Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_contact_author 'Prof. Francis J. DiSalvo' _publ_contact_author_address ; Prof. Francis J. DiSalvo Department of Chemistry and Chemical Biology Cornell University Ithaca, NY 14853 USA ; _publ_contact_author_email 'fjd3@cornell.edu' _publ_contact_author_fax '607-255-4137' _publ_contact_author_phone '607-255-7238' _publ_contact_letter ; This is a CIF submission as the Supporting Information for the paper submitted for publication in Chemical Communications ; _publ_requested_journal 'Chemical Communications' # Title and Author List _publ_section_title ; Novel octahedral tungsten sulfidocyanide cluster anion [W6S8(CN)6]6- ; loop_ _publ_author_name 'Jin, Song' 'DiSalvo, Francis J.' _publ_author_address ; Department of Chemistry and Chemical Biology Cornell University Ithaca, NY 14853 USA ; # =========================================END data_final _database_code_CSD 163699 _audit_creation_method SHELXL-97 _chemical_name_systematic ; hexa sodium octakis(mu!3$-sulfido)-hexakis(cyano) -hexa-tungsten-octadecakis(dimethylsulfide)solvate ; _chemical_name_common 'Tugsten sulfide cyano cluster' _chemical_melting_point ? _chemical_formula_moiety Na6W6S8(CN)6(C2H6SO)18 _chemical_formula_sum 'C42 H108 N6 Na6 O18 S26 W6' _chemical_formula_weight 3059.94 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' 'N' 'N' 0.0061 0.0033 '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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'W' 'W' -0.8490 6.8722 '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Rhombohedral _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 26.497(3) _cell_length_b 26.497(3) _cell_length_c 12.1761(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 7403.3(15) _cell_formula_units_Z 3 _cell_measurement_temperature 165(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'brown red' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'NOT MEASURED' _exptl_crystal_density_diffrn 2.059 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4416 _exptl_absorpt_coefficient_mu 7.593 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.493099 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details ? _exptl_special_details ; SADABS beta version was used for the empirical absorption correction. This program gives a ratio of the Tmin to Tmax, so the T max above is 1 and the Tmin is such ratio. ; _diffrn_ambient_temperature 165(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 ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 17304 _diffrn_reflns_av_R_equivalents 0.0328 _diffrn_reflns_av_sigmaI/netI 0.0216 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 26.36 _reflns_number_total 3370 _reflns_number_gt 2958 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction SHELXTL _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material 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. The non-solvent atoms(W,S, cyanide CN, and Na) are refined anisotropically. The DMSO solvent molecules are disordered into three positions and refined successfully. The hydrogen atoms are added and refined with riding models. ; _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^)+(0.0180P)^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 3370 _refine_ls_number_parameters 166 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.0314 _refine_ls_R_factor_gt 0.0249 _refine_ls_wR_factor_ref 0.0576 _refine_ls_wR_factor_gt 0.0563 _refine_ls_goodness_of_fit_ref 1.572 _refine_ls_restrained_S_all 1.615 _refine_ls_shift/su_max 0.072 _refine_ls_shift/su_mean 0.009 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 W1 W 0.050857(7) 0.063831(7) 0.909794(14) 0.02129(7) Uani 1 1 d . . . S2 S 0.0000 0.0000 0.75367(16) 0.0280(4) Uani 1 3 d S . . S3 S 0.09298(5) 0.11707(4) 1.08160(10) 0.0277(3) Uani 1 1 d . . . C1 C 0.10824(19) 0.13547(19) 0.7998(4) 0.0314(10) Uani 1 1 d . . . N1 N 0.13625(17) 0.17215(17) 0.7379(4) 0.0414(10) Uani 1 1 d . A . Na1 Na 0.17599(8) 0.25565(7) 0.62957(16) 0.0378(5) Uani 1 1 d D . . S4 S 0.1459(2) 0.20268(17) 0.3473(2) 0.0412(9) Uiso 0.707(19) 1 d PD A 1 O41 O 0.1645(3) 0.2423(3) 0.4409(4) 0.043(2) Uiso 0.707(19) 1 d PD A 1 C41 C 0.1906(4) 0.1714(4) 0.3365(9) 0.052(3) Uiso 0.707(19) 1 d PD A 1 H41A H 0.2292 0.2007 0.3098 0.079 Uiso 0.707(19) 1 calc PR A 1 H41B H 0.1731 0.1386 0.2849 0.079 Uiso 0.707(19) 1 calc PR A 1 H41C H 0.1944 0.1574 0.4088 0.079 Uiso 0.707(19) 1 calc PR A 1 C42 C 0.0807(4) 0.1387(5) 0.3945(9) 0.054(3) Uiso 0.707(19) 1 d PD A 1 H42A H 0.0498 0.1483 0.4060 0.082 Uiso 0.707(19) 1 calc PR A 1 H42B H 0.0888 0.1254 0.4639 0.082 Uiso 0.707(19) 1 calc PR A 1 H42C H 0.0681 0.1078 0.3394 0.082 Uiso 0.707(19) 1 calc PR A 1 S4A S 0.1652(5) 0.1752(5) 0.4242(9) 0.055(4) Uiso 0.131(4) 1 d PD A 2 O42 O 0.1777(10) 0.2323(8) 0.4638(12) 0.009(5) Uiso 0.131(4) 1 d PD A 2 C43 C 0.2012(12) 0.1890(12) 0.2967(18) 0.002(6) Uiso 0.131(4) 1 d PD A 2 H43A H 0.1869 0.1523 0.2565 0.002 Uiso 0.131(4) 1 calc PR A 2 H43B H 0.2432 0.2067 0.3089 0.002 Uiso 0.131(4) 1 calc PR A 2 H43C H 0.1935 0.2157 0.2537 0.002 Uiso 0.131(4) 1 calc PR A 2 C44 C 0.0922(8) 0.1403(18) 0.373(3) 0.023(10) Uiso 0.131(4) 1 d PD A 2 H44A H 0.0887 0.1156 0.3106 0.035 Uiso 0.131(4) 1 calc PR A 2 H44B H 0.0825 0.1699 0.3502 0.035 Uiso 0.131(4) 1 calc PR A 2 H44C H 0.0653 0.1162 0.4315 0.035 Uiso 0.131(4) 1 calc PR A 2 S4B S 0.1303(9) 0.1926(7) 0.3479(8) 0.033(4) Uiso 0.163(18) 1 d PD A 3 O43 O 0.161(2) 0.226(3) 0.453(2) 0.13(3) Uiso 0.163(18) 1 d PD A 3 C46 C 0.0887(13) 0.1229(12) 0.407(3) 0.039(10) Uiso 0.163(18) 1 d PD A 3 H46A H 0.0570 0.1216 0.4506 0.059 Uiso 0.163(18) 1 calc PR A 3 H46B H 0.1136 0.1147 0.4543 0.059 Uiso 0.163(18) 1 calc PR A 3 H46C H 0.0722 0.0935 0.3486 0.059 Uiso 0.163(18) 1 calc PR A 3 C45 C 0.1866(17) 0.1836(19) 0.289(4) 0.070(19) Uiso 0.163(18) 1 d PD A 3 H45A H 0.2219 0.2218 0.2809 0.106 Uiso 0.163(18) 1 calc PR A 3 H45B H 0.1742 0.1653 0.2166 0.106 Uiso 0.163(18) 1 calc PR A 3 H45C H 0.1949 0.1589 0.3367 0.106 Uiso 0.163(18) 1 calc PR A 3 S5 S 0.17338(8) 0.38342(8) 0.64262(14) 0.0298(5) Uiso 0.654(4) 1 d P A 1 O51 O 0.1455(3) 0.3202(3) 0.6477(5) 0.0310(17) Uiso 0.654(4) 1 d P A 1 C51 C 0.2337(3) 0.4148(3) 0.7360(6) 0.0271(19) Uiso 0.654(4) 1 d P A 1 H51A H 0.2646 0.4080 0.7088 0.041 Uiso 0.654(4) 1 calc PR A 1 H51B H 0.2208 0.3968 0.8085 0.041 Uiso 0.654(4) 1 calc PR A 1 H51C H 0.2486 0.4568 0.7418 0.041 Uiso 0.654(4) 1 calc PR A 1 C52 C 0.1273(3) 0.4034(3) 0.7151(7) 0.0315(17) Uiso 0.654(4) 1 d P A 1 H52A H 0.0907 0.3894 0.6747 0.047 Uiso 0.654(4) 1 calc PR A 1 H52B H 0.1469 0.4459 0.7219 0.047 Uiso 0.654(4) 1 calc PR A 1 H52C H 0.1190 0.3858 0.7884 0.047 Uiso 0.654(4) 1 calc PR A 1 S5' S 0.15891(14) 0.37196(14) 0.7325(3) 0.0284(10) Uiso 0.346(4) 1 d P A 2 O51' O 0.1419(4) 0.3154(4) 0.6791(9) 0.021(3) Uiso 0.346(4) 1 d P A 2 C51' C 0.2344(6) 0.4205(6) 0.6986(13) 0.027(4) Uiso 0.346(4) 1 d P A 2 H51D H 0.2584 0.4055 0.7299 0.041 Uiso 0.346(4) 1 calc PR A 2 H51E H 0.2468 0.4593 0.7288 0.041 Uiso 0.346(4) 1 calc PR A 2 H51F H 0.2390 0.4232 0.6186 0.041 Uiso 0.346(4) 1 calc PR A 2 C52' C 0.1301(5) 0.4110(5) 0.6631(11) 0.023(3) Uiso 0.346(4) 1 d P A 2 H52D H 0.0876 0.3900 0.6705 0.034 Uiso 0.346(4) 1 calc PR A 2 H52E H 0.1405 0.4145 0.5851 0.034 Uiso 0.346(4) 1 calc PR A 2 H52F H 0.1463 0.4499 0.6953 0.034 Uiso 0.346(4) 1 calc PR A 2 S6 S 0.31954(16) 0.28637(19) 0.6929(5) 0.0286(10) Uiso 0.56(2) 1 d P A 1 O61 O 0.2750(3) 0.3054(3) 0.6875(8) 0.030(2) Uiso 0.56(2) 1 d P A 1 C61 C 0.2943(7) 0.2295(7) 0.5681(10) 0.063(4) Uiso 0.56(2) 1 d P A 1 H61A H 0.3056 0.2508 0.4983 0.095 Uiso 0.56(2) 1 calc PR A 1 H61B H 0.2518 0.2042 0.5702 0.095 Uiso 0.56(2) 1 calc PR A 1 H61C H 0.3130 0.2058 0.5747 0.095 Uiso 0.56(2) 1 calc PR A 1 C62 C 0.2907(5) 0.2277(5) 0.7862(10) 0.026(3) Uiso 0.56(2) 1 d P A 1 H62A H 0.2965 0.2428 0.8614 0.039 Uiso 0.56(2) 1 calc PR A 1 H62B H 0.3107 0.2053 0.7769 0.039 Uiso 0.56(2) 1 calc PR A 1 H62C H 0.2490 0.2025 0.7722 0.039 Uiso 0.56(2) 1 calc PR A 1 S6' S 0.3138(2) 0.2775(3) 0.6686(7) 0.0345(12) Uiso 0.44(2) 1 d P A 2 O61' O 0.2727(4) 0.3012(4) 0.6572(11) 0.030(3) Uiso 0.44(2) 1 d P A 2 C61' C 0.3258(10) 0.2582(10) 0.5645(13) 0.077(6) Uiso 0.44(2) 1 d P A 2 H61D H 0.3393 0.2897 0.5105 0.115 Uiso 0.44(2) 1 calc PR A 2 H61E H 0.2902 0.2241 0.5377 0.115 Uiso 0.44(2) 1 calc PR A 2 H61F H 0.3561 0.2477 0.5756 0.115 Uiso 0.44(2) 1 calc PR A 2 C62' C 0.2883(8) 0.2205(9) 0.7596(16) 0.056(6) Uiso 0.44(2) 1 d P A 2 H62D H 0.2809 0.2328 0.8308 0.085 Uiso 0.44(2) 1 calc PR A 2 H62E H 0.3174 0.2083 0.7685 0.085 Uiso 0.44(2) 1 calc PR A 2 H62F H 0.2520 0.1877 0.7315 0.085 Uiso 0.44(2) 1 calc PR 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 W1 0.01309(9) 0.01180(9) 0.03809(11) 0.00117(7) 0.00100(7) 0.00555(7) S2 0.0237(6) 0.0237(6) 0.0366(11) 0.000 0.000 0.0119(3) S3 0.0173(5) 0.0143(5) 0.0470(7) -0.0045(5) -0.0031(5) 0.0046(4) C1 0.022(2) 0.021(2) 0.052(3) -0.002(2) -0.001(2) 0.011(2) N1 0.034(2) 0.022(2) 0.064(3) 0.013(2) 0.013(2) 0.0103(19) Na1 0.0292(10) 0.0229(9) 0.0602(12) 0.0102(9) 0.0091(9) 0.0121(8) _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 W1 C1 2.196(5) . ? W1 S2 2.4518(15) . ? W1 S3 2.4571(11) . ? W1 S3 2.4587(11) 11_557 ? W1 S3 2.4667(11) 12_557 ? W1 W1 2.6818(4) 2 ? W1 W1 2.6818(4) 3 ? W1 W1 2.6875(4) 11_557 ? W1 W1 2.6875(4) 12_557 ? S2 W1 2.4518(15) 3 ? S2 W1 2.4518(15) 2 ? S3 W1 2.4587(11) 12_557 ? S3 W1 2.4667(11) 11_557 ? C1 N1 1.158(6) . ? N1 Na1 2.327(4) . ? Na1 O42 2.118(13) . ? Na1 O51 2.239(6) . ? Na1 O61' 2.246(10) . ? Na1 O43 2.255(15) . ? Na1 O51' 2.261(10) . ? Na1 O41 2.322(5) . ? Na1 O61 2.378(8) . ? Na1 S4A 3.204(11) . ? S4 O41 1.458(5) . ? S4 C41 1.757(7) . ? S4 C42 1.805(9) . ? S4A O42 1.458(16) . ? S4A C43 1.763(15) . ? S4A C44 1.786(16) . ? S4B O43 1.534(17) . ? S4B C46 1.763(16) . ? S4B C45 1.775(16) . ? S5 O51 1.455(6) . ? S5 C52 1.787(7) . ? S5 C51 1.791(8) . ? S5' O51' 1.482(10) . ? S5' C52' 1.776(13) . ? S5' C51' 1.804(15) . ? S6 O61 1.500(8) . ? S6 C62 1.761(11) . ? S6 C61 2.004(16) . ? S6' C61' 1.460(18) . ? S6' O61' 1.510(10) . ? S6' C62' 1.718(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 C1 W1 S2 91.57(13) . . ? C1 W1 S3 95.96(12) . . ? S2 W1 S3 172.47(4) . . ? C1 W1 S3 93.57(11) . 11_557 ? S2 W1 S3 90.08(3) . 11_557 ? S3 W1 S3 89.60(3) . 11_557 ? C1 W1 S3 94.19(11) . 12_557 ? S2 W1 S3 89.89(3) . 12_557 ? S3 W1 S3 89.42(3) . 12_557 ? S3 W1 S3 172.24(4) 11_557 12_557 ? C1 W1 W1 133.47(12) . 2 ? S2 W1 W1 56.85(2) . 2 ? S3 W1 W1 116.92(3) . 2 ? S3 W1 W1 117.09(3) 11_557 2 ? S3 W1 W1 56.87(3) 12_557 2 ? C1 W1 W1 133.20(12) . 3 ? S2 W1 W1 56.85(2) . 3 ? S3 W1 W1 117.11(3) . 3 ? S3 W1 W1 57.15(3) 11_557 3 ? S3 W1 W1 116.81(3) 12_557 3 ? W1 W1 W1 60.0 2 3 ? C1 W1 W1 136.48(12) . 11_557 ? S2 W1 W1 116.86(3) . 11_557 ? S3 W1 W1 57.09(3) . 11_557 ? S3 W1 W1 56.83(3) 11_557 11_557 ? S3 W1 W1 116.56(3) 12_557 11_557 ? W1 W1 W1 90.0 2 11_557 ? W1 W1 W1 60.071(6) 3 11_557 ? C1 W1 W1 136.77(12) . 12_557 ? S2 W1 W1 116.86(3) . 12_557 ? S3 W1 W1 56.89(3) . 12_557 ? S3 W1 W1 116.65(3) 11_557 12_557 ? S3 W1 W1 56.75(3) 12_557 12_557 ? W1 W1 W1 60.071(6) 2 12_557 ? W1 W1 W1 90.0 3 12_557 ? W1 W1 W1 59.858(12) 11_557 12_557 ? W1 S2 W1 66.31(5) . 3 ? W1 S2 W1 66.31(5) . 2 ? W1 S2 W1 66.31(5) 3 2 ? W1 S3 W1 66.28(3) . 12_557 ? W1 S3 W1 66.16(3) . 11_557 ? W1 S3 W1 65.98(3) 12_557 11_557 ? N1 C1 W1 176.6(4) . . ? C1 N1 Na1 164.2(4) . . ? O42 Na1 O51 112.7(6) . . ? O42 Na1 O61' 96.6(7) . . ? O51 Na1 O61' 109.0(3) . . ? O42 Na1 O43 10.4(18) . . ? O51 Na1 O43 107.0(19) . . ? O61' Na1 O43 106.8(15) . . ? O42 Na1 O51' 122.2(7) . . ? O51 Na1 O51' 10.1(3) . . ? O61' Na1 O51' 109.3(4) . . ? O43 Na1 O51' 115.8(19) . . ? O42 Na1 O41 14.8(6) . . ? O51 Na1 O41 98.3(3) . . ? O61' Na1 O41 104.9(4) . . ? O43 Na1 O41 10.5(18) . . ? O51' Na1 O41 107.6(4) . . ? O42 Na1 N1 109.1(5) . . ? O51 Na1 N1 120.4(2) . . ? O61' Na1 N1 106.2(3) . . ? O43 Na1 N1 106.8(17) . . ? O51' Na1 N1 111.4(3) . . ? O41 Na1 N1 117.0(2) . . ? O42 Na1 O61 105.4(7) . . ? O51 Na1 O61 105.5(3) . . ? O61' Na1 O61 8.9(3) . . ? O43 Na1 O61 115.6(15) . . ? O51' Na1 O61 104.4(3) . . ? O41 Na1 O61 113.7(3) . . ? N1 Na1 O61 102.0(2) . . ? O42 Na1 S4A 21.5(5) . . ? O51 Na1 S4A 129.7(3) . . ? O61' Na1 S4A 100.0(4) . . ? O43 Na1 S4A 23.5(19) . . ? O51' Na1 S4A 137.7(4) . . ? O41 Na1 S4A 33.4(3) . . ? N1 Na1 S4A 87.8(2) . . ? O61 Na1 S4A 107.9(3) . . ? O41 S4 C41 109.5(5) . . ? O41 S4 C42 104.3(5) . . ? C41 S4 C42 97.8(5) . . ? S4 O41 Na1 148.7(5) . . ? O42 S4A C43 104.9(12) . . ? O42 S4A C44 106.2(19) . . ? C43 S4A C44 97.8(11) . . ? O42 S4A Na1 32.2(7) . . ? C43 S4A Na1 133.7(10) . . ? C44 S4A Na1 109.2(14) . . ? S4A O42 Na1 126.3(12) . . ? O43 S4B C46 98(3) . . ? O43 S4B C45 100(3) . . ? C46 S4B C45 98.7(12) . . ? S4B O43 Na1 161(3) . . ? O51 S5 C52 106.9(4) . . ? O51 S5 C51 109.2(4) . . ? C52 S5 C51 97.6(4) . . ? S5 O51 Na1 134.9(4) . . ? O51' S5' C52' 112.2(6) . . ? O51' S5' C51' 106.8(6) . . ? C52' S5' C51' 97.0(6) . . ? S5' O51' Na1 143.1(6) . . ? O61 S6 C62 104.9(5) . . ? O61 S6 C61 101.3(5) . . ? C62 S6 C61 89.5(6) . . ? S6 O61 Na1 131.5(4) . . ? C61' S6' O61' 113.3(9) . . ? C61' S6' C62' 108.1(10) . . ? O61' S6' C62' 112.1(8) . . ? S6' O61' Na1 131.0(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.36 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.043 _refine_diff_density_min -1.080 _refine_diff_density_rms 0.119 # ========================================= END data_final_2 _database_code_CSD 163700 _audit_creation_method SHELXL-97 _chemical_name_systematic ; hexa potassium octakis(mu!3$-sulfido)-hexakis(cyano) -hexa-tungsten-decakis(water)solvate ; _chemical_name_common 'Tugsten sulfidocyanide cluster' _chemical_melting_point ? _chemical_formula_moiety K6W6S8(CN)6(H2O)10 _chemical_formula_sum 'C6 H20 K6 N6 O10 S8 W6' _chemical_formula_weight 1930.46 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M Fm-3m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, -z' '-y, -x, -z' 'y, -x, z' '-y, x, z' 'x, z, -y' '-x, z, y' '-x, -z, -y' 'x, -z, y' 'z, y, -x' 'z, -y, x' '-z, y, x' '-z, -y, -x' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' 'z, x+1/2, y+1/2' 'z, -x+1/2, -y+1/2' '-z, -x+1/2, y+1/2' '-z, x+1/2, -y+1/2' 'y, z+1/2, x+1/2' '-y, z+1/2, -x+1/2' 'y, -z+1/2, -x+1/2' '-y, -z+1/2, x+1/2' 'y, x+1/2, -z+1/2' '-y, -x+1/2, -z+1/2' 'y, -x+1/2, z+1/2' '-y, x+1/2, z+1/2' 'x, z+1/2, -y+1/2' '-x, z+1/2, y+1/2' '-x, -z+1/2, -y+1/2' 'x, -z+1/2, y+1/2' 'z, y+1/2, -x+1/2' 'z, -y+1/2, x+1/2' '-z, y+1/2, x+1/2' '-z, -y+1/2, -x+1/2' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+1/2, y, -z+1/2' 'x+1/2, -y, -z+1/2' 'z+1/2, x, y+1/2' 'z+1/2, -x, -y+1/2' '-z+1/2, -x, y+1/2' '-z+1/2, x, -y+1/2' 'y+1/2, z, x+1/2' '-y+1/2, z, -x+1/2' 'y+1/2, -z, -x+1/2' '-y+1/2, -z, x+1/2' 'y+1/2, x, -z+1/2' '-y+1/2, -x, -z+1/2' 'y+1/2, -x, z+1/2' '-y+1/2, x, z+1/2' 'x+1/2, z, -y+1/2' '-x+1/2, z, y+1/2' '-x+1/2, -z, -y+1/2' 'x+1/2, -z, y+1/2' 'z+1/2, y, -x+1/2' 'z+1/2, -y, x+1/2' '-z+1/2, y, x+1/2' '-z+1/2, -y, -x+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'z+1/2, x+1/2, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x+1/2, y' '-z+1/2, x+1/2, -y' 'y+1/2, z+1/2, x' '-y+1/2, z+1/2, -x' 'y+1/2, -z+1/2, -x' '-y+1/2, -z+1/2, x' 'y+1/2, x+1/2, -z' '-y+1/2, -x+1/2, -z' 'y+1/2, -x+1/2, z' '-y+1/2, x+1/2, z' 'x+1/2, z+1/2, -y' '-x+1/2, z+1/2, y' '-x+1/2, -z+1/2, -y' 'x+1/2, -z+1/2, y' 'z+1/2, y+1/2, -x' 'z+1/2, -y+1/2, x' '-z+1/2, y+1/2, x' '-z+1/2, -y+1/2, -x' '-x, -y, -z' 'x, y, -z' 'x, -y, z' '-x, y, z' '-z, -x, -y' '-z, x, y' 'z, x, -y' 'z, -x, y' '-y, -z, -x' 'y, -z, x' '-y, z, x' 'y, z, -x' '-y, -x, z' 'y, x, z' '-y, x, -z' 'y, -x, -z' '-x, -z, y' 'x, -z, -y' 'x, z, y' '-x, z, -y' '-z, -y, x' '-z, y, -x' 'z, -y, -x' 'z, y, x' '-x, -y+1/2, -z+1/2' 'x, y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' '-x, y+1/2, z+1/2' '-z, -x+1/2, -y+1/2' '-z, x+1/2, y+1/2' 'z, x+1/2, -y+1/2' 'z, -x+1/2, y+1/2' '-y, -z+1/2, -x+1/2' 'y, -z+1/2, x+1/2' '-y, z+1/2, x+1/2' 'y, z+1/2, -x+1/2' '-y, -x+1/2, z+1/2' 'y, x+1/2, z+1/2' '-y, x+1/2, -z+1/2' 'y, -x+1/2, -z+1/2' '-x, -z+1/2, y+1/2' 'x, -z+1/2, -y+1/2' 'x, z+1/2, y+1/2' '-x, z+1/2, -y+1/2' '-z, -y+1/2, x+1/2' '-z, y+1/2, -x+1/2' 'z, -y+1/2, -x+1/2' 'z, y+1/2, x+1/2' '-x+1/2, -y, -z+1/2' 'x+1/2, y, -z+1/2' 'x+1/2, -y, z+1/2' '-x+1/2, y, z+1/2' '-z+1/2, -x, -y+1/2' '-z+1/2, x, y+1/2' 'z+1/2, x, -y+1/2' 'z+1/2, -x, y+1/2' '-y+1/2, -z, -x+1/2' 'y+1/2, -z, x+1/2' '-y+1/2, z, x+1/2' 'y+1/2, z, -x+1/2' '-y+1/2, -x, z+1/2' 'y+1/2, x, z+1/2' '-y+1/2, x, -z+1/2' 'y+1/2, -x, -z+1/2' '-x+1/2, -z, y+1/2' 'x+1/2, -z, -y+1/2' 'x+1/2, z, y+1/2' '-x+1/2, z, -y+1/2' '-z+1/2, -y, x+1/2' '-z+1/2, y, -x+1/2' 'z+1/2, -y, -x+1/2' 'z+1/2, y, x+1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' '-z+1/2, -x+1/2, -y' '-z+1/2, x+1/2, y' 'z+1/2, x+1/2, -y' 'z+1/2, -x+1/2, y' '-y+1/2, -z+1/2, -x' 'y+1/2, -z+1/2, x' '-y+1/2, z+1/2, x' 'y+1/2, z+1/2, -x' '-y+1/2, -x+1/2, z' 'y+1/2, x+1/2, z' '-y+1/2, x+1/2, -z' 'y+1/2, -x+1/2, -z' '-x+1/2, -z+1/2, y' 'x+1/2, -z+1/2, -y' 'x+1/2, z+1/2, y' '-x+1/2, z+1/2, -y' '-z+1/2, -y+1/2, x' '-z+1/2, y+1/2, -x' 'z+1/2, -y+1/2, -x' 'z+1/2, y+1/2, x' _cell_length_a 15.3084(15) _cell_length_b 15.3084(16) _cell_length_c 15.3084(16) _cell_angle_alpha 90.000(2) _cell_angle_beta 90.000(3) _cell_angle_gamma 90.000(3) _cell_volume 3587.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 165(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'NOT MEASURED' _exptl_crystal_density_diffrn 3.574 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3456 _exptl_absorpt_coefficient_mu 20.369 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.656265 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details ? _exptl_special_details ; SADABS beta version was used for the empirical absorption correction. This program gives a ratio of the Tmin to Tmax, so the T max above is 1 and the Tmin is such ratio. ; _diffrn_ambient_temperature 165(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 ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 2749 _diffrn_reflns_av_R_equivalents 0.0445 _diffrn_reflns_av_sigmaI/netI 0.0248 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 30.39 _reflns_number_total 327 _reflns_number_gt 310 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction SHELXTL _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material 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. Both K positions are partially ocuppied and refined as such. There is no strong preference in the refinements to any specific K stoichiometries in the reasonable range of 5-7 per cluster. Based upon the chemical knowledge, the number of the K ions is fixed as 6 using SUMP command over 2 sites. Two solvent water sites are very close to each and refined as disordered. No hydrogen atoms are added for the solvent water molecules. The W,S,C,N and K atoms are refined anistropically. ; _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^)+(0.0000P)^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 none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00029(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 327 _refine_ls_number_parameters 27 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0457 _refine_ls_wR_factor_gt 0.0453 _refine_ls_goodness_of_fit_ref 2.075 _refine_ls_restrained_S_all 2.079 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.004 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 W1 W 0.5000 0.37634(3) 0.0000 0.00682(18) Uani 1 8 d S . . S2 S 0.38701(10) 0.38701(10) 0.11299(10) 0.0140(7) Uani 1 6 d S . . C3 C 0.5000 0.2358(10) 0.0000 0.008(3) Uani 1 8 d S . . N4 N 0.5000 0.1599(8) 0.0000 0.031(3) Uani 1 8 d S . . K5 K 0.5000 0.0000 0.0000 0.016(4) Uani 0.63(3) 48 d SP . . K6 K 0.3554(2) 0.1446(2) 0.1446(2) 0.064(2) Uani 0.677(5) 6 d SP . . O1S O 0.2500 0.2500 0.2500 0.028(5) Uiso 1 24 d S . . O2S O 0.258(3) 0.013(3) 0.242(3) 0.030(14) Uiso 0.169(11) 2 d SP . . O3S O 0.2767(16) 0.0000 0.2233(16) 0.020(10) Uiso 0.32(5) 4 d SP . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.0075(2) 0.0054(3) 0.0075(2) 0.000 0.000 0.000 S2 0.0140(7) 0.0140(7) 0.0140(7) 0.0045(6) 0.0045(6) -0.0045(6) C3 0.008(5) 0.008(6) 0.008(5) 0.000 0.000 0.000 N4 0.041(6) 0.012(7) 0.041(6) 0.000 0.000 0.000 K5 0.016(4) 0.016(4) 0.016(4) 0.000 0.000 0.000 K6 0.064(2) 0.064(2) 0.064(2) -0.0119(19) 0.0119(19) 0.0119(19) _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 W1 C3 2.152(16) . ? W1 S2 2.452(2) 100_655 ? W1 S2 2.452(2) 98 ? W1 S2 2.452(2) . ? W1 S2 2.452(2) 3_655 ? W1 W1 2.6772(7) 149_565 ? W1 W1 2.6772(7) 129_655 ? W1 W1 2.6772(7) 53_554 ? W1 W1 2.6772(7) 33_554 ? S2 W1 2.452(2) 149_565 ? S2 W1 2.452(2) 33_554 ? S2 K6 3.774(3) 28 ? S2 K6 3.774(3) . ? S2 K6 3.774(3) 74 ? C3 N4 1.162(19) . ? C3 K6 3.427(7) 98 ? C3 K6 3.427(7) 100_655 ? C3 K6 3.427(7) . ? C3 K6 3.427(7) 3_655 ? N4 K5 2.447(13) . ? N4 K6 3.139(5) 100_655 ? N4 K6 3.139(5) 98 ? N4 K6 3.139(5) . ? N4 K6 3.139(5) 3_655 ? K5 N4 2.447(13) 153 ? K5 N4 2.447(13) 57_554 ? K5 N4 2.447(13) 77_545 ? K5 N4 2.447(13) 97_655 ? K5 N4 2.447(13) 173 ? K5 K6 3.833(6) 100_655 ? K5 K6 3.833(6) 4 ? K5 K6 3.833(6) . ? K5 K6 3.833(6) 2_655 ? K5 K6 3.833(6) 98 ? K5 K6 3.833(6) 3_655 ? K6 O3S 2.79(2) 58 ? K6 O3S 2.79(2) . ? K6 O3S 2.79(2) 173 ? K6 O1S 2.795(6) . ? K6 O2S 2.91(6) 58 ? K6 O2S 2.91(6) 79 ? K6 O2S 2.91(6) . ? K6 N4 3.139(5) 153 ? K6 N4 3.139(5) 77_545 ? K6 O2S 3.18(6) 84 ? K6 O2S 3.18(6) 5 ? O1S K6 2.795(6) 28 ? O1S K6 2.795(6) 74 ? O1S K6 2.795(6) 51 ? O2S O2S 0.36(14) 51 ? O2S O2S 0.40(9) 99 ? O2S O2S 0.54(11) 145 ? O2S O3S 0.78(8) 145 ? O2S K6 3.18(6) 51 ? O2S K6 3.20(6) 99 ? O3S O2S 0.45(7) 99 ? O3S O2S 0.78(8) 145 ? O3S O2S 0.78(8) 51 ? O3S O3S 1.16(7) 145 ? O3S K6 2.79(2) 99 ? 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 C3 W1 S2 93.82(4) . 100_655 ? C3 W1 S2 93.82(4) . 98 ? S2 W1 S2 172.36(9) 100_655 98 ? C3 W1 S2 93.82(4) . . ? S2 W1 S2 89.746(6) 100_655 . ? S2 W1 S2 89.746(6) 98 . ? C3 W1 S2 93.82(4) . 3_655 ? S2 W1 S2 89.746(6) 100_655 3_655 ? S2 W1 S2 89.746(6) 98 3_655 ? S2 W1 S2 172.36(9) . 3_655 ? C3 W1 W1 135.0 . 149_565 ? S2 W1 W1 56.91(3) 100_655 149_565 ? S2 W1 W1 116.86(4) 98 149_565 ? S2 W1 W1 56.91(3) . 149_565 ? S2 W1 W1 116.86(4) 3_655 149_565 ? C3 W1 W1 135.0 . 129_655 ? S2 W1 W1 56.91(3) 100_655 129_655 ? S2 W1 W1 116.86(4) 98 129_655 ? S2 W1 W1 116.86(4) . 129_655 ? S2 W1 W1 56.91(3) 3_655 129_655 ? W1 W1 W1 60.0 149_565 129_655 ? C3 W1 W1 135.0 . 53_554 ? S2 W1 W1 116.86(4) 100_655 53_554 ? S2 W1 W1 56.91(3) 98 53_554 ? S2 W1 W1 116.86(4) . 53_554 ? S2 W1 W1 56.91(3) 3_655 53_554 ? W1 W1 W1 90.0 149_565 53_554 ? W1 W1 W1 60.0 129_655 53_554 ? C3 W1 W1 135.000(1) . 33_554 ? S2 W1 W1 116.86(4) 100_655 33_554 ? S2 W1 W1 56.91(3) 98 33_554 ? S2 W1 W1 56.91(3) . 33_554 ? S2 W1 W1 116.86(4) 3_655 33_554 ? W1 W1 W1 60.0 149_565 33_554 ? W1 W1 W1 90.0 129_655 33_554 ? W1 W1 W1 60.0 53_554 33_554 ? W1 S2 W1 66.19(7) 149_565 33_554 ? W1 S2 W1 66.19(7) 149_565 . ? W1 S2 W1 66.19(7) 33_554 . ? W1 S2 K6 96.62(9) 149_565 28 ? W1 S2 K6 140.87(4) 33_554 28 ? W1 S2 K6 140.87(4) . 28 ? W1 S2 K6 140.87(4) 149_565 . ? W1 S2 K6 140.87(4) 33_554 . ? W1 S2 K6 96.62(9) . . ? K6 S2 K6 74.43(14) 28 . ? W1 S2 K6 140.87(4) 149_565 74 ? W1 S2 K6 96.62(9) 33_554 74 ? W1 S2 K6 140.87(4) . 74 ? K6 S2 K6 74.43(14) 28 74 ? K6 S2 K6 74.43(14) . 74 ? N4 C3 W1 180.0 . . ? N4 C3 K6 66.0(3) . 98 ? W1 C3 K6 114.0(3) . 98 ? N4 C3 K6 66.0(3) . 100_655 ? W1 C3 K6 114.0(3) . 100_655 ? K6 C3 K6 131.9(5) 98 100_655 ? N4 C3 K6 66.0(3) . . ? W1 C3 K6 114.0(3) . . ? K6 C3 K6 80.4(2) 98 . ? K6 C3 K6 80.4(2) 100_655 . ? N4 C3 K6 66.0(3) . 3_655 ? W1 C3 K6 114.0(3) . 3_655 ? K6 C3 K6 80.4(2) 98 3_655 ? K6 C3 K6 80.4(2) 100_655 3_655 ? K6 C3 K6 131.9(5) . 3_655 ? C3 N4 K5 180.0 . . ? C3 N4 K6 94.3(2) . 100_655 ? K5 N4 K6 85.7(2) . 100_655 ? C3 N4 K6 94.3(2) . 98 ? K5 N4 K6 85.7(2) . 98 ? K6 N4 K6 171.4(5) 100_655 98 ? C3 N4 K6 94.3(2) . . ? K5 N4 K6 85.7(2) . . ? K6 N4 K6 89.68(4) 100_655 . ? K6 N4 K6 89.68(4) 98 . ? C3 N4 K6 94.3(2) . 3_655 ? K5 N4 K6 85.7(2) . 3_655 ? K6 N4 K6 89.68(4) 100_655 3_655 ? K6 N4 K6 89.68(4) 98 3_655 ? K6 N4 K6 171.4(5) . 3_655 ? N4 K5 N4 180.0 153 57_554 ? N4 K5 N4 90.0 153 77_545 ? N4 K5 N4 90.0 57_554 77_545 ? N4 K5 N4 90.0 153 . ? N4 K5 N4 90.0 57_554 . ? N4 K5 N4 90.0 77_545 . ? N4 K5 N4 90.0 153 97_655 ? N4 K5 N4 90.0 57_554 97_655 ? N4 K5 N4 90.0 77_545 97_655 ? N4 K5 N4 180.0 . 97_655 ? N4 K5 N4 90.0 153 173 ? N4 K5 N4 90.0 57_554 173 ? N4 K5 N4 180.0 77_545 173 ? N4 K5 N4 90.0 . 173 ? N4 K5 N4 90.0 97_655 173 ? N4 K5 K6 125.3 153 100_655 ? N4 K5 K6 54.7 57_554 100_655 ? N4 K5 K6 54.7 77_545 100_655 ? N4 K5 K6 54.7 . 100_655 ? N4 K5 K6 125.3 97_655 100_655 ? N4 K5 K6 125.3 173 100_655 ? N4 K5 K6 54.7 153 4 ? N4 K5 K6 125.3 57_554 4 ? N4 K5 K6 125.3 77_545 4 ? N4 K5 K6 125.3 . 4 ? N4 K5 K6 54.7 97_655 4 ? N4 K5 K6 54.7 173 4 ? K6 K5 K6 180.00(18) 100_655 4 ? N4 K5 K6 54.7 153 . ? N4 K5 K6 125.3 57_554 . ? N4 K5 K6 54.7 77_545 . ? N4 K5 K6 54.7 . . ? N4 K5 K6 125.3 97_655 . ? N4 K5 K6 125.3 173 . ? K6 K5 K6 70.5 100_655 . ? K6 K5 K6 109.5 4 . ? N4 K5 K6 125.3 153 2_655 ? N4 K5 K6 54.7 57_554 2_655 ? N4 K5 K6 54.7 77_545 2_655 ? N4 K5 K6 125.3 . 2_655 ? N4 K5 K6 54.7 97_655 2_655 ? N4 K5 K6 125.3 173 2_655 ? K6 K5 K6 70.5 100_655 2_655 ? K6 K5 K6 109.5 4 2_655 ? K6 K5 K6 109.5 . 2_655 ? N4 K5 K6 54.7 153 98 ? N4 K5 K6 125.3 57_554 98 ? N4 K5 K6 125.3 77_545 98 ? N4 K5 K6 54.7 . 98 ? N4 K5 K6 125.3 97_655 98 ? N4 K5 K6 54.7 173 98 ? K6 K5 K6 109.5 100_655 98 ? K6 K5 K6 70.5 4 98 ? K6 K5 K6 70.5 . 98 ? K6 K5 K6 180.00(18) 2_655 98 ? N4 K5 K6 125.3 153 3_655 ? N4 K5 K6 54.7 57_554 3_655 ? N4 K5 K6 125.3 77_545 3_655 ? N4 K5 K6 54.7 . 3_655 ? N4 K5 K6 125.3 97_655 3_655 ? N4 K5 K6 54.7 173 3_655 ? K6 K5 K6 70.5 100_655 3_655 ? K6 K5 K6 109.5 4 3_655 ? K6 K5 K6 109.5 . 3_655 ? K6 K5 K6 109.5 2_655 3_655 ? K6 K5 K6 70.5 98 3_655 ? O3S K6 O3S 119.84(8) 58 . ? O3S K6 O3S 119.84(8) 58 173 ? O3S K6 O3S 119.84(8) . 173 ? O3S K6 O1S 87.7(6) 58 . ? O3S K6 O1S 87.7(6) . . ? O3S K6 O1S 87.7(6) 173 . ? O3S K6 O2S 8.7(12) 58 58 ? O3S K6 O2S 118.9(3) . 58 ? O3S K6 O2S 118.9(3) 173 58 ? O1S K6 O2S 79.0(12) . 58 ? O3S K6 O2S 118.9(3) 58 79 ? O3S K6 O2S 118.9(3) . 79 ? O3S K6 O2S 8.7(12) 173 79 ? O1S K6 O2S 79.0(12) . 79 ? O2S K6 O2S 116.4(8) 58 79 ? O3S K6 O2S 118.9(3) 58 . ? O3S K6 O2S 8.7(12) . . ? O3S K6 O2S 118.9(3) 173 . ? O1S K6 O2S 79.0(12) . . ? O2S K6 O2S 116.4(8) 58 . ? O2S K6 O2S 116.4(8) 79 . ? O3S K6 N4 131.9(6) 58 153 ? O3S K6 N4 73.3(5) . 153 ? O3S K6 N4 73.3(5) 173 153 ? O1S K6 N4 140.5(2) . 153 ? O2S K6 N4 140.5(12) 58 153 ? O2S K6 N4 80.5(10) 79 153 ? O2S K6 N4 80.5(10) . 153 ? O3S K6 N4 73.3(5) 58 . ? O3S K6 N4 131.9(6) . . ? O3S K6 N4 73.3(5) 173 . ? O1S K6 N4 140.5(2) . . ? O2S K6 N4 80.5(10) 58 . ? O2S K6 N4 80.5(10) 79 . ? O2S K6 N4 140.5(12) . . ? N4 K6 N4 66.9(4) 153 . ? O3S K6 N4 73.3(5) 58 77_545 ? O3S K6 N4 73.3(5) . 77_545 ? O3S K6 N4 131.9(6) 173 77_545 ? O1S K6 N4 140.5(2) . 77_545 ? O2S K6 N4 80.5(10) 58 77_545 ? O2S K6 N4 140.5(12) 79 77_545 ? O2S K6 N4 80.5(10) . 77_545 ? N4 K6 N4 66.9(4) 153 77_545 ? N4 K6 N4 66.9(4) . 77_545 ? O3S K6 O2S 13.1(11) 58 84 ? O3S K6 O2S 118.1(3) . 84 ? O3S K6 O2S 118.1(3) 173 84 ? O1S K6 O2S 74.5(10) . 84 ? O2S K6 O2S 4.5(18) 58 84 ? O2S K6 O2S 115.0(5) 79 84 ? O2S K6 O2S 115.0(5) . 84 ? N4 K6 O2S 145.0(10) 153 84 ? N4 K6 O2S 84.2(8) . 84 ? N4 K6 O2S 84.2(8) 77_545 84 ? O3S K6 O2S 118.1(3) 58 5 ? O3S K6 O2S 118.1(3) . 5 ? O3S K6 O2S 13.1(11) 173 5 ? O1S K6 O2S 74.5(10) . 5 ? O2S K6 O2S 115.0(5) 58 5 ? O2S K6 O2S 4.5(18) 79 5 ? O2S K6 O2S 115.0(5) . 5 ? N4 K6 O2S 84.2(8) 153 5 ? N4 K6 O2S 84.2(8) . 5 ? N4 K6 O2S 145.0(10) 77_545 5 ? O2S K6 O2S 113.2(8) 84 5 ? K6 O1S K6 109.471(1) 28 . ? K6 O1S K6 109.5 28 74 ? K6 O1S K6 109.5 . 74 ? K6 O1S K6 109.5 28 51 ? K6 O1S K6 109.5 . 51 ? K6 O1S K6 109.471(1) 74 51 ? O2S O2S O2S 90.00(6) 51 99 ? O2S O2S O2S 48(10) 51 145 ? O2S O2S O2S 42(10) 99 145 ? O2S O2S O3S 15(4) 51 145 ? O2S O2S O3S 75(4) 99 145 ? O2S O2S O3S 33(10) 145 145 ? O2S O2S K6 136.3(13) 51 . ? O2S O2S K6 133.7(12) 99 . ? O2S O2S K6 175(10) 145 . ? O3S O2S K6 151(5) 145 . ? O2S O2S K6 39.3(10) 51 51 ? O2S O2S K6 129.3(10) 99 51 ? O2S O2S K6 88(10) 145 51 ? O3S O2S K6 54(4) 145 51 ? K6 O2S K6 97.0(13) . 51 ? O2S O2S K6 131.1(11) 51 99 ? O2S O2S K6 41.1(10) 99 99 ? O2S O2S K6 83(10) 145 99 ? O3S O2S K6 116(4) 145 99 ? K6 O2S K6 92.7(19) . 99 ? K6 O2S K6 170(2) 51 99 ? O2S O3S O2S 12(6) 99 145 ? O2S O3S O2S 42(9) 99 51 ? O2S O3S O2S 30(7) 145 51 ? O2S O3S O3S 27(7) 99 145 ? O2S O3S O3S 15(4) 145 145 ? O2S O3S O3S 15(4) 51 145 ? O2S O3S K6 154(7) 99 . ? O2S O3S K6 142(4) 145 . ? O2S O3S K6 113(4) 51 . ? O3S O3S K6 127.6(6) 145 . ? O2S O3S K6 101(6) 99 99 ? O2S O3S K6 113(4) 145 99 ? O2S O3S K6 142(4) 51 99 ? O3S O3S K6 127.6(6) 145 99 ? K6 O3S K6 104.8(11) . 99 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.39 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.866 _refine_diff_density_min -1.694 _refine_diff_density_rms 0.283 #==========================================END