Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Chen-Wei Liu' _publ_contact_author_address ; Department of Chemistry National Dong Hwa University Hualien 974 TAIWAN ; _publ_contact_author_email CHENWEI@MAIL.NDHU.EDU.TW _publ_section_title ; Coordination chemistry of group 12 metals with phosphorodiselenoates: syntheses, structures and VT 31P NMR study of monomer - dimer exchange equilibrium ; loop_ _publ_author_name 'Chen-Wei Liu.' 'Chiu-Mine Hung.' 'Ben-Jie Liaw.' 'Hong Yuan Liu.' ; T.S.Lobana ; 'Bidyut Kumar Santra' 'Ju-Chun Wang.' data_compound_1 _database_code_depnum_ccdc_archive 'CCDC 227427' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H20 Cd O4 P2 Se4' _chemical_formula_weight 670.42 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' Se Se -0.0929 2.2259 '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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 20.798(3) _cell_length_b 20.798(3) _cell_length_c 4.4144(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1909.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 733 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 24.94 _exptl_crystal_description needle _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.332 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 8.940 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6166 _exptl_absorpt_correction_T_max 0.9703 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1739 _diffrn_reflns_av_R_equivalents 0.0523 _diffrn_reflns_av_sigmaI/netI 0.0485 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 24.99 _reflns_number_total 812 _reflns_number_gt 600 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0651P)^2^+8.9684P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 812 _refine_ls_number_parameters 57 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0739 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1317 _refine_ls_wR_factor_gt 0.1226 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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 Cd1 Cd 0.5000 0.2500 0.8750 0.0496(5) Uani 1 4 d S . . Se1 Se 0.60429(4) 0.29372(5) 1.1661(3) 0.0604(4) Uani 1 1 d . . . P1 P 0.5523(2) 0.3776(2) 1.3734(11) 0.0474(12) Uani 0.50 1 d P . . O1 O 0.6020(5) 0.4069(5) 1.609(3) 0.052(3) Uani 0.50 1 d P . . O2 O 0.5365(5) 0.4333(6) 1.143(3) 0.056(3) Uani 0.50 1 d P . . C1 C 0.5813(7) 0.4602(7) 1.805(5) 0.128(6) Uani 1 1 d . . . C2 C 0.6283(13) 0.4876(10) 1.963(6) 0.200(12) Uani 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 Cd1 0.0420(5) 0.0420(5) 0.0646(10) 0.000 0.000 0.000 Se1 0.0448(6) 0.0602(6) 0.0763(8) -0.0019(5) -0.0053(5) -0.0078(4) P1 0.040(2) 0.034(2) 0.068(4) -0.004(2) 0.003(2) -0.0017(17) O1 0.048(6) 0.044(6) 0.064(9) -0.009(6) -0.007(6) -0.003(5) O2 0.046(6) 0.052(7) 0.069(9) 0.032(6) 0.013(6) 0.009(5) C1 0.082(9) 0.088(9) 0.213(18) -0.075(11) -0.022(11) 0.017(7) C2 0.26(3) 0.123(14) 0.22(2) -0.086(16) -0.11(2) 0.042(18) _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 Se1 2.6800(10) . ? Cd1 Se1 2.6800(10) 11_667 ? Cd1 Se1 2.6800(10) 6_554 ? Cd1 Se1 2.6800(10) 16_657 ? Se1 P1 2.248(4) . ? Se1 P1 2.256(4) 11_668 ? P1 O2 1.577(12) . ? P1 O1 1.587(12) . ? P1 Se1 2.256(4) 16_658 ? O1 C1 1.474(18) . ? O2 C1 1.84(2) 1_554 ? C1 C2 1.33(2) . ? C1 O2 1.84(2) 1_556 ? 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 Se1 Cd1 Se1 103.29(2) . 11_667 ? Se1 Cd1 Se1 122.69(5) . 6_554 ? Se1 Cd1 Se1 103.29(2) 11_667 6_554 ? Se1 Cd1 Se1 103.29(2) . 16_657 ? Se1 Cd1 Se1 122.69(5) 11_667 16_657 ? Se1 Cd1 Se1 103.29(2) 6_554 16_657 ? P1 Se1 P1 128.57(12) . 11_668 ? P1 Se1 Cd1 93.99(12) . . ? P1 Se1 Cd1 94.09(12) 11_668 . ? O2 P1 O1 106.1(7) . . ? O2 P1 Se1 114.1(5) . . ? O1 P1 Se1 104.5(5) . . ? O2 P1 Se1 103.9(5) . 16_658 ? O1 P1 Se1 113.0(5) . 16_658 ? Se1 P1 Se1 115.23(18) . 16_658 ? C1 O1 P1 118.9(9) . . ? P1 O2 C1 129.7(8) . 1_554 ? C2 C1 O1 114.6(14) . . ? C2 C1 O2 94.5(19) . 1_556 ? O1 C1 O2 113.3(12) . 1_556 ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 0.832 _refine_diff_density_min -0.452 _refine_diff_density_rms 0.138 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 227428' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H56 Cd2 O8 P4 Se8' _chemical_formula_weight 1453.05 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' Se Se -0.0929 2.2259 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 11.287(2) _cell_length_b 17.274(2) _cell_length_c 26.846(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.838(15) _cell_angle_gamma 90.00 _cell_volume 5157.0(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 35 _cell_measurement_theta_min 3.39 _cell_measurement_theta_max 12.35 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.872 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2768 _exptl_absorpt_coefficient_mu 6.628 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5058 _exptl_absorpt_correction_T_max 0.9711 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 297 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4239 _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_sigmaI/netI 0.0909 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 22.49 _reflns_number_total 3326 _reflns_number_gt 1452 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0798P)^2^+11.6123P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3326 _refine_ls_number_parameters 200 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1707 _refine_ls_R_factor_gt 0.0673 _refine_ls_wR_factor_ref 0.1903 _refine_ls_wR_factor_gt 0.1463 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _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 0.02930(13) 0.63161(8) 0.17415(4) 0.1155(6) Uani 1 1 d . . . Se3 Se 0.18536(18) 0.66793(11) 0.25408(7) 0.1204(7) Uani 1 1 d . . . Se1 Se 0.1484(2) 0.62136(15) 0.09480(7) 0.1534(9) Uani 1 1 d . . . Se4 Se -0.1073(2) 0.50977(12) 0.16904(8) 0.1422(9) Uani 1 1 d . . . Se2 Se -0.0678(2) 0.75424(13) 0.12408(7) 0.1446(9) Uani 1 1 d . . . P1 P 0.0275(5) 0.7121(3) 0.06713(18) 0.1252(18) Uani 1 1 d . . . P2 P 0.2288(5) 0.5558(3) 0.2863(2) 0.1202(17) Uani 1 1 d . . . O3 O 0.2413(15) 0.4998(9) 0.2405(6) 0.177(6) Uani 1 1 d . . . O1 O 0.0892(15) 0.7796(9) 0.0411(4) 0.157(5) Uani 1 1 d . A . O2 O -0.0632(14) 0.6881(10) 0.0177(5) 0.162(5) Uani 1 1 d . . . O4 O 0.3564(13) 0.5588(9) 0.3178(7) 0.227(8) Uani 1 1 d D B . C1 C 0.156(3) 0.8373(17) 0.0708(10) 0.173(9) Uani 1 1 d . . . C4 C -0.122(4) 0.6179(16) 0.0088(11) 0.214(15) Uani 1 1 d . . . H4A H -0.0834 0.5767 0.0311 0.257 Uiso 1 1 calc R . . C5 C -0.245(3) 0.619(2) 0.0056(15) 0.36(3) Uani 1 1 d . . . H5A H -0.2643 0.6254 0.0388 0.535 Uiso 1 1 calc R . . H5B H -0.2781 0.5714 -0.0088 0.535 Uiso 1 1 calc R . . H5C H -0.2775 0.6616 -0.0154 0.535 Uiso 1 1 calc R . . C2 C 0.275(3) 0.827(2) 0.0669(15) 0.34(3) Uani 1 1 d . A . H2A H 0.3104 0.7896 0.0915 0.515 Uiso 1 1 calc R . . H2B H 0.3169 0.8752 0.0728 0.515 Uiso 1 1 calc R . . H2C H 0.2804 0.8084 0.0336 0.515 Uiso 1 1 calc R . . C7 C 0.226(3) 0.4187(18) 0.2374(12) 0.207(12) Uani 1 1 d . . . H7A H 0.1546 0.4060 0.2520 0.248 Uiso 1 1 calc R . . C8 C 0.203(3) 0.3957(17) 0.1871(11) 0.33(2) Uani 1 1 d . . . H8A H 0.1323 0.4210 0.1700 0.500 Uiso 1 1 calc R . . H8B H 0.1920 0.3406 0.1853 0.500 Uiso 1 1 calc R . . H8C H 0.2705 0.4095 0.1712 0.500 Uiso 1 1 calc R . . C6 C -0.106(3) 0.606(2) -0.0477(13) 0.37(3) Uani 1 1 d . . . H6A H -0.1447 0.5584 -0.0602 0.558 Uiso 1 1 calc R . . H6B H -0.0224 0.6035 -0.0497 0.558 Uiso 1 1 calc R . . H6C H -0.1428 0.6484 -0.0677 0.558 Uiso 1 1 calc R . . C9 C 0.328(4) 0.382(2) 0.2682(19) 0.46(4) Uani 1 1 d . . . H9A H 0.3172 0.3269 0.2669 0.697 Uiso 1 1 calc R . . H9B H 0.3336 0.3994 0.3026 0.697 Uiso 1 1 calc R . . H9C H 0.3998 0.3956 0.2558 0.697 Uiso 1 1 calc R . . C3A C 0.104(5) 0.919(4) 0.058(2) 0.20(2) Uiso 0.50 1 d P A 1 C3B C 0.150(5) 0.902(3) 0.0241(18) 0.169(17) Uiso 0.50 1 d P A 2 C10 C 0.452(3) 0.5914(15) 0.3515(12) 0.33(2) Uiso 1 1 d D . . C11A C 0.493(4) 0.665(2) 0.3284(17) 0.20(2) Uiso 0.50 1 d PD B 1 C12A C 0.552(3) 0.529(3) 0.357(2) 0.26(3) Uiso 0.50 1 d PD B 1 C11B C 0.421(4) 0.6735(18) 0.3619(18) 0.21(2) Uiso 0.50 1 d PD B 2 C12B C 0.463(5) 0.545(4) 0.4007(12) 0.30(3) Uiso 0.50 1 d PD B 2 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 0.1339(11) 0.1222(11) 0.0865(8) 0.0129(8) 0.0080(7) 0.0015(10) Se3 0.1325(16) 0.1124(14) 0.1106(13) 0.0013(11) 0.0045(12) -0.0159(13) Se1 0.161(2) 0.191(2) 0.1136(14) 0.0069(15) 0.0385(14) 0.0467(18) Se4 0.171(2) 0.1237(16) 0.1302(16) -0.0336(13) 0.0214(14) -0.0217(16) Se2 0.176(2) 0.1452(18) 0.1172(15) 0.0317(13) 0.0381(14) 0.0482(17) P1 0.146(5) 0.143(5) 0.086(3) 0.008(3) 0.016(3) -0.002(4) P2 0.116(4) 0.117(4) 0.117(4) -0.001(3) -0.009(3) 0.007(4) O3 0.242(18) 0.117(11) 0.184(14) -0.040(10) 0.070(13) 0.001(12) O1 0.219(15) 0.166(12) 0.086(8) -0.003(9) 0.028(9) -0.022(12) O2 0.181(13) 0.157(13) 0.141(12) 0.017(10) 0.008(10) -0.025(12) O4 0.138(13) 0.216(17) 0.29(2) 0.081(16) -0.055(14) 0.023(13) C1 0.16(2) 0.17(2) 0.18(2) -0.04(2) -0.018(19) 0.00(2) C4 0.32(5) 0.13(2) 0.16(2) -0.013(18) -0.05(3) -0.03(3) C5 0.21(3) 0.48(7) 0.34(5) 0.08(5) -0.06(4) -0.17(4) C2 0.19(3) 0.38(5) 0.46(6) -0.27(5) 0.07(4) -0.10(4) C7 0.23(3) 0.17(3) 0.21(3) -0.06(2) 0.03(2) 0.04(3) C8 0.50(6) 0.28(4) 0.21(3) -0.13(3) 0.01(4) 0.20(4) C6 0.29(4) 0.51(7) 0.31(5) -0.26(5) 0.03(4) -0.04(5) C9 0.55(8) 0.18(3) 0.57(8) 0.00(4) -0.17(7) 0.14(4) _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 Se4 2.598(3) . ? Cd1 Se3 2.609(2) . ? Cd1 Se2 2.644(2) . ? Cd1 Se1 2.712(2) . ? Se3 P2 2.144(5) . ? Se1 P1 2.127(6) . ? Se4 P2 2.125(6) 2 ? Se2 P1 2.141(6) . ? P1 O1 1.581(15) . ? P1 O2 1.586(15) . ? P2 O4 1.542(14) . ? P2 O3 1.589(14) . ? P2 Se4 2.125(6) 2 ? O3 C7 1.41(3) . ? O1 C1 1.41(2) . ? O2 C4 1.38(3) . ? O4 C10 1.404(19) . ? C1 C2 1.37(3) . ? C1 C3A 1.54(6) . ? C1 C3B 1.67(5) . ? C4 C5 1.38(4) . ? C4 C6 1.57(4) . ? C7 C8 1.39(3) . ? C7 C9 1.44(4) . ? C10 C11B 1.499(19) . ? C10 C11A 1.514(19) . ? C10 C12B 1.534(19) . ? C10 C12A 1.549(19) . ? 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 Se4 Cd1 Se3 123.31(8) . . ? Se4 Cd1 Se2 115.56(9) . . ? Se3 Cd1 Se2 112.85(9) . . ? Se4 Cd1 Se1 105.95(9) . . ? Se3 Cd1 Se1 107.82(8) . . ? Se2 Cd1 Se1 82.58(7) . . ? P2 Se3 Cd1 100.95(16) . . ? P1 Se1 Cd1 81.46(15) . . ? P2 Se4 Cd1 95.83(16) 2 . ? P1 Se2 Cd1 82.86(16) . . ? O1 P1 O2 95.4(8) . . ? O1 P1 Se1 113.2(6) . . ? O2 P1 Se1 112.5(6) . . ? O1 P1 Se2 112.2(6) . . ? O2 P1 Se2 110.8(6) . . ? Se1 P1 Se2 111.8(2) . . ? O4 P2 O3 104.3(10) . . ? O4 P2 Se4 109.6(7) . 2 ? O3 P2 Se4 111.1(6) . 2 ? O4 P2 Se3 108.5(7) . . ? O3 P2 Se3 106.5(6) . . ? Se4 P2 Se3 116.1(3) 2 . ? C7 O3 P2 128.7(18) . . ? C1 O1 P1 120.4(14) . . ? C4 O2 P1 126.5(15) . . ? C10 O4 P2 155.8(17) . . ? C2 C1 O1 107(3) . . ? C2 C1 C3A 117(4) . . ? O1 C1 C3A 112(3) . . ? C2 C1 C3B 87(3) . . ? O1 C1 C3B 96(2) . . ? C3A C1 C3B 42(2) . . ? C5 C4 O2 116(3) . . ? C5 C4 C6 103(3) . . ? O2 C4 C6 99(3) . . ? C8 C7 O3 110(3) . . ? C8 C7 C9 115(3) . . ? O3 C7 C9 109(3) . . ? O4 C10 C11B 108.5(19) . . ? O4 C10 C11A 109.0(18) . . ? C11B C10 C11A 52(3) . . ? O4 C10 C12B 106.4(18) . . ? C11B C10 C12B 109(5) . . ? C11A C10 C12B 144(3) . . ? O4 C10 C12A 104.8(17) . . ? C11B C10 C12A 146(3) . . ? C11A C10 C12A 111(4) . . ? C12B C10 C12A 66(3) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 22.49 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.530 _refine_diff_density_min -0.390 _refine_diff_density_rms 0.092 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 279621' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H28 Hg O4 P2 Se4' _chemical_formula_weight 814.71 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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 11.956(3) _cell_length_b 9.2117(18) _cell_length_c 22.082(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.808(13) _cell_angle_gamma 90.00 _cell_volume 2426.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 43 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 11.51 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.230 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 12.486 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7299 _exptl_absorpt_correction_T_max 0.8401 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 297 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4197 _diffrn_reflns_av_R_equivalents 0.0662 _diffrn_reflns_av_sigmaI/netI 0.0692 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 22.49 _reflns_number_total 3135 _reflns_number_gt 2256 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1075P)^2^+0.0000P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3135 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0940 _refine_ls_R_factor_gt 0.0633 _refine_ls_wR_factor_ref 0.1703 _refine_ls_wR_factor_gt 0.1506 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 Hg1 Hg 0.90428(6) 0.23074(8) 0.18712(3) 0.0603(3) Uani 1 1 d . . . Se1 Se 0.77470(15) 0.0862(2) 0.09110(8) 0.0655(6) Uani 1 1 d . . . Se2 Se 0.70825(14) 0.3399(2) 0.20645(7) 0.0550(5) Uani 1 1 d . . . Se3 Se 1.03401(14) 0.0884(2) 0.26135(7) 0.0585(5) Uani 1 1 d . . . Se4 Se 1.02693(15) 0.37379(19) 0.11031(7) 0.0561(5) Uani 1 1 d . . . P1 P 0.6529(4) 0.2337(5) 0.12285(18) 0.0492(11) Uani 1 1 d . . . P2 P 0.9124(3) 0.0355(5) 0.32602(18) 0.0474(11) Uani 1 1 d . . . O1 O 0.6141(9) 0.3487(12) 0.0725(5) 0.056(3) Uani 1 1 d . . . O2 O 0.5390(9) 0.1598(12) 0.1337(5) 0.053(3) Uani 1 1 d . . . O3 O 0.8733(9) 0.1717(12) 0.3611(5) 0.059(3) Uani 1 1 d . . . O4 O 0.8059(9) -0.0079(15) 0.2876(5) 0.073(4) Uani 1 1 d . . . C1 C 0.6941(16) 0.458(2) 0.0531(8) 0.066(5) Uani 1 1 d . . . H1A H 0.7686 0.4397 0.0729 0.079 Uiso 1 1 calc R . . C2 C 0.698(2) 0.443(3) -0.0141(9) 0.103(8) Uani 1 1 d . . . H2A H 0.7254 0.3480 -0.0234 0.154 Uiso 1 1 calc R . . H2B H 0.7469 0.5152 -0.0290 0.154 Uiso 1 1 calc R . . H2C H 0.6239 0.4552 -0.0331 0.154 Uiso 1 1 calc R . . C3 C 0.6528(19) 0.606(2) 0.0718(9) 0.090(7) Uani 1 1 d . . . H3A H 0.6540 0.6114 0.1153 0.135 Uiso 1 1 calc R . . H3B H 0.5777 0.6210 0.0549 0.135 Uiso 1 1 calc R . . H3C H 0.7008 0.6803 0.0572 0.135 Uiso 1 1 calc R . . C4 C 0.4818(16) 0.072(3) 0.0879(10) 0.087(7) Uani 1 1 d . . . H4A H 0.5312 0.0548 0.0549 0.105 Uiso 1 1 calc R . . C5 C 0.3777(18) 0.136(3) 0.0634(10) 0.109(9) Uani 1 1 d . . . H5A H 0.3930 0.2258 0.0439 0.164 Uiso 1 1 calc R . . H5B H 0.3294 0.1525 0.0957 0.164 Uiso 1 1 calc R . . H5C H 0.3417 0.0702 0.0343 0.164 Uiso 1 1 calc R . . C6 C 0.455(2) -0.078(3) 0.1196(16) 0.150(14) Uani 1 1 d . . . H6A H 0.5238 -0.1222 0.1352 0.225 Uiso 1 1 calc R . . H6B H 0.4176 -0.1417 0.0904 0.225 Uiso 1 1 calc R . . H6C H 0.4077 -0.0609 0.1523 0.225 Uiso 1 1 calc R . . C7 C 0.9458(18) 0.2895(19) 0.3848(9) 0.070(5) Uani 1 1 d . . . H7A H 0.9984 0.3122 0.3540 0.084 Uiso 1 1 calc R . . C8 C 0.8675(19) 0.418(2) 0.3889(10) 0.092(7) Uani 1 1 d . . . H8A H 0.8285 0.4338 0.3501 0.138 Uiso 1 1 calc R . . H8B H 0.9102 0.5027 0.4006 0.138 Uiso 1 1 calc R . . H8C H 0.8143 0.3981 0.4185 0.138 Uiso 1 1 calc R . . C9 C 1.013(3) 0.256(3) 0.4423(11) 0.155(14) Uani 1 1 d . . . H9A H 1.0599 0.1732 0.4362 0.232 Uiso 1 1 calc R . . H9B H 0.9634 0.2345 0.4736 0.232 Uiso 1 1 calc R . . H9C H 1.0588 0.3378 0.4541 0.232 Uiso 1 1 calc R . . C10 C 0.7049(17) -0.081(2) 0.3069(9) 0.080(6) Uani 1 1 d . . . H10A H 0.7233 -0.1270 0.3464 0.096 Uiso 1 1 calc R . . C11 C 0.6120(15) 0.021(2) 0.3134(10) 0.095(8) Uani 1 1 d . . . H11A H 0.6342 0.0933 0.3432 0.142 Uiso 1 1 calc R . . H11B H 0.5478 -0.0303 0.3261 0.142 Uiso 1 1 calc R . . H11C H 0.5933 0.0678 0.2752 0.142 Uiso 1 1 calc R . . C12 C 0.677(2) -0.197(3) 0.2619(14) 0.126(10) Uani 1 1 d . . . H12A H 0.7406 -0.2605 0.2598 0.189 Uiso 1 1 calc R . . H12B H 0.6600 -0.1538 0.2228 0.189 Uiso 1 1 calc R . . H12C H 0.6140 -0.2509 0.2739 0.189 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 Hg1 0.0494(5) 0.0675(5) 0.0627(5) 0.0193(4) -0.0057(3) -0.0013(4) Se1 0.0562(11) 0.0651(12) 0.0743(12) -0.0271(10) -0.0020(9) 0.0052(9) Se2 0.0525(10) 0.0632(11) 0.0492(9) -0.0124(8) 0.0019(8) 0.0032(9) Se3 0.0486(10) 0.0753(13) 0.0527(9) 0.0216(9) 0.0113(8) 0.0171(9) Se4 0.0699(12) 0.0561(11) 0.0436(9) -0.0105(8) 0.0126(8) -0.0128(9) P1 0.044(2) 0.055(3) 0.048(2) 0.001(2) -0.0010(19) -0.003(2) P2 0.038(2) 0.058(3) 0.045(2) 0.007(2) 0.0030(18) 0.007(2) O1 0.051(7) 0.057(7) 0.059(7) 0.007(6) -0.007(5) -0.020(6) O2 0.046(6) 0.055(7) 0.058(6) -0.013(6) 0.002(5) -0.021(6) O3 0.058(7) 0.045(7) 0.074(7) 0.000(6) 0.010(6) 0.003(6) O4 0.060(8) 0.090(9) 0.066(7) 0.021(7) -0.016(6) -0.018(7) C1 0.067(13) 0.050(12) 0.078(12) 0.018(9) -0.013(10) 0.003(10) C2 0.12(2) 0.106(19) 0.083(15) 0.020(14) 0.017(14) -0.012(16) C3 0.101(17) 0.079(16) 0.086(14) 0.014(12) -0.012(13) -0.031(13) C4 0.050(12) 0.12(2) 0.091(14) -0.039(14) 0.013(11) -0.002(13) C5 0.080(16) 0.14(2) 0.106(17) 0.050(16) -0.037(14) -0.015(15) C6 0.12(2) 0.067(17) 0.25(4) 0.02(2) -0.08(2) -0.008(15) C7 0.088(15) 0.055(12) 0.071(12) -0.003(10) 0.026(11) 0.013(11) C8 0.105(18) 0.067(15) 0.104(16) -0.005(12) 0.017(14) 0.024(13) C9 0.23(4) 0.12(2) 0.097(19) -0.005(16) -0.09(2) 0.00(2) C10 0.076(14) 0.081(15) 0.083(13) 0.020(12) 0.013(11) -0.038(13) C11 0.058(13) 0.072(15) 0.16(2) 0.017(14) 0.036(14) 0.028(12) C12 0.084(18) 0.10(2) 0.19(3) -0.06(2) 0.019(19) -0.022(16) _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 Hg1 Se3 2.5442(17) . ? Hg1 Se2 2.6114(19) . ? Hg1 Se4 2.6635(18) . ? Hg1 Se1 2.8692(19) . ? Se1 P1 2.143(5) . ? Se2 P1 2.154(4) . ? Se3 P2 2.160(4) . ? Se4 P2 2.141(4) 2_755 ? P1 O2 1.555(11) . ? P1 O1 1.583(11) . ? P2 O4 1.536(11) . ? P2 O3 1.563(12) . ? P2 Se4 2.141(4) 2_745 ? O1 C1 1.47(2) . ? O2 C4 1.43(2) . ? O3 C7 1.46(2) . ? O4 C10 1.47(2) . ? C1 C2 1.49(3) . ? C1 C3 1.52(3) . ? C4 C5 1.45(3) . ? C4 C6 1.59(3) . ? C7 C9 1.49(3) . ? C7 C8 1.51(2) . ? C10 C11 1.47(3) . ? C10 C12 1.48(3) . ? 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 Se3 Hg1 Se2 127.48(6) . . ? Se3 Hg1 Se4 109.11(6) . . ? Se2 Hg1 Se4 116.85(6) . . ? Se3 Hg1 Se1 120.87(7) . . ? Se2 Hg1 Se1 81.55(5) . . ? Se4 Hg1 Se1 92.98(6) . . ? P1 Se1 Hg1 79.01(12) . . ? P1 Se2 Hg1 85.00(13) . . ? P2 Se3 Hg1 97.70(12) . . ? P2 Se4 Hg1 95.89(12) 2_755 . ? O2 P1 O1 100.5(6) . . ? O2 P1 Se1 113.2(5) . . ? O1 P1 Se1 111.6(5) . . ? O2 P1 Se2 106.8(4) . . ? O1 P1 Se2 110.9(4) . . ? Se1 P1 Se2 113.1(2) . . ? O4 P2 O3 102.6(7) . . ? O4 P2 Se4 114.5(5) . 2_745 ? O3 P2 Se4 109.4(5) . 2_745 ? O4 P2 Se3 105.3(5) . . ? O3 P2 Se3 112.6(5) . . ? Se4 P2 Se3 112.19(19) 2_745 . ? C1 O1 P1 119.8(10) . . ? C4 O2 P1 121.3(11) . . ? C7 O3 P2 125.7(11) . . ? C10 O4 P2 128.7(11) . . ? O1 C1 C2 106.6(15) . . ? O1 C1 C3 107.9(15) . . ? C2 C1 C3 112.9(17) . . ? O2 C4 C5 113.2(19) . . ? O2 C4 C6 106.3(18) . . ? C5 C4 C6 108.8(19) . . ? O3 C7 C9 115.0(17) . . ? O3 C7 C8 104.3(16) . . ? C9 C7 C8 114.4(19) . . ? O4 C10 C11 111.9(17) . . ? O4 C10 C12 106.6(17) . . ? C11 C10 C12 113(2) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 22.49 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.062 _refine_diff_density_min -2.385 _refine_diff_density_rms 0.292 #===END data_10 _database_code_depnum_ccdc_archive 'CCDC 279622' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H60 O13 P6 Se12 Zn4' _chemical_formula_weight 1951.54 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 21.2128(16) _cell_length_b 21.2128(16) _cell_length_c 11.5527(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4502.0(8) _cell_formula_units_Z 3 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 777 _cell_measurement_theta_min 2.83 _cell_measurement_theta_max 24.93 _exptl_crystal_description column _exptl_crystal_colour white _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.159 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2778 _exptl_absorpt_coefficient_mu 9.060 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5810 _exptl_absorpt_correction_T_max 0.9700 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4430 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0268 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.02 _reflns_number_total 1703 _reflns_number_gt 1361 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0534P)^2^+27.7327P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1703 _refine_ls_number_parameters 96 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0561 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1118 _refine_ls_wR_factor_gt 0.1055 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 Se1 Se 0.73933(4) 0.28354(4) 0.08113(7) 0.0688(3) Uani 1 1 d . . . Se2 Se 0.86432(3) 0.43643(4) 0.26167(7) 0.0698(3) Uani 1 1 d . . . O3 O 0.6667 0.3333 0.3333 0.0350(18) Uani 1 6 d S . . Zn1 Zn 0.6667 0.3333 0.1595(2) 0.0455(5) Uani 0.50 3 d SP . . Zn2 Zn 0.68282(6) 0.25451(6) 0.27877(12) 0.0441(3) Uani 0.50 1 d P . . P1 P 0.84880(9) 0.36091(10) 0.12794(17) 0.0651(5) Uani 1 1 d . . . O1 O 0.8942(3) 0.3985(3) 0.0176(5) 0.0947(17) Uani 1 1 d . . . O2 O 0.8912(4) 0.3221(4) 0.1743(7) 0.131(3) Uani 1 1 d . . . C1 C 0.8756(6) 0.4393(6) -0.0588(11) 0.125(4) Uani 1 1 d . . . H1A H 0.8285 0.4070 -0.0931 0.150 Uiso 1 1 calc R . . H1B H 0.8713 0.4758 -0.0145 0.150 Uiso 1 1 calc R . . C2 C 0.9272(6) 0.4742(8) -0.1483(9) 0.163(6) Uani 1 1 d . . . H2A H 0.9113 0.4999 -0.1979 0.245 Uiso 1 1 calc R . . H2B H 0.9318 0.4384 -0.1927 0.245 Uiso 1 1 calc R . . H2C H 0.9735 0.5080 -0.1151 0.245 Uiso 1 1 calc R . . C3 C 0.9056(9) 0.2771(9) 0.1358(14) 0.183(7) Uani 1 1 d . . . H3A H 0.9246 0.2929 0.0584 0.219 Uiso 1 1 calc R . . H3B H 0.8597 0.2320 0.1274 0.219 Uiso 1 1 calc R . . C4 C 0.9540(7) 0.2600(7) 0.1935(12) 0.158(5) Uani 1 1 d . . . H4A H 0.9559 0.2214 0.1529 0.236 Uiso 1 1 calc R . . H4B H 0.9373 0.2447 0.2712 0.236 Uiso 1 1 calc R . . H4C H 1.0018 0.3022 0.1954 0.236 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 Se1 0.0612(4) 0.0691(4) 0.0729(5) -0.0108(3) 0.0106(3) 0.0303(3) Se2 0.0442(4) 0.0733(5) 0.0803(6) -0.0032(4) 0.0075(3) 0.0207(3) O3 0.031(2) 0.031(2) 0.042(5) 0.000 0.000 0.0157(12) Zn1 0.0461(7) 0.0461(7) 0.0442(13) 0.000 0.000 0.0231(4) Zn2 0.0441(7) 0.0382(6) 0.0529(8) -0.0020(5) 0.0003(6) 0.0229(5) P1 0.0526(9) 0.0758(11) 0.0727(12) 0.0096(9) 0.0191(8) 0.0364(9) O1 0.076(3) 0.112(4) 0.084(4) 0.017(3) 0.026(3) 0.038(3) O2 0.125(5) 0.154(6) 0.173(7) 0.039(5) 0.037(5) 0.113(5) C1 0.110(7) 0.130(9) 0.157(10) 0.065(8) 0.041(7) 0.076(7) C2 0.083(7) 0.241(15) 0.100(8) 0.072(9) 0.017(6) 0.032(8) C3 0.217(16) 0.214(15) 0.208(16) 0.063(12) 0.063(13) 0.176(14) C4 0.169(11) 0.171(12) 0.210(13) -0.044(10) -0.053(10) 0.143(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 Se1 P1 2.137(2) . ? Se1 Zn1 2.4369(11) . ? Se1 Zn2 2.5083(15) . ? Se2 P1 2.129(2) . ? Se2 Zn2 2.4473(14) 2_655 ? Se2 Zn2 2.5009(14) 18_545 ? O3 Zn2 1.9706(12) 16_655 ? O3 Zn2 1.9707(12) . ? O3 Zn2 1.9707(12) 2_655 ? O3 Zn2 1.9707(12) 17 ? O3 Zn2 1.9707(12) 3_665 ? O3 Zn2 1.9708(12) 18_545 ? O3 Zn1 2.009(2) 16_655 ? O3 Zn1 2.009(2) . ? Zn1 Zn2 2.3208(18) . ? Zn1 Zn2 2.3208(18) 2_655 ? Zn1 Zn2 2.3208(18) 3_665 ? Zn1 Se1 2.4369(11) 3_665 ? Zn1 Se1 2.4369(11) 2_655 ? Zn2 Zn2 2.2529(18) 17 ? Zn2 Zn2 2.2529(18) 18_545 ? Zn2 Se2 2.4473(14) 3_665 ? Zn2 Se2 2.5010(14) 17 ? P1 O1 1.556(5) . ? P1 O2 1.587(6) . ? O1 C1 1.422(10) . ? O2 C3 1.220(14) . ? C1 C2 1.416(13) . ? C3 C4 1.417(16) . ? 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 P1 Se1 Zn1 104.66(6) . . ? P1 Se1 Zn2 99.24(6) . . ? Zn1 Se1 Zn2 55.96(5) . . ? P1 Se2 Zn2 103.85(6) . 2_655 ? P1 Se2 Zn2 96.79(6) . 18_545 ? Zn2 Se2 Zn2 54.16(5) 2_655 18_545 ? Zn2 O3 Zn2 180.00(7) 16_655 . ? Zn2 O3 Zn2 69.72(4) 16_655 2_655 ? Zn2 O3 Zn2 110.27(4) . 2_655 ? Zn2 O3 Zn2 110.28(4) 16_655 17 ? Zn2 O3 Zn2 69.72(4) . 17 ? Zn2 O3 Zn2 180.0 2_655 17 ? Zn2 O3 Zn2 69.73(4) 16_655 3_665 ? Zn2 O3 Zn2 110.27(4) . 3_665 ? Zn2 O3 Zn2 110.27(4) 2_655 3_665 ? Zn2 O3 Zn2 69.73(4) 17 3_665 ? Zn2 O3 Zn2 110.28(4) 16_655 18_545 ? Zn2 O3 Zn2 69.72(4) . 18_545 ? Zn2 O3 Zn2 69.73(4) 2_655 18_545 ? Zn2 O3 Zn2 110.27(4) 17 18_545 ? Zn2 O3 Zn2 180.0 3_665 18_545 ? Zn2 O3 Zn1 71.35(4) 16_655 16_655 ? Zn2 O3 Zn1 108.65(4) . 16_655 ? Zn2 O3 Zn1 108.66(4) 2_655 16_655 ? Zn2 O3 Zn1 71.35(4) 17 16_655 ? Zn2 O3 Zn1 108.66(4) 3_665 16_655 ? Zn2 O3 Zn1 71.34(4) 18_545 16_655 ? Zn2 O3 Zn1 108.66(4) 16_655 . ? Zn2 O3 Zn1 71.34(4) . . ? Zn2 O3 Zn1 71.34(4) 2_655 . ? Zn2 O3 Zn1 108.65(4) 17 . ? Zn2 O3 Zn1 71.34(4) 3_665 . ? Zn2 O3 Zn1 108.65(4) 18_545 . ? Zn1 O3 Zn1 180.0 16_655 . ? O3 Zn1 Zn2 53.57(5) . . ? O3 Zn1 Zn2 53.57(5) . 2_655 ? Zn2 Zn1 Zn2 88.33(8) . 2_655 ? O3 Zn1 Zn2 53.57(5) . 3_665 ? Zn2 Zn1 Zn2 88.33(8) . 3_665 ? Zn2 Zn1 Zn2 88.33(8) 2_655 3_665 ? O3 Zn1 Se1 111.80(5) . . ? Zn2 Zn1 Se1 63.58(4) . . ? Zn2 Zn1 Se1 105.04(4) 2_655 . ? Zn2 Zn1 Se1 147.90(5) 3_665 . ? O3 Zn1 Se1 111.80(5) . 3_665 ? Zn2 Zn1 Se1 105.04(4) . 3_665 ? Zn2 Zn1 Se1 147.90(5) 2_655 3_665 ? Zn2 Zn1 Se1 63.58(4) 3_665 3_665 ? Se1 Zn1 Se1 107.05(6) . 3_665 ? O3 Zn1 Se1 111.80(5) . 2_655 ? Zn2 Zn1 Se1 147.90(5) . 2_655 ? Zn2 Zn1 Se1 63.58(4) 2_655 2_655 ? Zn2 Zn1 Se1 105.04(4) 3_665 2_655 ? Se1 Zn1 Se1 107.05(6) . 2_655 ? Se1 Zn1 Se1 107.05(6) 3_665 2_655 ? O3 Zn2 Zn2 55.139(19) . 17 ? O3 Zn2 Zn2 55.140(19) . 18_545 ? Zn2 Zn2 Zn2 91.74(8) 17 18_545 ? O3 Zn2 Zn1 55.09(5) . . ? Zn2 Zn2 Zn1 89.94(5) 17 . ? Zn2 Zn2 Zn1 89.94(5) 18_545 . ? O3 Zn2 Se2 114.54(6) . 3_665 ? Zn2 Zn2 Se2 64.14(5) 17 3_665 ? Zn2 Zn2 Se2 150.14(9) 18_545 3_665 ? Zn1 Zn2 Se2 106.43(5) . 3_665 ? O3 Zn2 Se2 112.30(6) . 17 ? Zn2 Zn2 Se2 108.45(9) 17 17 ? Zn2 Zn2 Se2 61.71(6) 18_545 17 ? Zn1 Zn2 Se2 145.78(6) . 17 ? Se2 Zn2 Se2 107.55(5) 3_665 17 ? O3 Zn2 Se1 110.33(6) . . ? Zn2 Zn2 Se1 145.90(8) 17 . ? Zn2 Zn2 Se1 103.88(6) 18_545 . ? Zn1 Zn2 Se1 60.47(5) . . ? Se2 Zn2 Se1 105.91(5) 3_665 . ? Se2 Zn2 Se1 105.65(5) 17 . ? O1 P1 O2 100.2(4) . . ? O1 P1 Se2 112.7(2) . . ? O2 P1 Se2 103.4(3) . . ? O1 P1 Se1 110.0(2) . . ? O2 P1 Se1 111.6(3) . . ? Se2 P1 Se1 117.47(8) . . ? C1 O1 P1 122.1(6) . . ? C3 O2 P1 135.3(11) . . ? C2 C1 O1 113.2(9) . . ? O2 C3 C4 121.7(16) . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 0.834 _refine_diff_density_min -0.634 _refine_diff_density_rms 0.095 #===END data_compound_2 _database_code_depnum_ccdc_archive 'CCDC 279623' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H84 O13 P6 Se12 Zn4' _chemical_formula_weight 2119.85 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 22.7200(3) _cell_length_b 22.7200(3) _cell_length_c 11.9987(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5363.9(2) _cell_formula_units_Z 3 _cell_measurement_temperature 566(2) _cell_measurement_reflns_used 3212 _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 20.49 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.969 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3066 _exptl_absorpt_coefficient_mu 7.612 _exptl_absorpt_correction_type SADBS _exptl_absorpt_correction_T_min 0.5156 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 566(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10353 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 24.96 _reflns_number_total 2106 _reflns_number_gt 1423 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^+93.3060P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00044(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2106 _refine_ls_number_parameters 107 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0918 _refine_ls_R_factor_gt 0.0666 _refine_ls_wR_factor_ref 0.1333 _refine_ls_wR_factor_gt 0.1276 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.033 _refine_ls_shift/su_mean 0.005 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 -0.01142(10) 0.91256(9) 0.05310(17) 0.0768(6) Uani 0.50 1 d P . . Zn2 Zn 0.0000 1.0000 0.1673(3) 0.0762(9) Uani 0.50 3 d SP . . Se1 Se 0.09737(6) 0.91319(6) 0.06718(11) 0.1153(5) Uani 1 1 d . . . Se2 Se -0.06425(6) 0.88472(6) 0.24263(11) 0.1199(5) Uani 1 1 d . . . P1 P 0.14322(16) 0.97793(19) 0.2056(3) 0.1184(11) Uani 1 1 d D . . O1 O 0.0000 1.0000 0.0000 0.052(3) Uani 1 6 d S . . O2 O 0.1538(7) 0.9450(7) 0.3108(11) 0.104(4) Uiso 0.50 1 d PD A 1 O3 O 0.2356(10) 1.0387(12) 0.173(2) 0.169(8) Uiso 0.50 1 d PD A 1 C1 C 0.1048(13) 0.9233(15) 0.3987(19) 0.179(15) Uiso 0.50 1 d PD A 1 C2 C 0.1038(17) 0.8553(9) 0.406(2) 0.26(2) Uiso 0.50 1 d PD A 1 C3 C 0.1493(17) 0.8784(16) 0.510(2) 0.159(11) Uiso 0.50 1 d PD A 1 C4 C 0.2884(15) 1.031(3) 0.224(4) 0.53(6) Uiso 0.50 1 d PD A 1 C5 C 0.3418(10) 1.0916(13) 0.155(3) 0.178(13) Uiso 0.50 1 d PD A 1 C6 C 0.3823(15) 1.0550(17) 0.133(3) 0.176(14) Uiso 0.50 1 d PD A 1 O2' O 0.1030(12) 0.9051(11) 0.3179(18) 0.175(8) Uiso 0.50 1 d PD A 2 O3' O 0.2207(8) 1.0013(12) 0.2032(16) 0.181(9) Uiso 0.50 1 d PD A 2 C1' C 0.081(2) 0.907(2) 0.429(2) 0.33(3) Uiso 0.50 1 d PD A 2 C2' C 0.1417(19) 0.9020(16) 0.476(3) 0.27(2) Uiso 0.50 1 d PD A 2 C3' C 0.0982(16) 0.8244(15) 0.487(3) 0.160(10) Uiso 0.50 1 d PD A 2 C4' C 0.2705(5) 1.0268(19) 0.1163(16) 0.209(15) Uiso 0.50 1 d PD A 2 C5' C 0.3276(8) 1.052(2) 0.203(2) 0.228(18) Uiso 0.50 1 d PD A 2 C6' C 0.3823(7) 1.091(2) 0.114(3) 0.219(17) Uiso 0.50 1 d PD A 2 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 0.0773(12) 0.0670(11) 0.0885(14) 0.0047(10) 0.0011(10) 0.0379(10) Zn2 0.0744(13) 0.0744(13) 0.080(2) 0.000 0.000 0.0372(6) Se1 0.1166(9) 0.1183(9) 0.1416(11) -0.0060(7) -0.0190(7) 0.0816(8) Se2 0.1158(9) 0.1220(10) 0.1208(10) 0.0427(7) 0.0207(7) 0.0585(8) P1 0.105(2) 0.155(3) 0.113(2) 0.019(2) -0.0140(18) 0.079(2) O1 0.048(4) 0.048(4) 0.061(7) 0.000 0.000 0.0239(18) _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 O1 1.9760(18) . ? Zn1 Zn1 2.263(3) 12_665 ? Zn1 Zn1 2.263(3) 11_455 ? Zn1 Zn2 2.318(3) . ? Zn1 Se1 2.466(2) 11_455 ? Zn1 Se1 2.471(2) . ? Zn1 Se2 2.501(2) . ? Zn2 O1 2.007(3) . ? Zn2 Zn1 2.318(3) 3_465 ? Zn2 Zn1 2.318(3) 2_675 ? Zn2 Se2 2.4466(17) 2_675 ? Zn2 Se2 2.4466(17) 3_465 ? Zn2 Se2 2.4466(17) . ? Se1 P1 2.116(4) . ? Se1 Zn1 2.466(2) 12_665 ? Se2 P1 2.101(4) 3_465 ? P1 O2 1.546(13) . ? P1 O3' 1.565(15) . ? P1 O3 1.89(2) . ? P1 O2' 1.97(2) . ? P1 Se2 2.101(4) 2_675 ? O1 Zn1 1.9760(18) 2_675 ? O1 Zn1 1.9760(18) 3_465 ? O1 Zn1 1.9760(18) 10_575 ? O1 Zn1 1.9760(18) 11_455 ? O1 Zn1 1.9760(18) 12_665 ? O1 Zn2 2.007(3) 10_575 ? O2 C1 1.430(5) . ? O3 C4 1.427(5) . ? C1 C2 1.536(5) . ? C2 C3 1.537(5) . ? C4 C5 1.540(5) . ? C5 C6 1.540(5) . ? O2' C1' 1.428(5) . ? O3' C4' 1.430(5) . ? C1' C2' 1.540(5) . ? C2' C3' 1.536(5) . ? C4' C5' 1.538(5) . ? C5' C6' 1.539(5) . ? 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 Zn1 Zn1 55.06(3) . 12_665 ? O1 Zn1 Zn1 55.06(3) . 11_455 ? Zn1 Zn1 Zn1 91.41(13) 12_665 11_455 ? O1 Zn1 Zn2 55.02(8) . . ? Zn1 Zn1 Zn2 89.96(7) 12_665 . ? Zn1 Zn1 Zn2 89.96(7) 11_455 . ? O1 Zn1 Se1 113.01(9) . 11_455 ? Zn1 Zn1 Se1 107.71(13) 12_665 11_455 ? Zn1 Zn1 Se1 62.81(9) 11_455 11_455 ? Zn2 Zn1 Se1 147.11(9) . 11_455 ? O1 Zn1 Se1 112.84(9) . . ? Zn1 Zn1 Se1 62.62(8) 12_665 . ? Zn1 Zn1 Se1 148.93(14) 11_455 . ? Zn2 Zn1 Se1 105.76(9) . . ? Se1 Zn1 Se1 106.99(8) 11_455 . ? O1 Zn1 Se2 110.65(9) . . ? Zn1 Zn1 Se2 146.32(12) 12_665 . ? Zn1 Zn1 Se2 104.11(10) 11_455 . ? Zn2 Zn1 Se2 60.88(8) . . ? Se1 Zn1 Se2 105.97(8) 11_455 . ? Se1 Zn1 Se2 106.95(9) . . ? O1 Zn2 Zn1 53.78(8) . 3_465 ? O1 Zn2 Zn1 53.78(8) . . ? Zn1 Zn2 Zn1 88.65(12) 3_465 . ? O1 Zn2 Zn1 53.78(8) . 2_675 ? Zn1 Zn2 Zn1 88.65(12) 3_465 2_675 ? Zn1 Zn2 Zn1 88.65(12) . 2_675 ? O1 Zn2 Se2 111.70(8) . 2_675 ? Zn1 Zn2 Se2 147.81(9) 3_465 2_675 ? Zn1 Zn2 Se2 105.02(6) . 2_675 ? Zn1 Zn2 Se2 63.24(6) 2_675 2_675 ? O1 Zn2 Se2 111.70(8) . 3_465 ? Zn1 Zn2 Se2 63.24(6) 3_465 3_465 ? Zn1 Zn2 Se2 147.81(9) . 3_465 ? Zn1 Zn2 Se2 105.02(6) 2_675 3_465 ? Se2 Zn2 Se2 107.16(9) 2_675 3_465 ? O1 Zn2 Se2 111.70(8) . . ? Zn1 Zn2 Se2 105.02(6) 3_465 . ? Zn1 Zn2 Se2 63.24(6) . . ? Zn1 Zn2 Se2 147.81(9) 2_675 . ? Se2 Zn2 Se2 107.16(9) 2_675 . ? Se2 Zn2 Se2 107.16(9) 3_465 . ? P1 Se1 Zn1 100.14(10) . 12_665 ? P1 Se1 Zn1 101.60(10) . . ? Zn1 Se1 Zn1 54.57(8) 12_665 . ? P1 Se2 Zn2 102.84(10) 3_465 . ? P1 Se2 Zn1 101.42(11) 3_465 . ? Zn2 Se2 Zn1 55.88(8) . . ? O2 P1 O3' 76.1(9) . . ? O2 P1 O3 98.1(9) . . ? O3' P1 O3 25.6(10) . . ? O2 P1 O2' 32.2(7) . . ? O3' P1 O2' 105.6(10) . . ? O3 P1 O2' 129.5(10) . . ? O2 P1 Se2 113.1(5) . 2_675 ? O3' P1 Se2 118.0(10) . 2_675 ? O3 P1 Se2 97.5(7) . 2_675 ? O2' P1 Se2 108.8(7) . 2_675 ? O2 P1 Se1 116.5(6) . . ? O3' P1 Se1 107.5(9) . . ? O3 P1 Se1 109.0(7) . . ? O2' P1 Se1 95.3(6) . . ? Se2 P1 Se1 118.51(13) 2_675 . ? Zn1 O1 Zn1 110.13(6) 2_675 3_465 ? Zn1 O1 Zn1 69.87(6) 2_675 10_575 ? Zn1 O1 Zn1 69.87(6) 3_465 10_575 ? Zn1 O1 Zn1 180.0 2_675 11_455 ? Zn1 O1 Zn1 69.87(6) 3_465 11_455 ? Zn1 O1 Zn1 110.13(6) 10_575 11_455 ? Zn1 O1 Zn1 69.87(6) 2_675 12_665 ? Zn1 O1 Zn1 180.0 3_465 12_665 ? Zn1 O1 Zn1 110.13(6) 10_575 12_665 ? Zn1 O1 Zn1 110.13(6) 11_455 12_665 ? Zn1 O1 Zn1 110.13(6) 2_675 . ? Zn1 O1 Zn1 110.13(6) 3_465 . ? Zn1 O1 Zn1 180.00(11) 10_575 . ? Zn1 O1 Zn1 69.87(6) 11_455 . ? Zn1 O1 Zn1 69.87(6) 12_665 . ? Zn1 O1 Zn2 108.81(6) 2_675 10_575 ? Zn1 O1 Zn2 108.81(6) 3_465 10_575 ? Zn1 O1 Zn2 71.19(6) 10_575 10_575 ? Zn1 O1 Zn2 71.19(6) 11_455 10_575 ? Zn1 O1 Zn2 71.19(6) 12_665 10_575 ? Zn1 O1 Zn2 108.81(6) . 10_575 ? Zn1 O1 Zn2 71.19(6) 2_675 . ? Zn1 O1 Zn2 71.19(6) 3_465 . ? Zn1 O1 Zn2 108.81(6) 10_575 . ? Zn1 O1 Zn2 108.81(6) 11_455 . ? Zn1 O1 Zn2 108.81(6) 12_665 . ? Zn1 O1 Zn2 71.19(6) . . ? Zn2 O1 Zn2 180.000(1) 10_575 . ? C1 O2 P1 119.0(14) . . ? C4 O3 P1 121.1(17) . . ? O2 C1 C2 90.4(4) . . ? C1 C2 C3 92.1(4) . . ? O3 C4 C5 90.1(4) . . ? C6 C5 C4 91.6(4) . . ? C1' O2' P1 130(2) . . ? C4' O3' P1 132.7(13) . . ? O2' C1' C2' 90.1(4) . . ? C3' C2' C1' 91.8(4) . . ? O3' C4' C5' 90.2(4) . . ? C4' C5' C6' 91.8(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.96 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.826 _refine_diff_density_min -0.536 _refine_diff_density_rms 0.112 #===END data_12 _database_code_depnum_ccdc_archive 'CCDC 279624' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H84 O13 P6 Se12 Zn4' _chemical_formula_weight 2119.85 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 '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 12.891(2) _cell_length_b 13.336(2) _cell_length_c 13.584(2) _cell_angle_alpha 112.847(3) _cell_angle_beta 105.662(3) _cell_angle_gamma 108.246(3) _cell_volume 1827.9(5) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 880 _cell_measurement_theta_min 3.11 _cell_measurement_theta_max 24.70 _exptl_crystal_description Column _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.926 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1022 _exptl_absorpt_coefficient_mu 7.446 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3495 _exptl_absorpt_correction_T_max 0.9633 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9394 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0391 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 25.09 _reflns_number_total 6365 _reflns_number_gt 4437 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0675P)^2^+10.5082P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6365 _refine_ls_number_parameters 340 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0914 _refine_ls_R_factor_gt 0.0599 _refine_ls_wR_factor_ref 0.1680 _refine_ls_wR_factor_gt 0.1441 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 0.83986(18) 0.49659(19) 0.48523(18) 0.0567(5) Uani 0.50 1 d P . . Zn2 Zn 0.99487(19) 0.44252(18) 0.34084(17) 0.0536(5) Uani 0.50 1 d P . . Zn3 Zn 1.13282(18) 0.67049(18) 0.61277(17) 0.0546(5) Uani 0.50 1 d P . . Zn4 Zn 1.02006(18) 0.38830(17) 0.55709(17) 0.0520(5) Uani 0.50 1 d P . . Se1 Se 1.17558(11) 0.78994(10) 0.51252(11) 0.0788(3) Uani 1 1 d . . . Se2 Se 1.20681(12) 0.51785(11) 0.35820(11) 0.0844(4) Uani 1 1 d . . . Se3 Se 0.87898(9) 0.51872(9) 0.22989(9) 0.0669(3) Uani 1 1 d . . . Se4 Se 0.66882(9) 0.32050(11) 0.28824(10) 0.0768(3) Uani 1 1 d . . . Se5 Se 0.85142(11) 0.69748(11) 0.50806(10) 0.0793(3) Uani 1 1 d . . . Se6 Se 1.10276(13) 0.78736(11) 0.77884(10) 0.0930(4) Uani 1 1 d . . . P1 P 1.2565(3) 0.7054(3) 0.4127(3) 0.0843(9) Uani 1 1 d . . . P2 P 0.6994(2) 0.3786(2) 0.1669(2) 0.0635(6) Uani 1 1 d . . . P3 P 0.9517(4) 0.8108(3) 0.6964(3) 0.0879(10) Uani 1 1 d . . . O1 O 1.0000 0.5000 0.5000 0.0397(15) Uani 1 2 d S . . O2 O 1.3994(10) 0.7845(12) 0.5010(17) 0.207(8) Uani 1 1 d . . . O3 O 1.244(2) 0.7260(12) 0.3107(14) 0.218(9) Uani 1 1 d . . . O4 O 0.6729(7) 0.2693(6) 0.0451(6) 0.083(2) Uani 1 1 d . . . O5 O 0.6001(7) 0.4159(8) 0.1218(7) 0.085(2) Uani 1 1 d . . . O6 O 0.8558(10) 0.7848(10) 0.7495(8) 0.118(3) Uani 1 1 d . . . O7 O 0.9847(12) 0.9474(8) 0.7359(8) 0.129(4) Uani 1 1 d . . . C1 C 1.500(2) 0.764(3) 0.499(2) 0.34(3) Uani 1 1 d D . . H1A H 1.4735 0.6904 0.4235 0.405 Uiso 1 1 calc R . . C2 C 1.578(5) 0.759(8) 0.605(5) 1.01(15) Uani 1 1 d D . . H2A H 1.5271 0.6915 0.6087 1.518 Uiso 1 1 calc R . . H2B H 1.6097 0.8347 0.6783 1.518 Uiso 1 1 calc R . . H2C H 1.6437 0.7468 0.5928 1.518 Uiso 1 1 calc R . . C3 C 1.580(2) 0.883(4) 0.501(4) 0.39(3) Uani 1 1 d . . . H3A H 1.5284 0.8986 0.4493 0.585 Uiso 1 1 calc R . . H3B H 1.6386 0.8700 0.4730 0.585 Uiso 1 1 calc R . . H3C H 1.6227 0.9532 0.5806 0.585 Uiso 1 1 calc R . . C4 C 1.1711(14) 0.6480(19) 0.1839(17) 0.133(6) Uani 1 1 d . . . H4A H 1.1011 0.5773 0.1687 0.160 Uiso 1 1 calc R . . C5 C 1.123(2) 0.716(3) 0.136(3) 0.248(15) Uani 1 1 d . . . H5A H 1.0768 0.7424 0.1755 0.373 Uiso 1 1 calc R . . H5B H 1.0711 0.6620 0.0520 0.373 Uiso 1 1 calc R . . H5C H 1.1898 0.7860 0.1507 0.373 Uiso 1 1 calc R . . C6 C 1.239(2) 0.600(2) 0.1261(18) 0.200(11) Uani 1 1 d . . . H6A H 1.2645 0.5547 0.1576 0.301 Uiso 1 1 calc R . . H6B H 1.3088 0.6679 0.1408 0.301 Uiso 1 1 calc R . . H6C H 1.1871 0.5473 0.0417 0.301 Uiso 1 1 calc R . . C7 C 0.5646(13) 0.1491(12) -0.0225(13) 0.112(5) Uani 1 1 d . . . H7A H 0.5362 0.1306 0.0315 0.135 Uiso 1 1 calc R . . C8 C 0.6034(18) 0.0585(14) -0.0833(16) 0.164(8) Uani 1 1 d . . . H8A H 0.5355 -0.0231 -0.1289 0.245 Uiso 1 1 calc R . . H8B H 0.6685 0.0625 -0.0246 0.245 Uiso 1 1 calc R . . H8C H 0.6313 0.0779 -0.1356 0.245 Uiso 1 1 calc R . . C9 C 0.471(2) 0.144(2) -0.110(3) 0.35(3) Uani 1 1 d . . . H9A H 0.4446 0.2017 -0.0711 0.531 Uiso 1 1 calc R . . H9B H 0.4028 0.0621 -0.1565 0.531 Uiso 1 1 calc R . . H9C H 0.5001 0.1643 -0.1605 0.531 Uiso 1 1 calc R . . C10 C 0.5729(14) 0.5013(14) 0.2032(12) 0.109(4) Uani 1 1 d . . . H10A H 0.6215 0.5263 0.2858 0.131 Uiso 1 1 calc R . . C11 C 0.605(2) 0.6129(18) 0.189(2) 0.193(10) Uani 1 1 d . . . H11A H 0.6911 0.6526 0.2117 0.290 Uiso 1 1 calc R . . H11B H 0.5849 0.6697 0.2385 0.290 Uiso 1 1 calc R . . H11C H 0.5599 0.5868 0.1068 0.290 Uiso 1 1 calc R . . C12 C 0.4412(18) 0.436(3) 0.169(2) 0.226(13) Uani 1 1 d . . . H12A H 0.4242 0.3667 0.1791 0.339 Uiso 1 1 calc R . . H12B H 0.3947 0.4085 0.0865 0.339 Uiso 1 1 calc R . . H12C H 0.4193 0.4916 0.2180 0.339 Uiso 1 1 calc R . . C13 C 0.896(3) 0.859(2) 0.869(2) 0.204(12) Uani 1 1 d . . . H13A H 0.9752 0.9322 0.9056 0.245 Uiso 1 1 calc R . . C14 C 0.900(3) 0.780(2) 0.9286(19) 0.219(12) Uani 1 1 d . . . H14A H 0.9667 0.7618 0.9302 0.328 Uiso 1 1 calc R . . H14B H 0.8247 0.7043 0.8833 0.328 Uiso 1 1 calc R . . H14C H 0.9110 0.8251 1.0087 0.328 Uiso 1 1 calc R . . C15 C 0.788(3) 0.895(2) 0.874(2) 0.230(13) Uani 1 1 d . . . H15A H 0.7861 0.9459 0.8396 0.345 Uiso 1 1 calc R . . H15B H 0.8025 0.9396 0.9554 0.345 Uiso 1 1 calc R . . H15C H 0.7110 0.8213 0.8294 0.345 Uiso 1 1 calc R . . C16 C 1.047(2) 1.0128(16) 0.691(2) 0.155(8) Uani 1 1 d . . . H16A H 1.0485 0.9549 0.6206 0.185 Uiso 1 1 calc R . . C17 C 1.164(3) 1.098(3) 0.778(4) 0.37(3) Uani 1 1 d . . . H17A H 1.2058 1.1437 0.7486 0.549 Uiso 1 1 calc R . . H17B H 1.2066 1.0558 0.7986 0.549 Uiso 1 1 calc R . . H17C H 1.1622 1.1532 0.8475 0.549 Uiso 1 1 calc R . . C18 C 0.998(3) 1.079(3) 0.663(3) 0.31(2) Uani 1 1 d . . . H18A H 1.0417 1.1179 0.6300 0.465 Uiso 1 1 calc R . . H18B H 1.0038 1.1415 0.7341 0.465 Uiso 1 1 calc R . . H18C H 0.9138 1.0261 0.6059 0.465 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 0.0586(11) 0.0625(12) 0.0562(12) 0.0295(10) 0.0310(10) 0.0335(10) Zn2 0.0662(12) 0.0531(11) 0.0465(10) 0.0233(9) 0.0299(9) 0.0326(10) Zn3 0.0609(11) 0.0466(10) 0.0508(11) 0.0219(9) 0.0246(9) 0.0239(9) Zn4 0.0608(11) 0.0485(10) 0.0509(11) 0.0251(9) 0.0275(9) 0.0289(9) Se1 0.0955(8) 0.0644(6) 0.0928(8) 0.0451(6) 0.0554(7) 0.0386(6) Se2 0.1081(9) 0.0926(8) 0.0893(8) 0.0525(7) 0.0679(7) 0.0605(7) Se3 0.0651(6) 0.0694(6) 0.0591(6) 0.0346(5) 0.0273(5) 0.0222(5) Se4 0.0620(6) 0.0905(8) 0.0728(7) 0.0520(6) 0.0267(5) 0.0208(5) Se5 0.0921(8) 0.0792(7) 0.0742(7) 0.0346(6) 0.0350(6) 0.0572(6) Se6 0.1115(9) 0.0780(7) 0.0594(6) 0.0132(6) 0.0251(6) 0.0510(7) P1 0.0796(19) 0.0789(19) 0.094(2) 0.0419(17) 0.0559(17) 0.0262(15) P2 0.0578(14) 0.0677(15) 0.0594(14) 0.0359(13) 0.0220(11) 0.0232(12) P3 0.150(3) 0.0807(19) 0.0648(17) 0.0369(15) 0.0572(19) 0.082(2) O1 0.045(4) 0.035(4) 0.033(4) 0.013(3) 0.017(3) 0.018(3) O2 0.081(7) 0.147(11) 0.32(2) 0.075(12) 0.088(10) 0.034(7) O3 0.47(3) 0.140(10) 0.186(13) 0.129(11) 0.234(17) 0.166(15) O4 0.086(5) 0.063(4) 0.063(4) 0.026(4) 0.022(4) 0.012(4) O5 0.077(5) 0.108(6) 0.080(5) 0.058(5) 0.028(4) 0.047(4) O6 0.178(9) 0.155(8) 0.085(6) 0.066(6) 0.082(6) 0.125(8) O7 0.200(11) 0.077(6) 0.096(6) 0.030(5) 0.059(7) 0.075(7) C1 0.117(17) 0.43(5) 0.136(19) -0.01(2) 0.081(16) -0.07(2) C2 0.47(10) 1.4(3) 0.32(7) 0.13(11) 0.32(8) -0.13(13) C3 0.12(2) 0.45(6) 0.63(9) 0.37(6) 0.15(4) 0.07(3) C4 0.099(10) 0.185(18) 0.135(14) 0.112(14) 0.046(10) 0.056(11) C5 0.24(3) 0.40(4) 0.35(4) 0.32(4) 0.19(3) 0.22(3) C6 0.27(3) 0.31(3) 0.142(16) 0.15(2) 0.15(2) 0.18(3) C7 0.097(9) 0.075(8) 0.097(9) 0.030(7) 0.018(8) 0.005(7) C8 0.20(2) 0.072(9) 0.127(14) 0.013(9) 0.050(14) 0.038(11) C9 0.17(2) 0.121(17) 0.39(4) 0.01(2) -0.15(3) 0.026(15) C10 0.118(11) 0.126(12) 0.081(9) 0.045(8) 0.036(8) 0.072(10) C11 0.26(3) 0.140(16) 0.20(2) 0.084(17) 0.09(2) 0.136(19) C12 0.123(16) 0.31(3) 0.26(3) 0.12(3) 0.107(19) 0.13(2) C13 0.37(4) 0.22(2) 0.17(2) 0.12(2) 0.18(2) 0.22(3) C14 0.31(3) 0.20(2) 0.118(16) 0.079(17) 0.084(19) 0.09(2) C15 0.38(4) 0.28(3) 0.25(3) 0.16(2) 0.24(3) 0.27(3) C16 0.176(19) 0.093(11) 0.169(18) 0.047(12) 0.109(16) 0.035(12) C17 0.17(3) 0.25(4) 0.62(8) 0.25(5) 0.13(4) 0.05(3) C18 0.42(5) 0.20(3) 0.31(4) 0.18(3) 0.06(4) 0.18(3) _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 O1 2.004(2) . ? Zn1 Zn3 2.303(3) 2_766 ? Zn1 Zn4 2.336(3) 2_766 ? Zn1 Zn2 2.343(3) 2_766 ? Zn1 Se2 2.421(2) 2_766 ? Zn1 Se4 2.496(2) . ? Zn1 Se5 2.525(2) . ? Zn2 O1 1.9674(18) . ? Zn2 Zn4 2.244(3) 2_766 ? Zn2 Zn3 2.263(3) 2_766 ? Zn2 Zn1 2.343(3) 2_766 ? Zn2 Se6 2.497(2) 2_766 ? Zn2 Se2 2.506(2) . ? Zn2 Se3 2.542(2) . ? Zn3 O1 1.9721(19) . ? Zn3 Zn4 2.235(3) 2_766 ? Zn3 Zn2 2.263(3) 2_766 ? Zn3 Zn1 2.303(3) 2_766 ? Zn3 Se6 2.406(2) . ? Zn3 Se4 2.487(2) 2_766 ? Zn3 Se1 2.497(2) . ? Zn4 O1 1.9792(19) . ? Zn4 Zn3 2.235(3) 2_766 ? Zn4 Zn2 2.244(3) 2_766 ? Zn4 Zn1 2.336(3) 2_766 ? Zn4 Se3 2.403(2) 2_766 ? Zn4 Se5 2.455(2) 2_766 ? Zn4 Se1 2.473(2) 2_766 ? Se1 P1 2.125(3) . ? Se1 Zn4 2.473(2) 2_766 ? Se2 P1 2.125(3) . ? Se2 Zn1 2.421(2) 2_766 ? Se3 P2 2.136(3) . ? Se3 Zn4 2.403(2) 2_766 ? Se4 P2 2.151(3) . ? Se4 Zn3 2.487(2) 2_766 ? Se5 P3 2.119(3) . ? Se5 Zn4 2.455(2) 2_766 ? Se6 P3 2.150(4) . ? Se6 Zn2 2.497(2) 2_766 ? P1 O3 1.491(12) . ? P1 O2 1.597(13) . ? P2 O5 1.572(8) . ? P2 O4 1.578(8) . ? P3 O7 1.555(9) . ? P3 O6 1.604(10) . ? O1 Zn2 1.9674(18) 2_766 ? O1 Zn3 1.972(2) 2_766 ? O1 Zn4 1.9792(19) 2_766 ? O1 Zn1 2.004(2) 2_766 ? O2 C1 1.41(3) . ? O3 C4 1.43(2) . ? O4 C7 1.458(13) . ? O5 C10 1.458(15) . ? O6 C13 1.36(2) . ? O7 C16 1.42(2) . ? C1 C2 1.56(4) . ? C1 C3 1.59(5) . ? C4 C6 1.45(2) . ? C4 C5 1.48(2) . ? C7 C9 1.41(3) . ? C7 C8 1.49(2) . ? C10 C12 1.48(2) . ? C10 C11 1.52(2) . ? C13 C14 1.57(3) . ? C13 C15 1.62(3) . ? C16 C18 1.34(3) . ? C16 C17 1.38(4) . ? 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 Zn1 Zn3 53.97(7) . 2_766 ? O1 Zn1 Zn4 53.60(7) . 2_766 ? Zn3 Zn1 Zn4 89.24(9) 2_766 2_766 ? O1 Zn1 Zn2 53.13(7) . 2_766 ? Zn3 Zn1 Zn2 87.90(10) 2_766 2_766 ? Zn4 Zn1 Zn2 87.86(10) 2_766 2_766 ? O1 Zn1 Se2 112.63(9) . 2_766 ? Zn3 Zn1 Se2 107.66(10) 2_766 2_766 ? Zn4 Zn1 Se2 145.27(11) 2_766 2_766 ? Zn2 Zn1 Se2 63.45(8) 2_766 2_766 ? O1 Zn1 Se4 111.16(9) . . ? Zn3 Zn1 Se4 62.29(8) 2_766 . ? Zn4 Zn1 Se4 106.21(9) 2_766 . ? Zn2 Zn1 Se4 146.15(11) 2_766 . ? Se2 Zn1 Se4 108.51(9) 2_766 . ? O1 Zn1 Se5 108.88(9) . . ? Zn3 Zn1 Se5 146.43(11) 2_766 . ? Zn4 Zn1 Se5 60.53(7) 2_766 . ? Zn2 Zn1 Se5 103.97(10) 2_766 . ? Se2 Zn1 Se5 105.73(8) 2_766 . ? Se4 Zn1 Se5 109.77(9) . . ? O1 Zn2 Zn4 55.60(7) . 2_766 ? O1 Zn2 Zn3 55.03(7) . 2_766 ? Zn4 Zn2 Zn3 92.59(10) 2_766 2_766 ? O1 Zn2 Zn1 54.56(7) . 2_766 ? Zn4 Zn2 Zn1 89.34(10) 2_766 2_766 ? Zn3 Zn2 Zn1 89.42(10) 2_766 2_766 ? O1 Zn2 Se6 111.02(9) . 2_766 ? Zn4 Zn2 Se6 148.22(11) 2_766 2_766 ? Zn3 Zn2 Se6 60.48(8) 2_766 2_766 ? Zn1 Zn2 Se6 105.71(10) 2_766 2_766 ? O1 Zn2 Se2 110.52(9) . . ? Zn4 Zn2 Se2 106.10(10) 2_766 . ? Zn3 Zn2 Se2 142.90(11) 2_766 . ? Zn1 Zn2 Se2 59.78(7) 2_766 . ? Se6 Zn2 Se2 105.66(8) 2_766 . ? O1 Zn2 Se3 110.45(8) . . ? Zn4 Zn2 Se3 59.90(7) 2_766 . ? Zn3 Zn2 Se3 107.71(10) 2_766 . ? Zn1 Zn2 Se3 144.60(10) 2_766 . ? Se6 Zn2 Se3 109.69(8) 2_766 . ? Se2 Zn2 Se3 109.38(8) . . ? O1 Zn3 Zn4 55.71(7) . 2_766 ? O1 Zn3 Zn2 54.84(7) . 2_766 ? Zn4 Zn3 Zn2 92.39(10) 2_766 2_766 ? O1 Zn3 Zn1 55.25(7) . 2_766 ? Zn4 Zn3 Zn1 90.60(10) 2_766 2_766 ? Zn2 Zn3 Zn1 89.21(10) 2_766 2_766 ? O1 Zn3 Se6 114.60(10) . . ? Zn4 Zn3 Se6 109.05(10) 2_766 . ? Zn2 Zn3 Se6 64.57(8) 2_766 . ? Zn1 Zn3 Se6 147.09(11) 2_766 . ? O1 Zn3 Se4 112.65(9) . 2_766 ? Zn4 Zn3 Se4 147.90(11) 2_766 2_766 ? Zn2 Zn3 Se4 103.92(10) 2_766 2_766 ? Zn1 Zn3 Se4 62.67(8) 2_766 2_766 ? Se6 Zn3 Se4 102.93(8) . 2_766 ? O1 Zn3 Se1 112.56(9) . . ? Zn4 Zn3 Se1 62.73(8) 2_766 . ? Zn2 Zn3 Se1 151.59(11) 2_766 . ? Zn1 Zn3 Se1 103.69(9) 2_766 . ? Se6 Zn3 Se1 108.72(9) . . ? Se4 Zn3 Se1 104.50(8) 2_766 . ? O1 Zn4 Zn3 55.40(7) . 2_766 ? O1 Zn4 Zn2 55.10(7) . 2_766 ? Zn3 Zn4 Zn2 92.09(10) 2_766 2_766 ? O1 Zn4 Zn1 54.57(7) . 2_766 ? Zn3 Zn4 Zn1 90.28(10) 2_766 2_766 ? Zn2 Zn4 Zn1 88.83(10) 2_766 2_766 ? O1 Zn4 Se3 115.75(9) . 2_766 ? Zn3 Zn4 Se3 153.05(11) 2_766 2_766 ? Zn2 Zn4 Se3 66.21(8) 2_766 2_766 ? Zn1 Zn4 Se3 104.37(9) 2_766 2_766 ? O1 Zn4 Se5 112.49(9) . 2_766 ? Zn3 Zn4 Se5 104.33(9) 2_766 2_766 ? Zn2 Zn4 Se5 147.37(11) 2_766 2_766 ? Zn1 Zn4 Se5 63.54(7) 2_766 2_766 ? Se3 Zn4 Se5 102.45(8) 2_766 2_766 ? O1 Zn4 Se1 113.28(9) . 2_766 ? Zn3 Zn4 Se1 63.83(8) 2_766 2_766 ? Zn2 Zn4 Se1 106.19(10) 2_766 2_766 ? Zn1 Zn4 Se1 149.93(11) 2_766 2_766 ? Se3 Zn4 Se1 105.52(8) 2_766 2_766 ? Se5 Zn4 Se1 106.34(8) 2_766 2_766 ? P1 Se1 Zn4 102.14(10) . 2_766 ? P1 Se1 Zn3 102.27(11) . . ? Zn4 Se1 Zn3 53.44(7) 2_766 . ? P1 Se2 Zn1 101.68(10) . 2_766 ? P1 Se2 Zn2 100.75(10) . . ? Zn1 Se2 Zn2 56.77(7) 2_766 . ? P2 Se3 Zn4 107.29(9) . 2_766 ? P2 Se3 Zn2 97.08(9) . . ? Zn4 Se3 Zn2 53.89(6) 2_766 . ? P2 Se4 Zn3 101.68(9) . 2_766 ? P2 Se4 Zn1 102.40(9) . . ? Zn3 Se4 Zn1 55.04(7) 2_766 . ? P3 Se5 Zn4 105.08(11) . 2_766 ? P3 Se5 Zn1 98.89(10) . . ? Zn4 Se5 Zn1 55.93(7) 2_766 . ? P3 Se6 Zn3 103.16(10) . . ? P3 Se6 Zn2 98.62(11) . 2_766 ? Zn3 Se6 Zn2 54.94(7) . 2_766 ? O3 P1 O2 104.6(11) . . ? O3 P1 Se1 110.6(6) . . ? O2 P1 Se1 104.1(6) . . ? O3 P1 Se2 111.7(5) . . ? O2 P1 Se2 107.3(6) . . ? Se1 P1 Se2 117.42(13) . . ? O5 P2 O4 100.7(4) . . ? O5 P2 Se3 111.2(3) . . ? O4 P2 Se3 105.1(3) . . ? O5 P2 Se4 109.7(3) . . ? O4 P2 Se4 112.8(3) . . ? Se3 P2 Se4 116.30(12) . . ? O7 P3 O6 98.4(6) . . ? O7 P3 Se5 110.1(4) . . ? O6 P3 Se5 106.6(4) . . ? O7 P3 Se6 113.7(5) . . ? O6 P3 Se6 109.8(4) . . ? Se5 P3 Se6 116.48(13) . . ? Zn2 O1 Zn2 180.000(1) . 2_766 ? Zn2 O1 Zn3 109.87(8) . . ? Zn2 O1 Zn3 70.13(8) 2_766 . ? Zn2 O1 Zn3 70.13(8) . 2_766 ? Zn2 O1 Zn3 109.87(8) 2_766 2_766 ? Zn3 O1 Zn3 180.0 . 2_766 ? Zn2 O1 Zn4 69.31(8) . 2_766 ? Zn2 O1 Zn4 110.69(8) 2_766 2_766 ? Zn3 O1 Zn4 68.89(8) . 2_766 ? Zn3 O1 Zn4 111.11(8) 2_766 2_766 ? Zn2 O1 Zn4 110.69(8) . . ? Zn2 O1 Zn4 69.31(8) 2_766 . ? Zn3 O1 Zn4 111.11(8) . . ? Zn3 O1 Zn4 68.89(8) 2_766 . ? Zn4 O1 Zn4 180.000(1) 2_766 . ? Zn2 O1 Zn1 107.68(8) . . ? Zn2 O1 Zn1 72.32(8) 2_766 . ? Zn3 O1 Zn1 109.22(8) . . ? Zn3 O1 Zn1 70.78(8) 2_766 . ? Zn4 O1 Zn1 71.83(8) 2_766 . ? Zn4 O1 Zn1 108.17(8) . . ? Zn2 O1 Zn1 72.32(8) . 2_766 ? Zn2 O1 Zn1 107.68(8) 2_766 2_766 ? Zn3 O1 Zn1 70.78(8) . 2_766 ? Zn3 O1 Zn1 109.22(8) 2_766 2_766 ? Zn4 O1 Zn1 108.17(8) 2_766 2_766 ? Zn4 O1 Zn1 71.83(8) . 2_766 ? Zn1 O1 Zn1 180.000(1) . 2_766 ? C1 O2 P1 132.8(16) . . ? C4 O3 P1 133.8(12) . . ? C7 O4 P2 123.4(8) . . ? C10 O5 P2 122.5(7) . . ? C13 O6 P3 117.3(15) . . ? C16 O7 P3 124.1(11) . . ? O2 C1 C2 119(3) . . ? O2 C1 C3 100(3) . . ? C2 C1 C3 109(3) . . ? O3 C4 C6 111.6(16) . . ? O3 C4 C5 109(2) . . ? C6 C4 C5 112.9(17) . . ? C9 C7 O4 111.2(15) . . ? C9 C7 C8 108.9(19) . . ? O4 C7 C8 105.7(13) . . ? O5 C10 C12 107.3(14) . . ? O5 C10 C11 107.1(13) . . ? C12 C10 C11 111.7(17) . . ? O6 C13 C14 108.0(18) . . ? O6 C13 C15 103(2) . . ? C14 C13 C15 109(2) . . ? C18 C16 C17 105(2) . . ? C18 C16 O7 114(2) . . ? C17 C16 O7 109(3) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.09 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.317 _refine_diff_density_min -1.000 _refine_diff_density_rms 0.116