Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Jonna Jokiniemi' _publ_contact_author_address ;Department of Chemistry University of Joensuu P.O.Box 111 FI-80101 Joensuu Finland ; _publ_contact_author_email jonna.jokiniemi@joensuu.fi _publ_contact_author_phone +358132513386 _publ_contact_author_fax +358132513390 _publ_section_title ; Structural study of metal complexes of bisphosphonate amide ester: copper, magnesium, zinc and cadmium complexes of (dichloromethylene)bisphosphonic acid P-piperidinium-P'-methyl ester ; loop_ _publ_author_name _publ_author_address J.Jokiniemi ;Department of Chemistry University of Joensuu P.O.Box 111 FI-80101 Joensuu Finland ; E.Vuokila-Laine ;Department of Chemistry University of Joensuu P.O.Box 111 FI-80101 Joensuu Finland ; S.Peraniemi ;Department of Chemistry University of Kuopio P.O.Box 1627 FI-70211 Kuopio Finland ; J.Vepsalainen ;Department of Chemistry University of Kuopio P.O.Box 1627 FI-70211 Kuopio Finland ; ; M.Ahlgren ; ;Department of Chemistry University of Joensuu P.O.Box 111 FI-80101 Joensuu Finland ; _publ_section_abstract ; Four metal complexes of the (dichloromethylene)bisphosphonic acid P-piperidinium-P'-methyl ester: [{Cu~3~ (CH~3~PO~3~CCl~2~PO~2~NC~5~H~10~)~3~(H~2~O)~2~}(H~2~O)~3~]~2~ (1), [(MgCH~3~PO~3~CCl~2~PO~2~NC~5~H~10~)(H~2~O)~3~]~n~ (2), {Na~2~Zn~3~(CH~3~PO~3~CCl~2~PO~2~NC~5~H~10~)~4~(H~2~O)~4~}(H~2~O)~2~]~n~ (3) and [{Cd~2~(CH~3~PO~3~CCl~2~PO~2~NC~5~H~10~)~2~(H~2~O)~6~}(H~2~O)~2~]~n~ (4) have been prepared and their crystal structures determined by X-ray single-crystal diffraction. The methyl ester of piperidine derivative of Cl~2~MBP ligand forms the first wheel-like metal complex of bisphosphonate 1. The packing of hexameric compound consists of channels occupied by aqua ligands and lattice water molecules. Compounds 2-4 are polymers consisting of one-dimensional chains of different compositions, and in 3, coordinated Na^+^ cations hold the chains together, forming a layered structure. ; #===END======================================================================== data_Structure(1) _database_code_depnum_ccdc_archive 'CCDC 273737' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H86 Cl12 Cu6 N6 O34 P12, 6(H2 O)' _chemical_formula_sum 'C42 H98 Cl12 Cu6 N6 O40 P12' _chemical_formula_weight 2505.61 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' Cu Cu 0.3201 1.2651 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6150(1) _cell_length_b 16.1796(2) _cell_length_c 18.0133(2) _cell_angle_alpha 66.868(1) _cell_angle_beta 82.440(1) _cell_angle_gamma 81.925(1) _cell_volume 2278.01(5) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 17345 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 26.00 _exptl_crystal_description plate _exptl_crystal_colour 'light blue' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 1.801 _exptl_crystal_density_diffrn 1.826 _exptl_crystal_density_method flotation _exptl_crystal_F_000 1270 _exptl_absorpt_coefficient_mu 2.024 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7441 _exptl_absorpt_correction_T_max 0.8672 _exptl_absorpt_process_details 'XPREP in SHELXTL (Bruker, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 KappaCCD' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17345 _diffrn_reflns_av_R_equivalents 0.0202 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8961 _reflns_number_gt 7561 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius,1997-200)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL v.5.1 (Bruker, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^+7.0000P] 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 8961 _refine_ls_number_parameters 541 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.0970 _refine_ls_wR_factor_gt 0.0922 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.067 _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 Cu1 Cu 0.48679(5) 0.26251(3) 0.45047(3) 0.02089(11) Uani 1 1 d . . . Cu2 Cu 0.70971(5) 0.21326(3) 0.70710(3) 0.02380(12) Uani 1 1 d . . . Cu3 Cu 0.70222(5) 0.44065(3) 0.73762(3) 0.01742(10) Uani 1 1 d . . . Cl1 Cl 0.30185(12) 0.25157(7) 0.26090(6) 0.0323(2) Uani 1 1 d . . . Cl2 Cl 0.21783(11) 0.44442(7) 0.17535(6) 0.0293(2) Uani 1 1 d . . . Cl3 Cl 0.72020(19) 0.00554(10) 0.70787(9) 0.0743(5) Uani 1 1 d . . . Cl4 Cl 0.5986(2) 0.01482(12) 0.56217(13) 0.0832(6) Uani 1 1 d . . . Cl5 Cl 0.89875(12) 0.10637(7) 0.92621(7) 0.0351(2) Uani 1 1 d . . . Cl6 Cl 0.89606(12) 0.27550(7) 0.94723(6) 0.0333(2) Uani 1 1 d . . . P1 P 0.19088(10) 0.36664(6) 0.35594(6) 0.01843(19) Uani 1 1 d . . . P2 P 0.50759(10) 0.38373(6) 0.26546(5) 0.01639(18) Uani 1 1 d . . . P3 P 0.77841(12) 0.16219(6) 0.55379(6) 0.0223(2) Uani 1 1 d . . . P4 P 0.45643(12) 0.14330(7) 0.63925(6) 0.0252(2) Uani 1 1 d . . . P5 P 0.95561(10) 0.27461(7) 0.78167(6) 0.0214(2) Uani 1 1 d . . . P6 P 0.63381(10) 0.24974(6) 0.86713(6) 0.01792(19) Uani 1 1 d . . . O1 O 0.5115(2) 0.39802(13) 0.45549(11) 0.0315(6) Uani 1 1 d . . . H1A H 0.4484 0.4068 0.4919 0.047 Uiso 1 1 d R . . H1B H 0.4800 0.4382 0.4128 0.047 Uiso 1 1 d R . . O2 O 0.6333(2) 0.37640(13) 0.65256(11) 0.0231(5) Uani 1 1 d R . . H2A H 0.5417 0.3829 0.6368 0.035 Uiso 1 1 d R . . H2B H 0.6929 0.3851 0.6091 0.035 Uiso 1 1 d R . . O3 O 0.3277(3) 0.41621(19) 0.58611(18) 0.0334(7) Uani 1 1 d . . . H3A H 0.2680 0.4633 0.5621 0.050 Uiso 1 1 d R . . H3B H 0.2701 0.3732 0.5990 0.050 Uiso 1 1 d R . . O4 O 0.0999(3) 0.3126(2) 0.57444(18) 0.0360(7) Uani 1 1 d . . . H4A H 0.0560 0.2757 0.6176 0.054 Uiso 1 1 d R . . H4B H 0.1465 0.2802 0.5495 0.054 Uiso 1 1 d R . . O5 O 0.8129(6) 0.4098(3) 0.5085(3) 0.0296(10) Uani 0.60 1 d P . . H5A H 0.7520 0.3914 0.4860 0.044 Uiso 0.60 1 d PR . . H5B H 0.8986 0.3741 0.5140 0.044 Uiso 0.60 1 d PR . . O5' O 0.8583(8) 0.4451(6) 0.5308(5) 0.0345(17) Uani 0.40 1 d P . . H5A' H 0.8678 0.4783 0.5557 0.052 Uiso 0.40 1 d PR . . H5B' H 0.9403 0.4063 0.5394 0.052 Uiso 0.40 1 d PR . . O11 O 0.2648(3) 0.29094(17) 0.42466(15) 0.0220(5) Uani 1 1 d . . . O12 O 0.1958(3) 0.46091(17) 0.35096(15) 0.0217(5) Uani 1 1 d . . . O13 O 0.0190(3) 0.34542(18) 0.35649(17) 0.0271(6) Uani 1 1 d . . . O21 O 0.5694(3) 0.30578(16) 0.33669(14) 0.0188(5) Uani 1 1 d . . . O22 O 0.4890(3) 0.47640(16) 0.26840(15) 0.0210(5) Uani 1 1 d . . . O31 O 0.7023(3) 0.2217(2) 0.47930(17) 0.0439(9) Uani 1 1 d . . . O32 O 0.8185(3) 0.2039(2) 0.60816(19) 0.0373(7) Uani 1 1 d . . . O33 O 0.9291(4) 0.1079(2) 0.53197(19) 0.0421(8) Uani 1 1 d . . . O41 O 0.3953(3) 0.1959(2) 0.55809(16) 0.0392(8) Uani 1 1 d . . . O42 O 0.5094(3) 0.1932(2) 0.68366(19) 0.0367(7) Uani 1 1 d . . . O51 O 0.9175(3) 0.22459(19) 0.73291(17) 0.0273(6) Uani 1 1 d . . . O52 O 0.9102(3) 0.37426(17) 0.75130(16) 0.0236(6) Uani 1 1 d . . . O53 O 1.1346(3) 0.25232(19) 0.79464(18) 0.0322(7) Uani 1 1 d . . . O61 O 0.6119(3) 0.20098(17) 0.81401(16) 0.0232(5) Uani 1 1 d . . . O62 O 0.6055(3) 0.35108(16) 0.83452(15) 0.0200(5) Uani 1 1 d . . . N2 N 0.6132(4) 0.3855(2) 0.18339(18) 0.0245(7) Uani 1 1 d . . . N4 N 0.3274(5) 0.0765(3) 0.6961(2) 0.0431(10) Uani 1 1 d D . . N6 N 0.5275(4) 0.2082(2) 0.95236(18) 0.0218(6) Uani 1 1 d . . . C1 C 0.3025(4) 0.3601(2) 0.2636(2) 0.0203(7) Uani 1 1 d . . . C2 C 0.6402(5) 0.0790(3) 0.6158(2) 0.0308(9) Uani 1 1 d . . . C3 C 0.8477(4) 0.2255(2) 0.8819(2) 0.0218(8) Uani 1 1 d . . . C11 C -0.1091(5) 0.4150(3) 0.3277(3) 0.0423(11) Uani 1 1 d . . . H11A H -0.0841 0.4713 0.3297 0.063 Uiso 1 1 calc R . . H11B H -0.2059 0.3961 0.3622 0.063 Uiso 1 1 calc R . . H11C H -0.1240 0.4247 0.2718 0.063 Uiso 1 1 calc R . . C21 C 0.7022(5) 0.3053(3) 0.1751(3) 0.0331(10) Uani 1 1 d . . . H21A H 0.6551 0.2893 0.1359 0.040 Uiso 1 1 calc R . . H21B H 0.6981 0.2538 0.2280 0.040 Uiso 1 1 calc R . . C22 C 0.8721(6) 0.3241(3) 0.1457(4) 0.0519(14) Uani 1 1 d . . . H22A H 0.9225 0.3331 0.1880 0.062 Uiso 1 1 calc R . . H22B H 0.9304 0.2715 0.1360 0.062 Uiso 1 1 calc R . . C23 C 0.8805(7) 0.4075(4) 0.0682(4) 0.073(2) Uani 1 1 d . . . H23A H 0.9914 0.4212 0.0525 0.088 Uiso 1 1 calc R . . H23B H 0.8425 0.3956 0.0242 0.088 Uiso 1 1 calc R . . C24 C 0.7823(6) 0.4881(3) 0.0783(3) 0.0491(13) Uani 1 1 d . . . H24A H 0.7831 0.5400 0.0256 0.059 Uiso 1 1 calc R . . H24B H 0.8288 0.5051 0.1171 0.059 Uiso 1 1 calc R . . C25 C 0.6145(5) 0.4673(3) 0.1090(2) 0.0379(11) Uani 1 1 d . . . H25A H 0.5550 0.5188 0.1201 0.045 Uiso 1 1 calc R . . H25B H 0.5629 0.4583 0.0671 0.045 Uiso 1 1 calc R . . C31 C 0.9910(8) 0.1220(4) 0.4501(4) 0.071(2) Uani 1 1 d . . . H31A H 0.9312 0.1742 0.4123 0.107 Uiso 1 1 calc R . . H31B H 0.9820 0.0681 0.4392 0.107 Uiso 1 1 calc R . . H31C H 1.1019 0.1332 0.4431 0.107 Uiso 1 1 calc R . . C41 C 0.1960(7) 0.0567(4) 0.6617(4) 0.0632(16) Uani 1 1 d D . . H41A H 0.0995 0.0956 0.6674 0.076 Uiso 1 1 calc R . . H41B H 0.2229 0.0696 0.6033 0.076 Uiso 1 1 calc R . . C42 C 0.1678(9) -0.0392(5) 0.7049(4) 0.097(3) Uani 1 1 d D . . H42A H 0.2607 -0.0777 0.6941 0.116 Uiso 1 1 calc R . . H42B H 0.0761 -0.0514 0.6842 0.116 Uiso 1 1 calc R . . C43 C 0.1369(7) -0.0633(4) 0.7965(4) 0.085(2) Uani 1 1 d D . . H43A H 0.0378 -0.0296 0.8080 0.102 Uiso 1 1 calc R . . H43B H 0.1255 -0.1287 0.8244 0.102 Uiso 1 1 calc R . . C44 C 0.2707(9) -0.0397(5) 0.8275(4) 0.113(3) Uani 1 1 d D . . H44A H 0.2462 -0.0516 0.8859 0.135 Uiso 1 1 calc R . . H44B H 0.3668 -0.0790 0.8219 0.135 Uiso 1 1 calc R . . C45 C 0.3009(9) 0.0546(5) 0.7842(3) 0.077(2) Uani 1 1 d D . . H45A H 0.3947 0.0660 0.8037 0.092 Uiso 1 1 calc R . . H45B H 0.2100 0.0940 0.7952 0.092 Uiso 1 1 calc R . . C51 C 1.2368(5) 0.3170(3) 0.7918(3) 0.0353(10) Uani 1 1 d . . . H51A H 1.1969 0.3776 0.7561 0.053 Uiso 1 1 calc R . . H51B H 1.3431 0.3017 0.7708 0.053 Uiso 1 1 calc R . . H51C H 1.2400 0.3157 0.8464 0.053 Uiso 1 1 calc R . . C61 C 0.4799(5) 0.1155(2) 0.9839(3) 0.0285(9) Uani 1 1 d . . . H61A H 0.5398 0.0767 1.0308 0.034 Uiso 1 1 calc R . . H61B H 0.5042 0.0901 0.9414 0.034 Uiso 1 1 calc R . . C62 C 0.3044(5) 0.1163(3) 1.0098(3) 0.0371(10) Uani 1 1 d . . . H62A H 0.2755 0.0535 1.0350 0.045 Uiso 1 1 calc R . . H62B H 0.2446 0.1486 0.9616 0.045 Uiso 1 1 calc R . . C63 C 0.2603(5) 0.1623(3) 1.0700(3) 0.0402(11) Uani 1 1 d . . . H63A H 0.1449 0.1658 1.0829 0.048 Uiso 1 1 calc R . . H63B H 0.3104 0.1262 1.1208 0.048 Uiso 1 1 calc R . . C64 C 0.3135(5) 0.2570(3) 1.0351(2) 0.0315(9) Uani 1 1 d . . . H64A H 0.2908 0.2842 1.0764 0.038 Uiso 1 1 calc R . . H64B H 0.2541 0.2953 0.9879 0.038 Uiso 1 1 calc R . . C65 C 0.4890(5) 0.2543(3) 1.0090(2) 0.0262(8) Uani 1 1 d . . . H65A H 0.5198 0.3167 0.9827 0.031 Uiso 1 1 calc R . . H65B H 0.5490 0.2223 1.0573 0.031 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 Cu1 0.0177(2) 0.0255(2) 0.0138(2) -0.00100(18) 0.00007(16) -0.00471(18) Cu2 0.0181(2) 0.0321(3) 0.0293(3) -0.0203(2) 0.00333(18) -0.00739(19) Cu3 0.0130(2) 0.0189(2) 0.0185(2) -0.00520(17) 0.00030(16) -0.00324(16) Cl1 0.0369(5) 0.0318(5) 0.0366(6) -0.0203(4) -0.0006(4) -0.0113(4) Cl2 0.0247(5) 0.0403(5) 0.0197(5) -0.0060(4) -0.0072(4) -0.0048(4) Cl3 0.0695(9) 0.0558(8) 0.0501(8) 0.0291(7) -0.0123(7) 0.0052(7) Cl4 0.0906(12) 0.0802(11) 0.1233(15) -0.0834(12) 0.0068(11) -0.0312(9) Cl5 0.0267(5) 0.0240(5) 0.0441(6) -0.0029(4) -0.0051(4) 0.0030(4) Cl6 0.0287(5) 0.0465(6) 0.0303(5) -0.0179(5) -0.0085(4) -0.0067(4) P1 0.0142(4) 0.0227(5) 0.0175(5) -0.0057(4) 0.0004(3) -0.0064(4) P2 0.0141(4) 0.0200(4) 0.0136(4) -0.0049(4) 0.0009(3) -0.0032(3) P3 0.0270(5) 0.0222(5) 0.0167(5) -0.0076(4) -0.0049(4) 0.0039(4) P4 0.0318(5) 0.0299(5) 0.0131(5) -0.0026(4) -0.0026(4) -0.0170(4) P5 0.0116(4) 0.0262(5) 0.0260(5) -0.0096(4) -0.0025(4) -0.0007(4) P6 0.0144(4) 0.0197(4) 0.0189(5) -0.0066(4) -0.0007(3) -0.0022(3) O1 0.0403(16) 0.0340(16) 0.0221(14) -0.0107(12) -0.0017(12) -0.0107(13) O2 0.0183(12) 0.0318(14) 0.0212(13) -0.0115(11) 0.0006(10) -0.0063(11) O3 0.0314(15) 0.0317(15) 0.0368(17) -0.0130(13) -0.0034(13) -0.0016(12) O4 0.0315(16) 0.0427(18) 0.0337(16) -0.0168(14) 0.0109(13) -0.0093(13) O5 0.030(3) 0.036(3) 0.026(3) -0.015(2) -0.006(2) -0.002(2) O5' 0.023(4) 0.046(5) 0.030(4) -0.013(4) 0.005(3) 0.000(3) O11 0.0181(12) 0.0266(14) 0.0173(13) -0.0039(11) 0.0017(10) -0.0051(10) O12 0.0195(12) 0.0245(13) 0.0198(13) -0.0069(11) 0.0038(10) -0.0078(10) O13 0.0146(12) 0.0296(14) 0.0361(16) -0.0101(12) -0.0022(11) -0.0064(11) O21 0.0171(12) 0.0214(13) 0.0149(12) -0.0042(10) 0.0005(9) -0.0017(10) O22 0.0155(12) 0.0205(13) 0.0253(14) -0.0066(11) -0.0015(10) -0.0033(10) O31 0.0211(14) 0.057(2) 0.0247(16) 0.0126(14) -0.0007(12) 0.0024(14) O32 0.0280(15) 0.056(2) 0.0444(18) -0.0378(16) 0.0137(13) -0.0169(14) O33 0.0432(18) 0.051(2) 0.0343(17) -0.0252(15) -0.0096(14) 0.0220(15) O41 0.0227(14) 0.061(2) 0.0166(14) 0.0049(14) -0.0001(11) -0.0104(14) O42 0.0240(14) 0.056(2) 0.0456(18) -0.0344(16) 0.0055(13) -0.0179(14) O51 0.0167(12) 0.0380(16) 0.0325(15) -0.0195(13) 0.0012(11) -0.0042(11) O52 0.0154(12) 0.0254(14) 0.0261(14) -0.0059(11) 0.0013(10) -0.0036(10) O53 0.0135(12) 0.0346(16) 0.0481(18) -0.0150(14) -0.0071(12) 0.0003(11) O61 0.0188(12) 0.0293(14) 0.0254(14) -0.0143(12) 0.0013(10) -0.0058(11) O62 0.0162(12) 0.0197(12) 0.0199(13) -0.0038(10) 0.0009(10) -0.0012(10) N2 0.0247(16) 0.0277(17) 0.0173(16) -0.0072(13) 0.0038(13) 0.0004(13) N4 0.060(3) 0.056(2) 0.0157(17) -0.0049(17) 0.0012(16) -0.043(2) N6 0.0227(16) 0.0197(15) 0.0206(16) -0.0057(13) 0.0027(12) -0.0048(12) C1 0.0213(18) 0.0224(18) 0.0184(18) -0.0075(15) -0.0043(14) -0.0042(15) C2 0.051(3) 0.0194(19) 0.023(2) -0.0062(16) -0.0119(18) -0.0041(18) C3 0.0190(17) 0.0216(18) 0.0236(19) -0.0071(15) -0.0039(14) -0.0007(14) C11 0.0159(19) 0.046(3) 0.068(3) -0.025(2) -0.006(2) -0.0008(19) C21 0.037(2) 0.035(2) 0.034(2) -0.0231(19) 0.0117(18) -0.0118(19) C22 0.039(3) 0.037(3) 0.077(4) -0.029(3) 0.030(3) -0.006(2) C23 0.072(4) 0.050(3) 0.088(5) -0.033(3) 0.061(4) -0.022(3) C24 0.053(3) 0.038(3) 0.045(3) -0.011(2) 0.025(2) -0.010(2) C25 0.041(2) 0.045(3) 0.015(2) 0.0006(18) 0.0043(17) -0.004(2) C31 0.099(5) 0.039(3) 0.061(4) -0.020(3) 0.043(3) -0.002(3) C41 0.059(3) 0.085(4) 0.061(4) -0.036(3) 0.003(3) -0.038(3) C42 0.091(5) 0.089(5) 0.121(7) -0.043(5) 0.023(5) -0.066(5) C43 0.059(4) 0.049(4) 0.105(6) 0.013(4) 0.028(4) -0.029(3) C44 0.079(5) 0.134(7) 0.052(4) 0.042(4) 0.008(4) -0.026(5) C45 0.095(5) 0.111(5) 0.019(3) -0.007(3) 0.004(3) -0.058(4) C51 0.0180(19) 0.050(3) 0.035(2) -0.010(2) -0.0048(17) -0.0089(18) C61 0.029(2) 0.0179(18) 0.033(2) -0.0056(16) 0.0044(17) -0.0039(16) C62 0.031(2) 0.026(2) 0.048(3) -0.009(2) 0.0083(19) -0.0130(18) C63 0.033(2) 0.035(2) 0.037(3) -0.002(2) 0.0113(19) -0.0054(19) C64 0.035(2) 0.033(2) 0.023(2) -0.0107(17) 0.0065(17) 0.0004(18) C65 0.036(2) 0.028(2) 0.0157(18) -0.0083(16) 0.0018(15) -0.0075(17) _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 Cu1 O41 1.933(3) . ? Cu1 O31 1.947(3) . ? Cu1 O21 1.956(2) . ? Cu1 O11 1.975(2) . ? Cu1 O1 2.270(2) . ? Cu2 O42 1.929(3) . ? Cu2 O61 1.944(3) . ? Cu2 O32 1.952(3) . ? Cu2 O51 1.957(3) . ? Cu3 O52 1.947(2) . ? Cu3 O62 1.952(2) . ? Cu3 O22 1.959(2) 2_666 ? Cu3 O12 1.970(2) 2_666 ? Cu3 O2 2.333(2) . ? Cl1 C1 1.777(4) . ? Cl2 C1 1.801(4) . ? Cl3 C2 1.778(4) . ? Cl4 C2 1.768(4) . ? Cl5 C3 1.786(4) . ? Cl6 C3 1.784(4) . ? P1 O11 1.495(3) . ? P1 O12 1.499(3) . ? P1 O13 1.564(3) . ? P1 C1 1.841(4) . ? P2 O21 1.497(2) . ? P2 O22 1.506(3) . ? P2 N2 1.623(3) . ? P2 C1 1.867(4) . ? P3 O31 1.482(3) . ? P3 O32 1.486(3) . ? P3 O33 1.558(3) . ? P3 C2 1.843(4) . ? P4 O42 1.485(3) . ? P4 O41 1.496(3) . ? P4 N4 1.619(3) . ? P4 C2 1.863(5) . ? P5 O52 1.496(3) . ? P5 O51 1.498(3) . ? P5 O53 1.561(3) . ? P5 C3 1.843(4) . ? P6 O61 1.502(3) . ? P6 O62 1.504(3) . ? P6 N6 1.625(3) . ? P6 C3 1.861(4) . ? O1 H1A 0.84 . ? O1 H1B 0.84 . ? O2 H2A 0.85 . ? O2 H2B 0.85 . ? O3 H3A 0.85 . ? O3 H3B 0.85 . ? O4 H4A 0.85 . ? O4 H4B 0.85 . ? O5 H5A 0.85 . ? O5 H5B 0.86 . ? O5 H5B' 1.28 . ? O5' H5B 1.29 . ? O5' H5A' 0.84 . ? O5' H5B' 0.86 . ? O12 Cu3 1.970(2) 2_666 ? O13 C11 1.449(5) . ? O22 Cu3 1.959(2) 2_666 ? O33 C31 1.440(6) . ? O53 C51 1.441(5) . ? N2 C21 1.461(5) . ? N2 C25 1.469(5) . ? N4 C45 1.476(5) . ? N4 C41 1.488(5) . ? N6 C65 1.466(5) . ? N6 C61 1.478(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C21 C22 1.520(6) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.515(8) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.512(7) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.513(6) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C41 C42 1.476(7) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.535(7) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.499(7) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.458(7) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C61 C62 1.522(5) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.522(7) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.522(6) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.523(5) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 H65A 0.9900 . ? C65 H65B 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 O41 Cu1 O31 93.90(12) . . ? O41 Cu1 O21 166.67(13) . . ? O31 Cu1 O21 87.98(11) . . ? O41 Cu1 O11 83.14(11) . . ? O31 Cu1 O11 174.21(13) . . ? O21 Cu1 O11 93.77(10) . . ? O41 Cu1 O1 102.56(12) . . ? O31 Cu1 O1 89.92(12) . . ? O21 Cu1 O1 90.62(9) . . ? O11 Cu1 O1 95.57(9) . . ? O42 Cu2 O61 87.11(12) . . ? O42 Cu2 O32 93.31(12) . . ? O61 Cu2 O32 170.38(13) . . ? O42 Cu2 O51 175.98(13) . . ? O61 Cu2 O51 93.27(11) . . ? O32 Cu2 O51 85.65(12) . . ? O52 Cu3 O62 93.58(10) . . ? O52 Cu3 O22 168.38(11) . 2_666 ? O62 Cu3 O22 89.51(10) . 2_666 ? O52 Cu3 O12 86.75(10) . 2_666 ? O62 Cu3 O12 172.53(11) . 2_666 ? O22 Cu3 O12 88.75(10) 2_666 2_666 ? O52 Cu3 O2 94.17(9) . . ? O62 Cu3 O2 93.01(9) . . ? O22 Cu3 O2 96.85(9) 2_666 . ? O12 Cu3 O2 94.40(9) 2_666 . ? O11 P1 O12 117.61(15) . . ? O11 P1 O13 107.39(15) . . ? O12 P1 O13 111.81(15) . . ? O11 P1 C1 105.29(15) . . ? O12 P1 C1 106.40(15) . . ? O13 P1 C1 107.77(16) . . ? O21 P2 O22 118.09(15) . . ? O21 P2 N2 109.47(15) . . ? O22 P2 N2 109.68(16) . . ? O21 P2 C1 104.39(15) . . ? O22 P2 C1 104.30(15) . . ? N2 P2 C1 110.6(2) . . ? O31 P3 O32 118.1(2) . . ? O31 P3 O33 110.1(2) . . ? O32 P3 O33 108.7(2) . . ? O31 P3 C2 107.1(2) . . ? O32 P3 C2 105.4(2) . . ? O33 P3 C2 106.8(2) . . ? O42 P4 O41 118.7(2) . . ? O42 P4 N4 110.1(2) . . ? O41 P4 N4 108.8(2) . . ? O42 P4 C2 103.8(2) . . ? O41 P4 C2 103.6(2) . . ? N4 P4 C2 111.6(2) . . ? O52 P5 O51 117.6(2) . . ? O52 P5 O53 111.12(15) . . ? O51 P5 O53 107.87(16) . . ? O52 P5 C3 106.52(16) . . ? O51 P5 C3 106.10(16) . . ? O53 P5 C3 107.00(16) . . ? O61 P6 O62 118.88(15) . . ? O61 P6 N6 108.95(16) . . ? O62 P6 N6 109.17(15) . . ? O61 P6 C3 103.67(16) . . ? O62 P6 C3 104.49(15) . . ? N6 P6 C3 111.4(2) . . ? Cu1 O1 H1A 110.8 . . ? Cu1 O1 H1B 107.5 . . ? H1A O1 H1B 103.4 . . ? Cu3 O2 H2A 124.8 . . ? Cu3 O2 H2B 115.5 . . ? H2A O2 H2B 102.9 . . ? H3A O3 H3B 104.3 . . ? H4A O4 H4B 104.9 . . ? H5A O5 H5B 106.6 . . ? H5A O5 H5B' 154.2 . . ? H5B O5 H5B' 47.6 . . ? H5B O5' H5A' 152.2 . . ? H5B O5' H5B' 47.1 . . ? H5A' O5' H5B' 105.9 . . ? P1 O11 Cu1 129.79(15) . . ? P1 O12 Cu3 126.97(15) . 2_666 ? C11 O13 P1 123.0(3) . . ? P2 O21 Cu1 129.49(15) . . ? P2 O22 Cu3 128.75(15) . 2_666 ? P3 O31 Cu1 135.7(2) . . ? P3 O32 Cu2 131.8(2) . . ? C31 O33 P3 123.6(3) . . ? P4 O41 Cu1 135.6(2) . . ? P4 O42 Cu2 135.6(2) . . ? P5 O51 Cu2 127.75(16) . . ? P5 O52 Cu3 129.63(15) . . ? C51 O53 P5 124.4(3) . . ? P6 O61 Cu2 130.40(16) . . ? P6 O62 Cu3 129.65(15) . . ? C21 N2 C25 114.7(3) . . ? C21 N2 P2 123.4(3) . . ? C25 N2 P2 121.7(3) . . ? C45 N4 C41 113.5(4) . . ? C45 N4 P4 122.2(3) . . ? C41 N4 P4 121.7(3) . . ? C65 N6 C61 114.3(3) . . ? C65 N6 P6 122.9(3) . . ? C61 N6 P6 122.3(3) . . ? Cl1 C1 Cl2 109.3(2) . . ? Cl1 C1 P1 110.9(2) . . ? Cl2 C1 P1 109.9(2) . . ? Cl1 C1 P2 110.5(2) . . ? Cl2 C1 P2 109.4(2) . . ? P1 C1 P2 106.8(2) . . ? Cl4 C2 Cl3 109.4(2) . . ? Cl4 C2 P3 110.5(2) . . ? Cl3 C2 P3 110.4(2) . . ? Cl4 C2 P4 110.0(2) . . ? Cl3 C2 P4 109.2(2) . . ? P3 C2 P4 107.2(2) . . ? Cl6 C3 Cl5 108.8(2) . . ? Cl6 C3 P5 109.6(2) . . ? Cl5 C3 P5 110.6(2) . . ? Cl6 C3 P6 110.3(2) . . ? Cl5 C3 P6 110.1(2) . . ? P5 C3 P6 107.5(2) . . ? O13 C11 H11A 109.5 . . ? O13 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O13 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C21 C22 109.6(3) . . ? N2 C21 H21A 109.8 . . ? C22 C21 H21A 109.8 . . ? N2 C21 H21B 109.8 . . ? C22 C21 H21B 109.8 . . ? H21A C21 H21B 108.2 . . ? C23 C22 C21 110.7(5) . . ? C23 C22 H22A 109.5 . . ? C21 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? C24 C23 C22 111.4(4) . . ? C24 C23 H23A 109.4 . . ? C22 C23 H23A 109.4 . . ? C24 C23 H23B 109.4 . . ? C22 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? C23 C24 C25 111.1(4) . . ? C23 C24 H24A 109.4 . . ? C25 C24 H24A 109.4 . . ? C23 C24 H24B 109.4 . . ? C25 C24 H24B 109.4 . . ? H24A C24 H24B 108.0 . . ? N2 C25 C24 109.8(4) . . ? N2 C25 H25A 109.7 . . ? C24 C25 H25A 109.7 . . ? N2 C25 H25B 109.7 . . ? C24 C25 H25B 109.7 . . ? H25A C25 H25B 108.2 . . ? O33 C31 H31A 109.5 . . ? O33 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O33 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C42 C41 N4 109.5(5) . . ? C42 C41 H41A 109.8 . . ? N4 C41 H41A 109.8 . . ? C42 C41 H41B 109.8 . . ? N4 C41 H41B 109.8 . . ? H41A C41 H41B 108.2 . . ? C41 C42 C43 111.2(5) . . ? C41 C42 H42A 109.4 . . ? C43 C42 H42A 109.4 . . ? C41 C42 H42B 109.4 . . ? C43 C42 H42B 109.4 . . ? H42A C42 H42B 108.0 . . ? C44 C43 C42 109.9(5) . . ? C44 C43 H43A 109.7 . . ? C42 C43 H43A 109.7 . . ? C44 C43 H43B 109.7 . . ? C42 C43 H43B 109.7 . . ? H43A C43 H43B 108.2 . . ? C45 C44 C43 112.1(5) . . ? C45 C44 H44A 109.2 . . ? C43 C44 H44A 109.2 . . ? C45 C44 H44B 109.2 . . ? C43 C44 H44B 109.2 . . ? H44A C44 H44B 107.9 . . ? C44 C45 N4 110.8(5) . . ? C44 C45 H45A 109.5 . . ? N4 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? N4 C45 H45B 109.5 . . ? H45A C45 H45B 108.1 . . ? O53 C51 H51A 109.5 . . ? O53 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? O53 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? N6 C61 C62 110.1(3) . . ? N6 C61 H61A 109.6 . . ? C62 C61 H61A 109.6 . . ? N6 C61 H61B 109.6 . . ? C62 C61 H61B 109.6 . . ? H61A C61 H61B 108.2 . . ? C61 C62 C63 111.1(4) . . ? C61 C62 H62A 109.4 . . ? C63 C62 H62A 109.4 . . ? C61 C62 H62B 109.4 . . ? C63 C62 H62B 109.4 . . ? H62A C62 H62B 108.0 . . ? C64 C63 C62 110.6(3) . . ? C64 C63 H63A 109.5 . . ? C62 C63 H63A 109.5 . . ? C64 C63 H63B 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 108.1 . . ? C63 C64 C65 110.7(3) . . ? C63 C64 H64A 109.5 . . ? C65 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? C65 C64 H64B 109.5 . . ? H64A C64 H64B 108.1 . . ? N6 C65 C64 110.6(3) . . ? N6 C65 H65A 109.5 . . ? C64 C65 H65A 109.5 . . ? N6 C65 H65B 109.5 . . ? C64 C65 H65B 109.5 . . ? H65A C65 H65B 108.1 . . ? 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 H1A O3 0.84 1.92 2.750(3) 171.3 . O1 H1B O22 0.84 2.42 3.122(3) 142.1 . O2 H2A O3 0.85 2.07 2.920(3) 171.9 . O2 H2B O5 0.85 1.89 2.738(5) 175.8 . O2 H2B O5' 0.85 1.94 2.716(7) 151.8 . O3 H3B O4 0.85 2.06 2.831(4) 151.3 . O3 H3A O5 0.85 2.02 2.847(6) 163.2 2_666 O3 H3A O5' 0.85 2.06 2.864(8) 156.9 2_666 O4 H4B O11 0.85 2.30 3.003(4) 141.3 . O4 H4B O41 0.85 2.36 3.003(4) 133.0 . O4 H4A O51 0.85 2.17 2.984(4) 160.4 1_455 O5 H5B O4 0.86 2.08 2.866(6) 150.4 1_655 O5 H5A O1 0.85 2.19 2.937(6) 146.5 . O5' H5B' O4 0.86 1.86 2.720(8) 170.5 1_655 O5' H5A' O5' 0.84 2.81 3.050(16) 98.9 2_766 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.830 _refine_diff_density_min -1.214 #===END======================================================================== data_Structure(2) _database_code_depnum_ccdc_archive 'CCDC 626400' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C7 H19 Cl2 Mg N O8 P2' _chemical_formula_sum 'C7 H19 Cl2 Mg N O8 P2' _chemical_formula_weight 402.38 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' 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 monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.3302(3) _cell_length_b 7.50440(10) _cell_length_c 17.4238(3) _cell_angle_alpha 90.00 _cell_angle_beta 120.6603(5) _cell_angle_gamma 90.00 _cell_volume 3186.48(8) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 27.42 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.678 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 0.681 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8329 _exptl_absorpt_correction_T_max 0.9661 _exptl_absorpt_process_details 'XPREP in SHELXTL' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 KappaCCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22752 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.0319 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 27.42 _reflns_number_total 3620 _reflns_number_gt 3155 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement Denzo _computing_data_reduction Denzo _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0280P)^2^+4.3000P] 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 0.00094(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3620 _refine_ls_number_parameters 194 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0346 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0702 _refine_ls_wR_factor_gt 0.0667 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 0.654536(16) 0.02976(5) 0.44725(3) 0.01990(11) Uani 1 1 d . . . Cl2 Cl 0.665294(16) 0.33489(5) 0.55739(3) 0.02002(11) Uani 1 1 d . . . P1 P 0.560073(16) 0.13202(5) 0.46568(3) 0.01258(11) Uani 1 1 d . . . P2 P 0.596711(16) 0.36607(5) 0.35901(3) 0.01220(11) Uani 1 1 d . . . Mg1 Mg 0.5000 0.05495(10) 0.2500 0.01260(16) Uani 1 2 d S . . Mg2 Mg 0.5000 0.5000 0.5000 0.01351(16) Uani 1 2 d S . . O1 O 0.55573(5) -0.15554(15) 0.26681(8) 0.0178(2) Uani 1 1 d . . . H1A H 0.5611 -0.2296 0.3074 0.027 Uiso 1 1 d R . . H1B H 0.5459 -0.2165 0.2199 0.027 Uiso 1 1 d R . . O2 O 0.47298(5) 0.54260(15) 0.36021(7) 0.0179(2) Uani 1 1 d . . . H2A H 0.4564 0.4540 0.3269 0.027 Uiso 1 1 d R . . H2B H 0.4976 0.5736 0.3487 0.027 Uiso 1 1 d R . . O3 O 0.56987(5) 0.63527(15) 0.52920(8) 0.0185(3) Uani 1 1 d . . . H3A H 0.5700 0.7483 0.5326 0.028 Uiso 1 1 d R . . H3B H 0.5856 0.6071 0.5004 0.028 Uiso 1 1 d R . . O11 O 0.52498(5) 0.03004(15) 0.38215(7) 0.0164(2) Uani 1 1 d . . . O12 O 0.53642(5) 0.28210(15) 0.49022(8) 0.0180(2) Uani 1 1 d . . . O13 O 0.58673(5) -0.00725(15) 0.54549(7) 0.0181(3) Uani 1 1 d . . . O21 O 0.55952(4) 0.25411(14) 0.27929(7) 0.0148(2) Uani 1 1 d . . . O22 O 0.57383(5) 0.52961(14) 0.37846(7) 0.0162(2) Uani 1 1 d . . . N2 N 0.65098(5) 0.42302(18) 0.35460(9) 0.0166(3) Uani 1 1 d . . . C1 C 0.61868(6) 0.2161(2) 0.45744(10) 0.0147(3) Uani 1 1 d . . . C13 C 0.60537(8) 0.0439(2) 0.63677(11) 0.0251(4) Uani 1 1 d . . . H13A H 0.5980 0.1708 0.6389 0.038 Uiso 1 1 calc R . . H13B H 0.6449 0.0218 0.6739 0.038 Uiso 1 1 calc R . . H13C H 0.5858 -0.0264 0.6593 0.038 Uiso 1 1 calc R . . C21 C 0.67375(7) 0.3127(2) 0.31168(12) 0.0233(4) Uani 1 1 d . . . H21A H 0.6477 0.2161 0.2771 0.028 Uiso 1 1 calc R . . H21B H 0.7086 0.2577 0.3577 0.028 Uiso 1 1 calc R . . C22 C 0.68415(8) 0.4280(3) 0.24967(13) 0.0287(4) Uani 1 1 d . . . H22A H 0.6489 0.4756 0.2011 0.034 Uiso 1 1 calc R . . H22B H 0.7008 0.3545 0.2224 0.034 Uiso 1 1 calc R . . C23 C 0.72254(8) 0.5823(3) 0.30135(13) 0.0311(4) Uani 1 1 d . . . H23A H 0.7593 0.5350 0.3447 0.037 Uiso 1 1 calc R . . H23B H 0.7263 0.6616 0.2594 0.037 Uiso 1 1 calc R . . C24 C 0.70045(8) 0.6884(3) 0.35069(13) 0.0289(4) Uani 1 1 d . . . H24A H 0.7278 0.7790 0.3888 0.035 Uiso 1 1 calc R . . H24B H 0.6666 0.7515 0.3069 0.035 Uiso 1 1 calc R . . C25 C 0.68790(7) 0.5685(2) 0.40832(11) 0.0215(4) Uani 1 1 d . . . H25A H 0.7225 0.5180 0.4574 0.026 Uiso 1 1 calc R . . H25B H 0.6705 0.6394 0.4351 0.026 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 Cl1 0.0192(2) 0.0177(2) 0.0215(2) 0.00030(14) 0.00947(17) 0.00678(14) Cl2 0.0196(2) 0.0212(2) 0.01383(19) -0.00333(14) 0.00451(16) -0.00214(15) P1 0.0166(2) 0.0101(2) 0.0118(2) 0.00104(14) 0.00776(17) 0.00135(14) P2 0.0131(2) 0.0118(2) 0.0123(2) 0.00039(14) 0.00689(16) 0.00054(14) Mg1 0.0139(4) 0.0116(4) 0.0120(4) 0.000 0.0064(3) 0.000 Mg2 0.0167(4) 0.0109(4) 0.0143(4) 0.0002(3) 0.0089(3) 0.0013(3) O1 0.0238(6) 0.0149(6) 0.0150(6) 0.0001(4) 0.0100(5) 0.0025(4) O2 0.0203(6) 0.0177(6) 0.0170(6) -0.0003(4) 0.0105(5) -0.0001(4) O3 0.0215(6) 0.0122(6) 0.0253(6) -0.0020(4) 0.0144(5) -0.0007(4) O11 0.0189(6) 0.0163(6) 0.0143(6) -0.0012(4) 0.0088(5) -0.0031(4) O12 0.0235(6) 0.0131(6) 0.0220(6) 0.0008(4) 0.0149(5) 0.0026(4) O13 0.0275(7) 0.0137(6) 0.0126(6) 0.0018(4) 0.0098(5) 0.0023(4) O21 0.0151(6) 0.0145(6) 0.0129(5) 0.0004(4) 0.0058(5) -0.0016(4) O22 0.0203(6) 0.0133(6) 0.0184(6) 0.0015(4) 0.0124(5) 0.0026(4) N2 0.0163(7) 0.0174(7) 0.0196(7) -0.0045(5) 0.0116(6) -0.0035(5) C1 0.0162(8) 0.0131(8) 0.0131(7) -0.0011(6) 0.0063(6) 0.0018(6) C13 0.0364(11) 0.0250(10) 0.0115(8) 0.0018(6) 0.0104(8) 0.0010(7) C21 0.0222(9) 0.0249(9) 0.0291(9) -0.0054(7) 0.0177(8) 0.0001(7) C22 0.0264(10) 0.0412(11) 0.0250(10) -0.0041(8) 0.0178(8) -0.0023(8) C23 0.0230(10) 0.0460(12) 0.0269(10) 0.0039(8) 0.0148(8) -0.0080(8) C24 0.0278(10) 0.0274(10) 0.0313(10) -0.0001(8) 0.0150(9) -0.0098(8) C25 0.0186(8) 0.0247(9) 0.0198(9) -0.0047(7) 0.0089(7) -0.0070(7) _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 1.7898(16) . ? Cl2 C1 1.7960(16) . ? P1 O12 1.4808(11) . ? P1 O11 1.4889(11) . ? P1 O13 1.5891(11) . ? P1 C1 1.8492(16) . ? P2 O21 1.5010(11) . ? P2 O22 1.5051(11) . ? P2 N2 1.6350(13) . ? P2 C1 1.8724(16) . ? Mg1 O11 2.0434(11) . ? Mg1 O11 2.0434(11) 2_655 ? Mg1 O21 2.1118(12) . ? Mg1 O21 2.1118(12) 2_655 ? Mg1 O1 2.1453(12) 2_655 ? Mg1 O1 2.1453(12) . ? Mg2 O12 1.9866(11) . ? Mg2 O12 1.9866(11) 5_666 ? Mg2 O3 2.0446(11) 5_666 ? Mg2 O3 2.0447(11) . ? Mg2 O2 2.1724(11) . ? Mg2 O2 2.1724(11) 5_666 ? O1 H1A 0.8500 . ? O1 H1B 0.8500 . ? O2 H2A 0.8500 . ? O2 H2B 0.8501 . ? O3 H3A 0.8500 . ? O3 H3B 0.8500 . ? O13 C13 1.449(2) . ? N2 C21 1.467(2) . ? N2 C25 1.471(2) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C21 C22 1.525(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.529(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.521(3) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.519(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 O12 P1 O11 119.89(7) . . ? O12 P1 O13 109.31(6) . . ? O11 P1 O13 107.45(6) . . ? O12 P1 C1 108.62(7) . . ? O11 P1 C1 106.14(7) . . ? O13 P1 C1 104.33(7) . . ? O21 P2 O22 119.02(7) . . ? O21 P2 N2 109.63(7) . . ? O22 P2 N2 108.71(7) . . ? O21 P2 C1 105.06(7) . . ? O22 P2 C1 105.31(7) . . ? N2 P2 C1 108.59(7) . . ? O11 Mg1 O11 169.50(7) . 2_655 ? O11 Mg1 O21 91.00(4) . . ? O11 Mg1 O21 96.43(4) 2_655 . ? O11 Mg1 O21 96.43(4) . 2_655 ? O11 Mg1 O21 91.00(4) 2_655 2_655 ? O21 Mg1 O21 89.90(7) . 2_655 ? O11 Mg1 O1 83.93(5) . 2_655 ? O11 Mg1 O1 88.34(5) 2_655 2_655 ? O21 Mg1 O1 174.54(4) . 2_655 ? O21 Mg1 O1 92.68(4) 2_655 2_655 ? O11 Mg1 O1 88.34(5) . . ? O11 Mg1 O1 83.93(5) 2_655 . ? O21 Mg1 O1 92.68(4) . . ? O21 Mg1 O1 174.54(4) 2_655 . ? O1 Mg1 O1 85.16(7) 2_655 . ? O12 Mg2 O12 180.00(7) . 5_666 ? O12 Mg2 O3 92.82(5) . 5_666 ? O12 Mg2 O3 87.18(5) 5_666 5_666 ? O12 Mg2 O3 87.18(5) . . ? O12 Mg2 O3 92.82(5) 5_666 . ? O3 Mg2 O3 179.999(1) 5_666 . ? O12 Mg2 O2 85.78(4) . . ? O12 Mg2 O2 94.22(4) 5_666 . ? O3 Mg2 O2 92.93(5) 5_666 . ? O3 Mg2 O2 87.07(4) . . ? O12 Mg2 O2 94.22(4) . 5_666 ? O12 Mg2 O2 85.78(4) 5_666 5_666 ? O3 Mg2 O2 87.07(5) 5_666 5_666 ? O3 Mg2 O2 92.93(5) . 5_666 ? O2 Mg2 O2 179.998(1) . 5_666 ? Mg1 O1 H1A 113.7 . . ? Mg1 O1 H1B 114.1 . . ? H1A O1 H1B 106.3 . . ? Mg2 O2 H2A 114.0 . . ? Mg2 O2 H2B 116.2 . . ? H2A O2 H2B 106.7 . . ? Mg2 O3 H3A 118.8 . . ? Mg2 O3 H3B 117.5 . . ? H3A O3 H3B 107.7 . . ? P1 O11 Mg1 136.84(7) . . ? P1 O12 Mg2 169.15(8) . . ? C13 O13 P1 122.07(11) . . ? P2 O21 Mg1 135.80(7) . . ? C21 N2 C25 112.86(13) . . ? C21 N2 P2 123.02(11) . . ? C25 N2 P2 123.00(11) . . ? Cl1 C1 Cl2 108.07(8) . . ? Cl1 C1 P1 108.57(8) . . ? Cl2 C1 P1 109.84(8) . . ? Cl1 C1 P2 108.62(8) . . ? Cl2 C1 P2 109.07(8) . . ? P1 C1 P2 112.58(8) . . ? O13 C13 H13A 109.5 . . ? O13 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O13 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N2 C21 C22 109.57(15) . . ? N2 C21 H21A 109.8 . . ? C22 C21 H21A 109.8 . . ? N2 C21 H21B 109.8 . . ? C22 C21 H21B 109.8 . . ? H21A C21 H21B 108.2 . . ? C21 C22 C23 110.41(15) . . ? C21 C22 H22A 109.6 . . ? C23 C22 H22A 109.6 . . ? C21 C22 H22B 109.6 . . ? C23 C22 H22B 109.6 . . ? H22A C22 H22B 108.1 . . ? C24 C23 C22 110.81(15) . . ? C24 C23 H23A 109.5 . . ? C22 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 108.1 . . ? C25 C24 C23 111.48(16) . . ? 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 110.43(14) . . ? N2 C25 H25A 109.6 . . ? C24 C25 H25A 109.6 . . ? N2 C25 H25B 109.6 . . ? C24 C25 H25B 109.6 . . ? H25A C25 H25B 108.1 . . ? 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 0.85 2.18 2.9757(16) 156.4 2_645 O1 H1A O22 0.85 2.11 2.9347(16) 161.9 1_545 O2 H2B O22 0.85 1.98 2.7105(16) 144.2 . O2 H2A O21 0.85 2.24 3.0265(16) 153.6 2_655 O3 H3B O22 0.85 2.06 2.8000(16) 145.2 . O3 H3A O13 0.85 1.88 2.7143(16) 166.9 1_565 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.42 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.410 _refine_diff_density_min -0.555 _refine_diff_density_rms 0.062 #===END===================================================================== data_Structure(3) _database_code_depnum_ccdc_archive 'CCDC 626401' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H60 Cl8 N4 Na2 O24 P8 Zn3, 2(H2 O)' _chemical_formula_sum 'C28 H64 Cl8 N4 Na2 O26 P8 Zn3' _chemical_formula_weight 1646.34 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8138(1) _cell_length_b 11.2658(1) _cell_length_c 15.1752(2) _cell_angle_alpha 100.624(1) _cell_angle_beta 105.179(1) _cell_angle_gamma 105.465(1) _cell_volume 1501.22(3) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.74 _cell_measurement_theta_max 27.44 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.821 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 836 _exptl_absorpt_coefficient_mu 1.852 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6565 _exptl_absorpt_correction_T_max 0.9131 _exptl_absorpt_process_details 'XPREP in SHELXTL (Bruker AXS, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 KappaCCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26594 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0396 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 27.44 _reflns_number_total 6808 _reflns_number_gt 5698 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL v.5.1 (Bruker AXS, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^+1.0000P] 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 0.0018(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6808 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0387 _refine_ls_R_factor_gt 0.0279 _refine_ls_wR_factor_ref 0.0710 _refine_ls_wR_factor_gt 0.0671 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 Zn1 Zn 0.5000 0.5000 0.0000 0.01399(9) Uani 1 2 d S . . Zn2 Zn 0.19075(3) 0.19530(2) 0.108844(17) 0.01305(7) Uani 1 1 d . . . Na1 Na 0.32561(10) 0.02449(9) -0.01820(6) 0.02077(19) Uani 1 1 d . . . Cl1 Cl 0.70015(6) 0.58009(5) 0.28334(4) 0.02182(12) Uani 1 1 d . . . Cl2 Cl 0.49518(6) 0.38363(5) 0.33099(4) 0.02241(13) Uani 1 1 d . . . Cl3 Cl 0.26800(6) 0.02160(5) 0.28570(4) 0.02104(12) Uani 1 1 d . . . Cl4 Cl -0.00441(7) -0.18405(5) 0.25619(4) 0.02408(13) Uani 1 1 d . . . P1 P 0.54657(6) 0.32248(5) 0.14727(4) 0.01392(12) Uani 1 1 d . . . P2 P 0.37272(6) 0.50353(5) 0.18054(4) 0.01386(12) Uani 1 1 d . . . P3 P 0.07100(6) -0.11545(5) 0.09015(4) 0.01386(12) Uani 1 1 d . . . P4 P -0.02168(6) 0.06716(5) 0.22253(4) 0.01567(12) Uani 1 1 d . . . O1 O 0.3021(2) 0.34899(18) -0.07548(13) 0.0359(5) Uani 1 1 d . . . H1A H 0.2534 0.3193 -0.0411 0.054 Uiso 1 1 d R . . H1B H 0.2395 0.3622 -0.1199 0.054 Uiso 1 1 d R . . O2 O 0.55882(18) 0.12301(16) -0.03740(12) 0.0253(4) Uani 1 1 d . . . H2A H 0.6023 0.1984 -0.0002 0.038 Uiso 1 1 d R . . H2B H 0.5503 0.1195 -0.0951 0.038 Uiso 1 1 d R . . O3 O 0.4328(2) -0.01442(17) -0.22364(14) 0.0355(4) Uani 1 1 d . . . H3A H 0.3459 -0.0187 -0.2215 0.053 Uiso 1 1 d R . . H3B H 0.4393 -0.0871 -0.2198 0.053 Uiso 1 1 d R . . O11 O 0.58263(17) 0.37750(14) 0.07082(11) 0.0188(3) Uani 1 1 d . . . O12 O 0.40684(16) 0.20927(14) 0.12013(11) 0.0189(3) Uani 1 1 d . . . O13 O 0.68017(17) 0.28213(15) 0.20108(12) 0.0215(3) Uani 1 1 d . . . O21 O 0.42094(17) 0.56079(14) 0.10754(11) 0.0185(3) Uani 1 1 d . . . O22 O 0.23650(17) 0.38678(14) 0.14884(11) 0.0199(3) Uani 1 1 d . . . O31 O 0.15798(16) -0.00410(13) 0.06514(11) 0.0158(3) Uani 1 1 d . . . O32 O -0.09001(16) -0.18354(13) 0.02907(11) 0.0162(3) Uani 1 1 d . . . O33 O 0.15949(17) -0.21300(14) 0.09579(12) 0.0211(3) Uani 1 1 d . . . O41 O 0.06164(18) 0.17018(15) 0.18702(12) 0.0209(3) Uani 1 1 d . . . O42 O -0.18365(17) -0.00261(16) 0.17024(11) 0.0237(4) Uani 1 1 d . . . N2 N 0.3603(2) 0.61353(17) 0.26125(13) 0.0176(4) Uani 1 1 d . . . N4 N 0.0047(2) 0.12821(18) 0.33479(13) 0.0189(4) Uani 1 1 d . . . C1 C 0.5287(2) 0.4476(2) 0.23596(15) 0.0158(4) Uani 1 1 d . . . C2 C 0.0758(2) -0.0539(2) 0.21267(15) 0.0151(4) Uani 1 1 d . . . C13 C 0.8321(3) 0.3410(3) 0.2017(2) 0.0391(7) Uani 1 1 d . . . H13A H 0.8349 0.4106 0.1711 0.059 Uiso 1 1 calc R . . H13B H 0.8634 0.2766 0.1670 0.059 Uiso 1 1 calc R . . H13C H 0.9002 0.3754 0.2673 0.059 Uiso 1 1 calc R . . C21 C 0.2640(3) 0.5853(2) 0.31969(18) 0.0252(5) Uani 1 1 d . . . H21A H 0.2222 0.4914 0.3082 0.030 Uiso 1 1 calc R . . H21B H 0.1796 0.6179 0.3011 0.030 Uiso 1 1 calc R . . C22 C 0.3518(3) 0.6468(3) 0.42477(19) 0.0339(6) Uani 1 1 d . . . H22A H 0.4284 0.6066 0.4452 0.041 Uiso 1 1 calc R . . H22B H 0.2831 0.6321 0.4622 0.041 Uiso 1 1 calc R . . C23 C 0.4280(3) 0.7908(3) 0.44393(19) 0.0373(7) Uani 1 1 d . . . H23A H 0.3510 0.8327 0.4306 0.045 Uiso 1 1 calc R . . H23B H 0.4903 0.8278 0.5116 0.045 Uiso 1 1 calc R . . C24 C 0.5261(3) 0.8165(2) 0.38161(19) 0.0320(6) Uani 1 1 d . . . H24A H 0.5676 0.9099 0.3909 0.038 Uiso 1 1 calc R . . H24B H 0.6108 0.7843 0.4008 0.038 Uiso 1 1 calc R . . C25 C 0.4367(3) 0.7513(2) 0.27787(17) 0.0223(5) Uani 1 1 d . . . H25A H 0.3612 0.7925 0.2565 0.027 Uiso 1 1 calc R . . H25B H 0.5045 0.7628 0.2397 0.027 Uiso 1 1 calc R . . C33 C 0.0898(3) -0.3502(2) 0.0610(2) 0.0297(6) Uani 1 1 d . . . H33A H 0.0533 -0.3832 0.1089 0.045 Uiso 1 1 calc R . . H33B H 0.1631 -0.3891 0.0479 0.045 Uiso 1 1 calc R . . H33C H 0.0055 -0.3715 0.0025 0.045 Uiso 1 1 calc R . . C41 C -0.0828(3) 0.0596(2) 0.38632(17) 0.0284(6) Uani 1 1 d . . . H41A H -0.0213 0.0204 0.4265 0.034 Uiso 1 1 calc R . . H41B H -0.1721 -0.0099 0.3403 0.034 Uiso 1 1 calc R . . C42 C -0.1313(3) 0.1504(3) 0.4477(2) 0.0430(8) Uani 1 1 d . . . H42A H -0.1845 0.1042 0.4849 0.052 Uiso 1 1 calc R . . H42B H -0.2014 0.1825 0.4068 0.052 Uiso 1 1 calc R . . C43 C 0.0036(3) 0.2633(3) 0.5152(2) 0.0371(7) Uani 1 1 d . . . H43A H 0.0678 0.2324 0.5611 0.045 Uiso 1 1 calc R . . H43B H -0.0311 0.3248 0.5514 0.045 Uiso 1 1 calc R . . C44 C 0.0943(3) 0.3305(2) 0.45993(18) 0.0296(6) Uani 1 1 d . . . H44A H 0.0341 0.3706 0.4198 0.036 Uiso 1 1 calc R . . H44B H 0.1855 0.3990 0.5049 0.036 Uiso 1 1 calc R . . C45 C 0.1381(3) 0.2357(2) 0.39790(17) 0.0249(5) Uani 1 1 d . . . H45A H 0.1907 0.2793 0.3593 0.030 Uiso 1 1 calc R . . H45B H 0.2074 0.2027 0.4385 0.030 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 Zn1 0.01292(17) 0.01492(17) 0.01330(18) 0.00546(13) 0.00431(13) 0.00223(14) Zn2 0.01234(12) 0.01291(12) 0.01295(14) 0.00357(9) 0.00510(9) 0.00174(9) Na1 0.0160(4) 0.0263(5) 0.0188(5) 0.0043(4) 0.0065(4) 0.0056(4) Cl1 0.0161(2) 0.0204(3) 0.0193(3) 0.0020(2) 0.0005(2) -0.0017(2) Cl2 0.0275(3) 0.0266(3) 0.0172(3) 0.0122(2) 0.0095(2) 0.0093(2) Cl3 0.0138(2) 0.0212(3) 0.0210(3) 0.0017(2) -0.0008(2) 0.0036(2) Cl4 0.0280(3) 0.0221(3) 0.0182(3) 0.0110(2) 0.0057(2) 0.0000(2) P1 0.0117(2) 0.0142(3) 0.0159(3) 0.0060(2) 0.0041(2) 0.0036(2) P2 0.0148(3) 0.0130(2) 0.0125(3) 0.0030(2) 0.0038(2) 0.0035(2) P3 0.0138(3) 0.0120(2) 0.0136(3) 0.0036(2) 0.0041(2) 0.0011(2) P4 0.0143(3) 0.0225(3) 0.0124(3) 0.0070(2) 0.0062(2) 0.0062(2) O1 0.0264(9) 0.0435(11) 0.0200(9) 0.0102(8) 0.0042(7) -0.0141(8) O2 0.0249(9) 0.0284(9) 0.0244(9) 0.0072(7) 0.0121(7) 0.0079(7) O3 0.0349(10) 0.0321(10) 0.0446(12) 0.0142(9) 0.0192(9) 0.0108(9) O11 0.0225(8) 0.0194(8) 0.0198(8) 0.0086(6) 0.0112(7) 0.0093(7) O12 0.0142(7) 0.0155(7) 0.0236(9) 0.0015(6) 0.0074(6) 0.0013(6) O13 0.0163(8) 0.0229(8) 0.0266(9) 0.0112(7) 0.0040(7) 0.0086(7) O21 0.0247(8) 0.0213(8) 0.0148(8) 0.0082(6) 0.0092(7) 0.0111(7) O22 0.0167(7) 0.0137(7) 0.0237(9) 0.0012(6) 0.0026(6) 0.0026(6) O31 0.0179(7) 0.0129(7) 0.0170(8) 0.0047(6) 0.0083(6) 0.0027(6) O32 0.0163(7) 0.0144(7) 0.0140(8) 0.0046(6) 0.0040(6) -0.0005(6) O33 0.0198(8) 0.0130(7) 0.0274(9) 0.0038(6) 0.0051(7) 0.0041(6) O41 0.0274(8) 0.0231(8) 0.0236(9) 0.0124(7) 0.0173(7) 0.0135(7) O42 0.0155(8) 0.0381(10) 0.0148(8) 0.0043(7) 0.0044(6) 0.0072(7) N2 0.0212(9) 0.0148(9) 0.0172(10) 0.0032(7) 0.0095(8) 0.0044(8) N4 0.0183(9) 0.0236(10) 0.0129(10) 0.0048(8) 0.0069(8) 0.0025(8) C1 0.0151(10) 0.0156(10) 0.0136(11) 0.0050(8) 0.0034(8) 0.0007(8) C2 0.0116(9) 0.0162(10) 0.0143(11) 0.0055(8) 0.0024(8) 0.0004(8) C13 0.0153(12) 0.0442(16) 0.058(2) 0.0178(15) 0.0070(12) 0.0126(12) C21 0.0294(13) 0.0266(12) 0.0249(13) 0.0080(10) 0.0163(11) 0.0098(11) C22 0.0501(17) 0.0415(15) 0.0199(14) 0.0113(12) 0.0192(12) 0.0211(14) C23 0.0487(17) 0.0382(15) 0.0190(14) -0.0036(11) 0.0083(12) 0.0156(14) C24 0.0318(14) 0.0262(13) 0.0266(14) -0.0051(11) 0.0050(11) 0.0046(11) C25 0.0273(12) 0.0138(10) 0.0234(13) 0.0029(9) 0.0079(10) 0.0049(9) C33 0.0339(14) 0.0131(11) 0.0351(15) 0.0021(10) 0.0048(11) 0.0060(10) C41 0.0281(13) 0.0328(13) 0.0164(12) 0.0054(10) 0.0104(10) -0.0044(11) C42 0.0315(14) 0.0583(19) 0.0252(15) -0.0073(13) 0.0184(12) -0.0034(14) C43 0.0326(14) 0.0443(16) 0.0223(14) -0.0046(12) 0.0131(12) -0.0014(13) C44 0.0332(14) 0.0279(13) 0.0191(13) -0.0002(10) 0.0071(11) 0.0022(11) C45 0.0210(11) 0.0275(12) 0.0201(13) 0.0044(10) 0.0072(10) -0.0008(10) _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 Zn1 O21 2.0660(15) . ? Zn1 O21 2.0661(15) 2_665 ? Zn1 O1 2.0815(17) . ? Zn1 O1 2.0815(17) 2_665 ? Zn1 O11 2.0987(15) . ? Zn1 O11 2.0987(15) 2_665 ? Zn2 O41 1.9526(15) . ? Zn2 O22 2.0202(15) . ? Zn2 O32 2.0296(15) 2 ? Zn2 O12 2.0429(15) . ? Zn2 O31 2.1315(14) . ? Zn2 Na1 3.2400(9) . ? Na1 O42 2.2910(18) 2 ? Na1 O31 2.3166(17) . ? Na1 O2 2.3809(18) . ? Na1 O2 2.4044(19) 2_655 ? Na1 O12 2.4501(18) . ? Na1 P4 3.4512(10) 2 ? Na1 Na1 3.5293(17) 2_655 ? Cl1 C1 1.791(2) . ? Cl2 C1 1.792(2) . ? Cl3 C2 1.792(2) . ? Cl4 C2 1.794(2) . ? P1 O11 1.4895(15) . ? P1 O12 1.5015(15) . ? P1 O13 1.5768(16) . ? P1 C1 1.840(2) . ? P2 O22 1.4969(15) . ? P2 O21 1.4975(15) . ? P2 N2 1.6275(19) . ? P2 C1 1.867(2) . ? P3 O31 1.4901(14) . ? P3 O32 1.5063(15) . ? P3 O33 1.5729(16) . ? P3 C2 1.844(2) . ? P4 O42 1.4891(16) . ? P4 O41 1.5037(15) . ? P4 N4 1.6383(19) . ? P4 C2 1.869(2) . ? P4 Na1 3.4512(10) 2 ? O1 H1A 0.8499 . ? O1 H1B 0.8500 . ? O2 Na1 2.4044(19) 2_655 ? O2 H2A 0.8522 . ? O2 H2B 0.8500 . ? O3 H3A 0.8501 . ? O3 H3B 0.8500 . ? O13 C13 1.459(3) . ? O32 Zn2 2.0296(15) 2 ? O33 C33 1.443(3) . ? O42 Na1 2.2911(18) 2 ? N2 C21 1.471(3) . ? N2 C25 1.474(3) . ? N4 C41 1.472(3) . ? N4 C45 1.472(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C21 C22 1.523(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.530(4) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.528(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.515(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C41 C42 1.510(4) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.527(4) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.528(4) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.516(4) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 H45A 0.9900 . ? C45 H45B 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 O21 Zn1 O21 179.999(2) . 2_665 ? O21 Zn1 O1 93.62(7) . . ? O21 Zn1 O1 86.38(7) 2_665 . ? O21 Zn1 O1 86.38(7) . 2_665 ? O21 Zn1 O1 93.62(7) 2_665 2_665 ? O1 Zn1 O1 179.999(2) . 2_665 ? O21 Zn1 O11 91.36(6) . . ? O21 Zn1 O11 88.64(6) 2_665 . ? O1 Zn1 O11 89.60(7) . . ? O1 Zn1 O11 90.40(7) 2_665 . ? O21 Zn1 O11 88.65(6) . 2_665 ? O21 Zn1 O11 91.35(6) 2_665 2_665 ? O1 Zn1 O11 90.40(7) . 2_665 ? O1 Zn1 O11 89.60(7) 2_665 2_665 ? O11 Zn1 O11 180.0 . 2_665 ? O41 Zn2 O22 91.09(6) . . ? O41 Zn2 O32 116.68(6) . 2 ? O22 Zn2 O32 92.31(6) . 2 ? O41 Zn2 O12 137.53(7) . . ? O22 Zn2 O12 93.97(6) . . ? O32 Zn2 O12 105.21(6) 2 . ? O41 Zn2 O31 92.62(6) . . ? O22 Zn2 O31 175.81(6) . . ? O32 Zn2 O31 87.76(6) 2 . ? O12 Zn2 O31 81.98(6) . . ? O41 Zn2 Na1 137.98(5) . . ? O22 Zn2 Na1 130.60(5) . . ? O32 Zn2 Na1 72.68(5) 2 . ? O12 Zn2 Na1 49.10(5) . . ? O31 Zn2 Na1 45.54(4) . . ? O42 Na1 O31 105.15(6) 2 . ? O42 Na1 O2 95.17(7) 2 . ? O31 Na1 O2 154.23(7) . . ? O42 Na1 O2 127.27(7) 2 2_655 ? O31 Na1 O2 94.84(6) . 2_655 ? O2 Na1 O2 84.96(6) . 2_655 ? O42 Na1 O12 127.45(7) 2 . ? O31 Na1 O12 70.08(5) . . ? O2 Na1 O12 85.06(6) . . ? O2 Na1 O12 105.16(6) 2_655 . ? O42 Na1 Zn2 102.77(5) 2 . ? O31 Na1 Zn2 41.05(4) . . ? O2 Na1 Zn2 119.38(5) . . ? O2 Na1 Zn2 122.88(5) 2_655 . ? O12 Na1 Zn2 39.06(4) . . ? O42 Na1 P4 19.11(4) 2 2 ? O31 Na1 P4 87.72(5) . 2 ? O2 Na1 P4 114.03(5) . 2 ? O2 Na1 P4 122.86(5) 2_655 2 ? O12 Na1 P4 128.68(5) . 2 ? Zn2 Na1 P4 94.89(2) . 2 ? O42 Na1 Na1 118.25(6) 2 2_655 ? O31 Na1 Na1 131.68(6) . 2_655 ? O2 Na1 Na1 42.74(4) . 2_655 ? O2 Na1 Na1 42.22(4) 2_655 2_655 ? O12 Na1 Na1 96.90(5) . 2_655 ? Zn2 Na1 Na1 134.50(4) . 2_655 ? P4 Na1 Na1 130.12(4) 2 2_655 ? O11 P1 O12 118.15(9) . . ? O11 P1 O13 110.09(9) . . ? O12 P1 O13 106.77(9) . . ? O11 P1 C1 108.82(9) . . ? O12 P1 C1 106.14(9) . . ? O13 P1 C1 106.20(10) . . ? O22 P2 O21 119.14(9) . . ? O22 P2 N2 110.11(9) . . ? O21 P2 N2 109.91(9) . . ? O22 P2 C1 103.97(9) . . ? O21 P2 C1 104.22(9) . . ? N2 P2 C1 108.77(10) . . ? O31 P3 O32 117.76(9) . . ? O31 P3 O33 108.40(9) . . ? O32 P3 O33 110.34(8) . . ? O31 P3 C2 106.09(9) . . ? O32 P3 C2 108.16(9) . . ? O33 P3 C2 105.32(9) . . ? O42 P4 O41 118.95(10) . . ? O42 P4 N4 110.33(9) . . ? O41 P4 N4 108.03(9) . . ? O42 P4 C2 106.54(10) . . ? O41 P4 C2 103.48(9) . . ? N4 P4 C2 108.98(10) . . ? O41 P4 Na1 90.16(7) . 2 ? N4 P4 Na1 133.44(7) . 2 ? C2 P4 Na1 107.60(7) . 2 ? Zn1 O1 H1A 114.2 . . ? Zn1 O1 H1B 117.0 . . ? H1A O1 H1B 106.0 . . ? Na1 O2 Na1 95.04(6) . 2_655 ? Na1 O2 H2A 111.2 . . ? Na1 O2 H2A 111.2 2_655 . ? Na1 O2 H2B 112.2 . . ? Na1 O2 H2B 112.3 2_655 . ? H2A O2 H2B 113.5 . . ? H3A O3 H3B 104.5 . . ? P1 O11 Zn1 131.97(9) . . ? P1 O12 Zn2 132.15(9) . . ? P1 O12 Na1 124.60(9) . . ? Zn2 O12 Na1 91.84(6) . . ? C13 O13 P1 121.14(16) . . ? P2 O21 Zn1 134.48(9) . . ? P2 O22 Zn2 136.56(10) . . ? P3 O31 Zn2 131.62(9) . . ? P3 O31 Na1 134.65(9) . . ? Zn2 O31 Na1 93.41(6) . . ? P3 O32 Zn2 128.93(9) . 2 ? C33 O33 P3 124.01(15) . . ? P4 O41 Zn2 140.47(10) . . ? P4 O42 Na1 130.65(10) . 2 ? C21 N2 C25 113.79(18) . . ? C21 N2 P2 123.14(15) . . ? C25 N2 P2 122.95(15) . . ? C41 N4 C45 113.23(18) . . ? C41 N4 P4 121.57(15) . . ? C45 N4 P4 123.43(15) . . ? Cl1 C1 Cl2 108.39(11) . . ? Cl1 C1 P1 109.45(11) . . ? Cl2 C1 P1 108.74(11) . . ? Cl1 C1 P2 109.32(11) . . ? Cl2 C1 P2 110.57(11) . . ? P1 C1 P2 110.32(11) . . ? Cl3 C2 Cl4 107.86(11) . . ? Cl3 C2 P3 107.88(11) . . ? Cl4 C2 P3 110.01(11) . . ? Cl3 C2 P4 108.19(11) . . ? Cl4 C2 P4 110.32(11) . . ? P3 C2 P4 112.43(11) . . ? O13 C13 H13A 109.5 . . ? O13 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O13 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N2 C21 C22 111.0(2) . . ? N2 C21 H21A 109.4 . . ? C22 C21 H21A 109.4 . . ? N2 C21 H21B 109.4 . . ? C22 C21 H21B 109.4 . . ? H21A C21 H21B 108.0 . . ? C21 C22 C23 110.9(2) . . ? C21 C22 H22A 109.5 . . ? C23 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? C23 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? C24 C23 C22 110.5(2) . . ? C24 C23 H23A 109.5 . . ? C22 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 108.1 . . ? C25 C24 C23 110.8(2) . . ? C25 C24 H24A 109.5 . . ? C23 C24 H24A 109.5 . . ? C25 C24 H24B 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 108.1 . . ? N2 C25 C24 111.9(2) . . ? N2 C25 H25A 109.2 . . ? C24 C25 H25A 109.2 . . ? N2 C25 H25B 109.2 . . ? C24 C25 H25B 109.2 . . ? H25A C25 H25B 107.9 . . ? O33 C33 H33A 109.5 . . ? O33 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O33 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N4 C41 C42 110.4(2) . . ? N4 C41 H41A 109.6 . . ? C42 C41 H41A 109.6 . . ? N4 C41 H41B 109.6 . . ? C42 C41 H41B 109.6 . . ? H41A C41 H41B 108.1 . . ? C41 C42 C43 110.8(2) . . ? C41 C42 H42A 109.5 . . ? C43 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? C43 C42 H42B 109.5 . . ? H42A C42 H42B 108.1 . . ? C42 C43 C44 110.5(2) . . ? C42 C43 H43A 109.5 . . ? C44 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? C44 C43 H43B 109.5 . . ? H43A C43 H43B 108.1 . . ? C45 C44 C43 110.5(2) . . ? C45 C44 H44A 109.6 . . ? C43 C44 H44A 109.6 . . ? C45 C44 H44B 109.6 . . ? C43 C44 H44B 109.6 . . ? H44A C44 H44B 108.1 . . ? N4 C45 C44 110.56(19) . . ? N4 C45 H45A 109.5 . . ? C44 C45 H45A 109.5 . . ? N4 C45 H45B 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 108.1 . . ? 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 H1A O32 0.85 1.97 2.736(2) 148.9 2 O1 H1B Cl4 0.85 2.67 3.2464(18) 126.3 2 O2 H2A O11 0.85 2.19 2.946(2) 148.2 . O2 H2B O3 0.85 2.05 2.729(3) 135.9 . O3 H3A O42 0.85 2.00 2.811(2) 160.3 2 O3 H3B O13 0.85 2.30 3.040(2) 144.9 2_655 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.472 _refine_diff_density_min -0.497 _refine_diff_density_rms 0.078 #===END===================================================================== data_Structure(4) _database_code_depnum_ccdc_archive 'CCDC 626402' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C7 H19 Cd Cl2 N O8 P2, H2 O' _chemical_formula_sum 'C7 H21 Cd Cl2 N O9 P2' _chemical_formula_weight 508.49 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' Cd Cd -0.8075 1.2024 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.1901(2) _cell_length_b 5.9097(1) _cell_length_c 16.0130(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.107(1) _cell_angle_gamma 90.00 _cell_volume 847.02(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 27.87 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.994 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 508 _exptl_absorpt_coefficient_mu 1.833 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6826 _exptl_absorpt_correction_T_max 0.7571 _exptl_absorpt_process_details 'XPREP in SHELXTL v.5.1 (Bruker AXS, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 KappaCCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12952 _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_sigmaI/netI 0.0386 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.87 _reflns_number_total 4020 _reflns_number_gt 3857 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL v.5.1 (Bruker AXS, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0100P)^2^+0.5000P] 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 0.0055(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.187(16) _chemical_absolute_configuration unk _refine_ls_number_reflns 4020 _refine_ls_number_parameters 201 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0247 _refine_ls_R_factor_gt 0.0224 _refine_ls_wR_factor_ref 0.0487 _refine_ls_wR_factor_gt 0.0479 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 Cd1 Cd 0.165106(18) 0.15000(3) 0.378806(10) 0.01182(6) Uani 1 1 d . . . Cl1 Cl -0.08540(7) 0.27970(10) 0.16863(4) 0.01467(13) Uani 1 1 d . . . Cl2 Cl -0.19399(7) 0.74189(11) 0.15540(4) 0.01569(13) Uani 1 1 d . . . P1 P -0.15370(7) 0.49460(11) 0.32000(4) 0.01037(14) Uani 1 1 d . . . P2 P 0.12244(6) 0.64352(15) 0.24785(3) 0.00954(12) Uani 1 1 d . . . O1 O 0.1038(2) -0.1484(3) 0.46160(12) 0.0160(4) Uani 1 1 d . . . H1A H 0.0210 -0.2135 0.4407 0.024 Uiso 1 1 d R . . H1B H 0.1055 -0.1168 0.5136 0.024 Uiso 1 1 d R . . O2 O 0.4109(2) 0.0602(4) 0.42340(13) 0.0194(4) Uani 1 1 d . . . H2A H 0.4315 -0.0797 0.4216 0.029 Uiso 1 1 d R . . H2B H 0.4469 0.0983 0.4751 0.029 Uiso 1 1 d R . . O3 O 0.2415(2) 0.3966(3) 0.49578(12) 0.0153(4) Uani 1 1 d . . . H3A H 0.2360 0.3408 0.5439 0.023 Uiso 1 1 d R . . H3B H 0.2002 0.5261 0.4915 0.023 Uiso 1 1 d R . . O4 O 0.4879(2) 0.6237(4) 0.39441(12) 0.0188(4) Uani 1 1 d . . . H4A H 0.5568 0.5688 0.3730 0.028 Uiso 1 1 d R . . H4B H 0.4056 0.5670 0.3675 0.028 Uiso 1 1 d R . . O11 O -0.0645(2) 0.3082(3) 0.37142(12) 0.0130(4) Uani 1 1 d . . . O12 O -0.1587(2) 0.7160(3) 0.36308(13) 0.0158(4) Uani 1 1 d . . . O13 O -0.3214(2) 0.4159(3) 0.28581(13) 0.0142(4) Uani 1 1 d . . . O21 O 0.2070(2) 0.4675(3) 0.30748(12) 0.0126(4) Uani 1 1 d . . . O22 O 0.1205(2) 0.8816(3) 0.27808(12) 0.0136(4) Uani 1 1 d . . . N2 N 0.1790(2) 0.6353(5) 0.15821(13) 0.0139(4) Uani 1 1 d . . . C1 C -0.0774(3) 0.5436(4) 0.22431(16) 0.0116(5) Uani 1 1 d . . . C13 C -0.3653(3) 0.1796(5) 0.2726(2) 0.0221(6) Uani 1 1 d . . . H13A H -0.3928 0.1473 0.2109 0.033 Uiso 1 1 calc R . . H13B H -0.4510 0.1499 0.2979 0.033 Uiso 1 1 calc R . . H13C H -0.2815 0.0825 0.2999 0.033 Uiso 1 1 calc R . . C21 C 0.2472(3) 0.4330(5) 0.1296(2) 0.0166(6) Uani 1 1 d . . . H21A H 0.1789 0.3681 0.0784 0.020 Uiso 1 1 calc R . . H21B H 0.2645 0.3173 0.1755 0.020 Uiso 1 1 calc R . . C22 C 0.3949(3) 0.4966(5) 0.10797(19) 0.0189(6) Uani 1 1 d . . . H22A H 0.4654 0.5513 0.1603 0.023 Uiso 1 1 calc R . . H22B H 0.4392 0.3614 0.0870 0.023 Uiso 1 1 calc R . . C23 C 0.3715(3) 0.6800(6) 0.03981(18) 0.0209(7) Uani 1 1 d . . . H23A H 0.3106 0.6196 -0.0146 0.025 Uiso 1 1 calc R . . H23B H 0.4693 0.7275 0.0296 0.025 Uiso 1 1 calc R . . C24 C 0.2931(4) 0.8831(5) 0.0680(2) 0.0209(6) Uani 1 1 d . . . H24A H 0.2697 0.9942 0.0206 0.025 Uiso 1 1 calc R . . H24B H 0.3608 0.9570 0.1174 0.025 Uiso 1 1 calc R . . C25 C 0.1495(3) 0.8142(5) 0.09334(18) 0.0172(6) Uani 1 1 d . . . H25A H 0.1060 0.9472 0.1164 0.021 Uiso 1 1 calc R . . H25B H 0.0762 0.7597 0.0421 0.021 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 Cd1 0.01224(9) 0.01047(9) 0.01268(9) -0.00013(9) 0.00267(6) 0.00054(8) Cl1 0.0170(3) 0.0111(3) 0.0158(3) -0.0043(2) 0.0033(2) -0.0008(2) Cl2 0.0160(3) 0.0140(3) 0.0150(3) 0.0030(3) -0.0008(2) 0.0028(3) P1 0.0091(3) 0.0117(3) 0.0102(3) -0.0001(3) 0.0020(3) 0.0004(3) P2 0.0104(3) 0.0093(3) 0.0088(2) -0.0001(3) 0.0021(2) -0.0004(3) O1 0.0187(10) 0.0169(10) 0.0128(9) -0.0010(8) 0.0041(8) -0.0032(8) O2 0.0142(10) 0.0181(9) 0.0247(11) -0.0041(8) 0.0019(8) 0.0029(8) O3 0.0189(11) 0.0140(9) 0.0129(9) 0.0003(8) 0.0036(8) 0.0019(8) O4 0.0127(8) 0.0204(12) 0.0229(9) -0.0054(10) 0.0031(7) -0.0019(9) O11 0.0087(9) 0.0179(9) 0.0112(8) 0.0035(8) -0.0001(7) 0.0026(7) O12 0.0180(10) 0.0140(10) 0.0155(9) -0.0023(7) 0.0043(8) 0.0020(7) O13 0.0105(9) 0.0145(9) 0.0178(9) 0.0006(8) 0.0034(8) -0.0018(7) O21 0.0117(9) 0.0123(9) 0.0134(9) 0.0045(8) 0.0018(8) -0.0003(7) O22 0.0153(10) 0.0119(9) 0.0130(9) -0.0031(8) 0.0021(8) -0.0023(8) N2 0.0179(10) 0.0103(10) 0.0155(9) 0.0034(11) 0.0080(8) 0.0032(11) C1 0.0129(12) 0.0105(12) 0.0099(12) -0.0014(10) -0.0004(10) -0.0003(10) C13 0.0180(13) 0.0154(16) 0.0316(14) 0.0017(13) 0.0029(11) -0.0041(12) C21 0.0203(15) 0.0107(12) 0.0220(15) -0.0024(11) 0.0117(12) 0.0019(11) C22 0.0170(14) 0.0219(14) 0.0198(14) 0.0020(12) 0.0081(12) 0.0050(12) C23 0.0228(13) 0.0231(18) 0.0211(13) 0.0041(13) 0.0135(11) 0.0018(13) C24 0.0282(17) 0.0176(14) 0.0193(14) 0.0060(12) 0.0102(13) -0.0009(12) C25 0.0235(15) 0.0171(13) 0.0118(13) 0.0045(11) 0.0058(12) 0.0055(11) _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 Cd1 O22 2.2328(18) 1_545 ? Cd1 O2 2.272(2) . ? Cd1 O21 2.2744(19) . ? Cd1 O11 2.2866(19) . ? Cd1 O1 2.350(2) . ? Cd1 O3 2.3512(19) . ? Cl1 C1 1.790(3) . ? Cl2 C1 1.789(3) . ? P1 O12 1.485(2) . ? P1 O11 1.5023(19) . ? P1 O13 1.584(2) . ? P1 C1 1.847(3) . ? P2 O22 1.489(2) . ? P2 O21 1.504(2) . ? P2 N2 1.634(2) . ? P2 C1 1.884(3) . ? O1 H1A 0.8500 . ? O1 H1B 0.8500 . ? O2 H2A 0.8500 . ? O2 H2B 0.8500 . ? O3 H3A 0.8500 . ? O3 H3B 0.8500 . ? O4 H4A 0.8500 . ? O4 H4B 0.8500 . ? O13 C13 1.456(4) . ? O22 Cd1 2.2329(18) 1_565 ? N2 C25 1.464(3) . ? N2 C21 1.471(4) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C21 C22 1.522(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.519(4) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.520(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.521(4) . ? 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 O22 Cd1 O2 93.88(7) 1_545 . ? O22 Cd1 O21 104.34(7) 1_545 . ? O2 Cd1 O21 94.66(7) . . ? O22 Cd1 O11 103.71(7) 1_545 . ? O2 Cd1 O11 162.16(7) . . ? O21 Cd1 O11 84.03(7) . . ? O22 Cd1 O1 81.15(7) 1_545 . ? O2 Cd1 O1 89.77(7) . . ? O21 Cd1 O1 172.66(7) . . ? O11 Cd1 O1 89.96(7) . . ? O22 Cd1 O3 171.29(7) 1_545 . ? O2 Cd1 O3 78.38(7) . . ? O21 Cd1 O3 80.49(7) . . ? O11 Cd1 O3 83.86(7) . . ? O1 Cd1 O3 94.71(7) . . ? O12 P1 O11 117.53(11) . . ? O12 P1 O13 106.79(11) . . ? O11 P1 O13 109.96(11) . . ? O12 P1 C1 107.75(12) . . ? O11 P1 C1 107.90(12) . . ? O13 P1 C1 106.38(11) . . ? O22 P2 O21 119.32(12) . . ? O22 P2 N2 110.07(14) . . ? O21 P2 N2 108.40(12) . . ? O22 P2 C1 106.14(12) . . ? O21 P2 C1 104.50(12) . . ? N2 P2 C1 107.74(11) . . ? Cd1 O1 H1A 115.2 . . ? Cd1 O1 H1B 115.7 . . ? H1A O1 H1B 107.5 . . ? Cd1 O2 H2A 115.5 . . ? Cd1 O2 H2B 112.6 . . ? H2A O2 H2B 104.5 . . ? Cd1 O3 H3A 114.5 . . ? Cd1 O3 H3B 116.5 . . ? H3A O3 H3B 107.8 . . ? H4A O4 H4B 107.7 . . ? P1 O11 Cd1 135.27(11) . . ? C13 O13 P1 123.20(17) . . ? P2 O21 Cd1 140.15(12) . . ? P2 O22 Cd1 153.14(12) . 1_565 ? C25 N2 C21 112.9(2) . . ? C25 N2 P2 123.9(2) . . ? C21 N2 P2 122.7(2) . . ? Cl2 C1 Cl1 108.19(13) . . ? Cl2 C1 P1 109.12(14) . . ? Cl1 C1 P1 107.22(14) . . ? Cl2 C1 P2 109.78(14) . . ? Cl1 C1 P2 107.50(14) . . ? P1 C1 P2 114.79(13) . . ? O13 C13 H13A 109.5 . . ? O13 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O13 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N2 C21 C22 109.6(2) . . ? N2 C21 H21A 109.8 . . ? C22 C21 H21A 109.8 . . ? N2 C21 H21B 109.8 . . ? C22 C21 H21B 109.8 . . ? H21A C21 H21B 108.2 . . ? C23 C22 C21 110.6(2) . . ? C23 C22 H22A 109.5 . . ? C21 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? C22 C23 C24 110.4(2) . . ? C22 C23 H23A 109.6 . . ? C24 C23 H23A 109.6 . . ? C22 C23 H23B 109.6 . . ? C24 C23 H23B 109.6 . . ? H23A C23 H23B 108.1 . . ? C23 C24 C25 111.5(2) . . ? C23 C24 H24A 109.3 . . ? C25 C24 H24A 109.3 . . ? C23 C24 H24B 109.3 . . ? C25 C24 H24B 109.3 . . ? H24A C24 H24B 108.0 . . ? N2 C25 C24 110.5(2) . . ? N2 C25 H25A 109.6 . . ? C24 C25 H25A 109.6 . . ? N2 C25 H25B 109.6 . . ? C24 C25 H25B 109.6 . . ? H25A C25 H25B 108.1 . . ? 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 H1A O12 0.85 1.88 2.688(3) 159.4 1_545 O1 H1B O11 0.85 2.01 2.790(3) 152.0 2_546 O2 H2A O4 0.85 1.91 2.742(3) 167.5 1_545 O2 H2B O4 0.85 2.04 2.879(3) 167.1 2_646 O3 H3A O12 0.85 1.94 2.758(3) 162.3 2_546 O3 H3B O1 0.85 2.13 2.970(3) 171.2 1_565 O4 H4A O13 0.85 2.17 2.997(3) 163.1 1_655 O4 H4B O21 0.85 1.95 2.797(3) 173.9 . _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.387 _refine_diff_density_min -0.437 _refine_diff_density_rms 0.077