . . . ? O13 Ba1 O11 Ba2 173.5(3) . . . . ? P1 Ba1 O11 Ba2 -178.5(4) . . . . ? O11 P1 O12 Ba1 -69.6(5) . . . 1_545 ? O13 P1 O12 Ba1 168.9(4) . . . 1_545 ? C1 P1 O12 Ba1 52.6(5) . . . 1_545 ? Ba1 P1 O12 Ba1 -126.1(3) . . . 1_545 ? O12 P1 O13 C13 -32.9(7) . . . . ? O11 P1 O13 C13 -163.2(6) . . . . ? C1 P1 O13 C13 84.7(7) . . . . ? Ba1 P1 O13 C13 -152.8(7) . . . . ? O12 P1 O13 Ba1 119.9(3) . . . . ? O11 P1 O13 Ba1 -10.3(3) . . . . ? C1 P1 O13 Ba1 -122.4(3) . . . . ? O12 Ba1 O13 C13 -47.8(7) 1_565 . . . ? O41 Ba1 O13 C13 165.8(6) . . . . ? O22 Ba1 O13 C13 -122.5(7) 1_565 . . . ? O31 Ba1 O13 C13 72.9(7) . . . . ? O1 Ba1 O13 C13 12.6(7) . . . . ? O11 Ba1 O13 C13 156.6(7) . . . . ? O2 Ba1 O13 C13 94.5(7) . . . . ? P1 Ba1 O13 C13 149.5(8) . . . . ? Ba2 Ba1 O13 C13 160.3(7) . . . . ? O12 Ba1 O13 P1 162.7(2) 1_565 . . . ? O41 Ba1 O13 P1 16.3(3) . . . . ? O22 Ba1 O13 P1 88.1(3) 1_565 . . . ? O31 Ba1 O13 P1 -76.6(4) . . . . ? O1 Ba1 O13 P1 -136.9(3) . . . . ? O11 Ba1 O13 P1 7.1(2) . . . . ? O2 Ba1 O13 P1 -55.0(3) . . . . ? Ba2 Ba1 O13 P1 10.8(2) . . . . ? O22 P2 O21 Ba2 -50.4(6) . . . . ? O23 P2 O21 Ba2 -179.8(4) . . . . ? C1 P2 O21 Ba2 69.5(5) . . . . ? O42 Ba2 O21 P2 80.1(5) 1_545 . . . ? O11 Ba2 O21 P2 -47.6(5) . . . . ? O32 Ba2 O21 P2 12.7(6) 1_545 . . . ? O4 Ba2 O21 P2 157.5(5) . . . . ? O41 Ba2 O21 P2 -94.3(5) . . . . ? O3 Ba2 O21 P2 -130.1(5) . . . . ? O43 Ba2 O21 P2 -158.1(4) . . . . ? P4 Ba2 O21 P2 -118.8(4) . . . . ? Ba1 Ba2 O21 P2 -69.3(5) . . . . ? O21 P2 O22 Ba1 78.0(6) . . . 1_545 ? O23 P2 O22 Ba1 -154.8(4) . . . 1_545 ? C1 P2 O22 Ba1 -41.7(6) . . . 1_545 ? O21 P2 O23 C23 156.8(6) . . . . ? O22 P2 O23 C23 23.2(7) . . . . ? C1 P2 O23 C23 -91.2(7) . . . . ? O32 P3 O31 Ba1 49.9(6) . . . . ? O33 P3 O31 Ba1 178.9(4) . . . . ? C2 P3 O31 Ba1 -71.2(5) . . . . ? O12 Ba1 O31 P3 -77.3(4) 1_565 . . . ? O41 Ba1 O31 P3 46.0(4) . . . . ? O22 Ba1 O31 P3 -7.7(5) 1_565 . . . ? O1 Ba1 O31 P3 -147.5(4) . . . . ? O11 Ba1 O31 P3 93.7(4) . . . . ? O2 Ba1 O31 P3 129.7(5) . . . . ? O13 Ba1 O31 P3 154.7(3) . . . . ? P1 Ba1 O31 P3 117.4(4) . . . . ? Ba2 Ba1 O31 P3 70.5(4) . . . . ? O31 P3 O32 Ba2 -79.4(6) . . . 1_565 ? O33 P3 O32 Ba2 153.5(4) . . . 1_565 ? C2 P3 O32 Ba2 41.6(6) . . . 1_565 ? O31 P3 O33 C33 -153.0(6) . . . . ? O32 P3 O33 C33 -19.8(7) . . . . ? C2 P3 O33 C33 94.6(7) . . . . ? O42 P4 O41 Ba1 -66.4(6) . . . . ? O43 P4 O41 Ba1 167.3(5) . . . . ? C2 P4 O41 Ba1 55.8(6) . . . . ? Ba2 P4 O41 Ba1 175.2(7) . . . . ? O42 P4 O41 Ba2 118.5(3) . . . . ? O43 P4 O41 Ba2 -7.8(3) . . . . ? C2 P4 O41 Ba2 -119.4(3) . . . . ? O12 Ba1 O41 P4 30.4(6) 1_565 . . . ? O22 Ba1 O41 P4 92.3(6) 1_565 . . . ? O31 Ba1 O41 P4 -40.0(5) . . . . ? O1 Ba1 O41 P4 -68.4(7) . . . . ? O11 Ba1 O41 P4 -177.1(6) . . . . ? O2 Ba1 O41 P4 -104.3(6) . . . . ? O13 Ba1 O41 P4 175.5(5) . . . . ? P1 Ba1 O41 P4 -177.3(5) . . . . ? Ba2 Ba1 O41 P4 -175.1(7) . . . . ? O12 Ba1 O41 Ba2 -154.50(18) 1_565 . . . ? O22 Ba1 O41 Ba2 -92.7(2) 1_565 . . . ? O31 Ba1 O41 Ba2 135.1(2) . . . . ? O1 Ba1 O41 Ba2 106.7(3) . . . . ? O11 Ba1 O41 Ba2 -1.98(17) . . . . ? O2 Ba1 O41 Ba2 70.8(2) . . . . ? O13 Ba1 O41 Ba2 -9.4(3) . . . . ? P1 Ba1 O41 Ba2 -2.20(17) . . . . ? O21 Ba2 O41 P4 -134.6(3) . . . . ? O42 Ba2 O41 P4 58.7(5) 1_545 . . . ? O11 Ba2 O41 P4 179.0(3) . . . . ? O32 Ba2 O41 P4 102.7(3) 1_545 . . . ? O4 Ba2 O41 P4 -38.9(3) . . . . ? O3 Ba2 O41 P4 -100.0(3) . . . . ? O43 Ba2 O41 P4 5.5(2) . . . . ? Ba1 Ba2 O41 P4 177.0(4) . . . . ? O21 Ba2 O41 Ba1 48.4(3) . . . . ? O42 Ba2 O41 Ba1 -118.2(3) 1_545 . . . ? O11 Ba2 O41 Ba1 2.04(17) . . . . ? O32 Ba2 O41 Ba1 -74.3(2) 1_545 . . . ? O4 Ba2 O41 Ba1 144.13(19) . . . . ? O3 Ba2 O41 Ba1 83.1(2) . . . . ? O43 Ba2 O41 Ba1 -171.5(3) . . . . ? P4 Ba2 O41 Ba1 -177.0(4) . . . . ? O41 P4 O42 Ba2 62.1(5) . . . 1_565 ? O43 P4 O42 Ba2 -176.2(3) . . . 1_565 ? C2 P4 O42 Ba2 -59.3(5) . . . 1_565 ? Ba2 P4 O42 Ba2 122.9(3) . . . 1_565 ? O41 P4 O43 C43 169.8(6) . . . . ? O42 P4 O43 C43 39.0(7) . . . . ? C2 P4 O43 C43 -78.8(7) . . . . ? Ba2 P4 O43 C43 162.4(7) . . . . ? O41 P4 O43 Ba2 7.4(3) . . . . ? O42 P4 O43 Ba2 -123.4(3) . . . . ? C2 P4 O43 Ba2 118.9(3) . . . . ? O21 Ba2 O43 C43 -78.2(7) . . . . ? O42 Ba2 O43 C43 35.6(7) 1_545 . . . ? O11 Ba2 O43 C43 -172.8(6) . . . . ? O32 Ba2 O43 C43 109.9(6) 1_545 . . . ? O4 Ba2 O43 C43 -30.6(6) . . . . ? O41 Ba2 O43 C43 -165.9(7) . . . . ? O3 Ba2 O43 C43 -103.1(6) . . . . ? P4 Ba2 O43 C43 -160.9(8) . . . . ? Ba1 Ba2 O43 C43 -170.7(6) . . . . ? O21 Ba2 O43 P4 82.7(4) . . . . ? O42 Ba2 O43 P4 -163.6(2) 1_545 . . . ? O11 Ba2 O43 P4 -11.9(3) . . . . ? O32 Ba2 O43 P4 -89.3(3) 1_545 . . . ? O4 Ba2 O43 P4 130.2(3) . . . . ? O41 Ba2 O43 P4 -5.0(2) . . . . ? O3 Ba2 O43 P4 57.8(3) . . . . ? Ba1 Ba2 O43 P4 -9.8(2) . . . . ? O12 P1 C1 Cl2 167.5(4) . . . . ? O11 P1 C1 Cl2 -62.6(5) . . . . ? O13 P1 C1 Cl2 47.6(5) . . . . ? Ba1 P1 C1 Cl2 -13.8(6) . . . . ? O12 P1 C1 Cl1 48.8(5) . . . . ? O11 P1 C1 Cl1 178.6(4) . . . . ? O13 P1 C1 Cl1 -71.1(5) . . . . ? Ba1 P1 C1 Cl1 -132.5(3) . . . . ? O12 P1 C1 P2 -72.7(5) . . . . ? O11 P1 C1 P2 57.2(5) . . . . ? O13 P1 C1 P2 167.4(4) . . . . ? Ba1 P1 C1 P2 106.0(4) . . . . ? O21 P2 C1 Cl2 57.4(5) . . . . ? O22 P2 C1 Cl2 -174.3(4) . . . . ? O23 P2 C1 Cl2 -55.6(5) . . . . ? O21 P2 C1 Cl1 174.6(4) . . . . ? O22 P2 C1 Cl1 -57.1(5) . . . . ? O23 P2 C1 Cl1 61.6(5) . . . . ? O21 P2 C1 P1 -62.9(5) . . . . ? O22 P2 C1 P1 65.4(5) . . . . ? O23 P2 C1 P1 -175.9(4) . . . . ? O31 P3 C2 Cl4 -55.2(5) . . . . ? O32 P3 C2 Cl4 175.9(4) . . . . ? O33 P3 C2 Cl4 57.9(5) . . . . ? O31 P3 C2 Cl3 -173.1(4) . . . . ? O32 P3 C2 Cl3 58.0(5) . . . . ? O33 P3 C2 Cl3 -60.0(5) . . . . ? O31 P3 C2 P4 65.6(5) . . . . ? O32 P3 C2 P4 -63.3(5) . . . . ? O33 P3 C2 P4 178.8(4) . . . . ? O41 P4 C2 Cl4 65.8(5) . . . . ? O42 P4 C2 Cl4 -164.6(4) . . . . ? O43 P4 C2 Cl4 -43.5(5) . . . . ? Ba2 P4 C2 Cl4 13.4(5) . . . . ? O41 P4 C2 Cl3 -176.8(4) . . . . ? O42 P4 C2 Cl3 -47.1(5) . . . . ? O43 P4 C2 Cl3 73.9(4) . . . . ? Ba2 P4 C2 Cl3 130.9(3) . . . . ? O41 P4 C2 P3 -55.4(5) . . . . ? O42 P4 C2 P3 74.3(5) . . . . ? O43 P4 C2 P3 -164.6(4) . . . . ? Ba2 P4 C2 P3 -107.7(4) . . . . ? P1 O13 C13 C14 -119.7(7) . . . . ? Ba1 O13 C13 C14 98.0(8) . . . . ? P2 O23 C23 C24 -119.1(7) . . . . ? P3 O33 C33 C34 -152.0(6) . . . . ? P4 O43 C43 C44 133.8(7) . . . . ? Ba2 O43 C43 C44 -69.6(9) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 2.031 _refine_diff_density_min -1.028 _refine_diff_density_rms 0.196 #===END