data_global _journal_coden_Cambridge 0004 _publ_requested_journal 'Journal of American Chemical Society' loop_ _publ_author_name 'Chung, In' 'Malliakas, Christos D.' 'Sootman, Joseph R.' 'Jang, Joon I.' 'Canlas, Christian G.' 'Weliky, David P.' 'Kanatzidis, Mercouri G.' _publ_contact_author_name 'Prof. Mercouri G. Kanatzidis' _publ_contact_author_address ; Prof. Mercouri Kanatzidis Department of Chemistry Northwestern University Evanston IL 60208 UNITED STATES OF AMERICA ; _publ_contact_author_email m-kanatzidis@northwestern.edu _publ_section_title ; The Helical Polymer 1/\\infty[P2Se62-]: Strong Second Harmonic Generation Response and Phase-Change Properties of its K and Rb Salts. ; data_k2p2se6_298K _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 660 _chemical_formula_moiety 'P2 Se6, 2(K)' _chemical_formula_sum 'K2 P2 Se6' _chemical_formula_weight 613.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'P' 'P' 0.1023 0.0942 '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' '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 P3(1)21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' 'y, x, -z' 'x-y, -y, -z+2/3' '-x, -x+y, -z+1/3' _cell_length_a 7.2746(8) _cell_length_b 7.2746(8) _cell_length_c 18.871(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 864.8(2) _cell_formula_units_Z 3 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 830 _cell_measurement_theta_min 3.24 _cell_measurement_theta_max 27.12 _exptl_crystal_description rod _exptl_crystal_colour 'orange red' _exptl_crystal_size_max 0.162 _exptl_crystal_size_mid 0.048 _exptl_crystal_size_min 0.048 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.536 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 19.974 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.09932 _exptl_absorpt_correction_T_max 0.39387 _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 'Bruker CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count 0.3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% ? _diffrn_reflns_number 7444 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0240 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 28.27 _reflns_number_total 1382 _reflns_number_gt 1306 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.1d (Crystal Impact Gbr, 2006)' _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^)+(0.0232P)^2^+1.0960P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.27(2) _refine_ls_number_reflns 1382 _refine_ls_number_parameters 47 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0264 _refine_ls_R_factor_gt 0.0234 _refine_ls_wR_factor_ref 0.0524 _refine_ls_wR_factor_gt 0.0511 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _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 Se1 Se 0.07574(7) 0.25839(7) 0.22327(2) 0.02683(11) Uani 1 1 d . . . Se2 Se 0.27689(8) 0.26490(10) 0.39571(3) 0.04410(15) Uani 1 1 d . . . Se3 Se 0.45720(8) 0.24953(9) 0.08010(2) 0.03391(13) Uani 1 1 d . . . K K 0.5542(2) 0.2697(2) 0.25379(6) 0.0487(3) Uani 1 1 d . . . P P 0.12847(16) 0.05920(16) 0.05480(5) 0.0200(2) 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 Se1 0.0296(2) 0.0220(2) 0.02088(18) -0.00075(16) 0.00421(17) 0.00684(17) Se2 0.0228(2) 0.0542(3) 0.0377(3) -0.0073(2) -0.0020(2) 0.0060(2) Se3 0.0206(2) 0.0524(3) 0.0251(2) 0.0001(2) -0.00221(17) 0.0154(2) K 0.0582(8) 0.0709(9) 0.0334(5) -0.0023(5) -0.0068(5) 0.0445(7) P 0.0215(5) 0.0221(5) 0.0160(4) -0.0003(4) 0.0001(4) 0.0106(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 Se1 P 2.3313(11) 6 ? Se1 Se1 2.3397(9) 6 ? Se1 K 3.4883(14) . ? Se1 K 3.8786(14) 1_455 ? Se2 P 2.1316(12) 2 ? Se2 K 3.3426(14) . ? Se2 K 3.3737(16) 5_565 ? Se2 K 3.9305(16) 5 ? Se3 P 2.1337(12) . ? Se3 K 3.3405(13) . ? Se3 K 3.4320(15) 6_665 ? Se3 K 3.4585(13) 3_664 ? Se3 K 3.8441(15) 6_655 ? K Se2 3.3737(16) 5_665 ? K Se3 3.4320(15) 6_655 ? K Se3 3.4585(13) 2_655 ? K Se3 3.8441(15) 6_665 ? K Se1 3.8786(14) 1_655 ? K Se2 3.9305(16) 5 ? K K 4.534(3) 5 ? K K 4.9507(16) 6_655 ? K K 4.9507(16) 6_665 ? P Se2 2.1316(12) 3_554 ? P P 2.2449(19) 4 ? P Se1 2.3314(11) 6 ? 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 P Se1 Se1 100.56(3) 6 6 ? P Se1 K 93.93(4) 6 . ? Se1 Se1 K 120.22(3) 6 . ? P Se1 K 79.94(3) 6 1_455 ? Se1 Se1 K 77.88(3) 6 1_455 ? K Se1 K 161.82(4) . 1_455 ? P Se2 K 115.98(4) 2 . ? P Se2 K 96.56(4) 2 5_565 ? K Se2 K 111.06(3) . 5_565 ? P Se2 K 85.64(4) 2 5 ? K Se2 K 76.66(4) . 5 ? K Se2 K 169.65(4) 5_565 5 ? P Se3 K 113.06(4) . . ? P Se3 K 93.87(4) . 6_665 ? K Se3 K 93.93(3) . 6_665 ? P Se3 K 105.92(4) . 3_664 ? K Se3 K 141.01(3) . 3_664 ? K Se3 K 82.31(4) 6_665 3_664 ? P Se3 K 83.84(4) . 6_655 ? K Se3 K 86.82(3) . 6_655 ? K Se3 K 177.70(5) 6_665 6_655 ? K Se3 K 98.48(2) 3_664 6_655 ? Se3 K Se2 132.26(4) . . ? Se3 K Se2 102.66(4) . 5_665 ? Se2 K Se2 102.79(4) . 5_665 ? Se3 K Se3 93.14(3) . 6_655 ? Se2 K Se3 106.42(4) . 6_655 ? Se2 K Se3 121.88(4) 5_665 6_655 ? Se3 K Se3 160.20(4) . 2_655 ? Se2 K Se3 65.61(3) . 2_655 ? Se2 K Se3 77.45(3) 5_665 2_655 ? Se3 K Se3 70.94(3) 6_655 2_655 ? Se3 K Se1 69.54(2) . . ? Se2 K Se1 62.75(3) . . ? Se2 K Se1 120.81(4) 5_665 . ? Se3 K Se1 117.16(4) 6_655 . ? Se3 K Se1 127.80(4) 2_655 . ? Se3 K Se3 86.11(3) . 6_665 ? Se2 K Se3 72.61(3) . 6_665 ? Se2 K Se3 60.42(3) 5_665 6_665 ? Se3 K Se3 177.70(5) 6_655 6_665 ? Se3 K Se3 110.24(3) 2_655 6_665 ? Se1 K Se3 60.54(2) . 6_665 ? Se3 K Se1 92.34(3) . 1_655 ? Se2 K Se1 135.27(4) . 1_655 ? Se2 K Se1 63.28(3) 5_665 1_655 ? Se3 K Se1 60.47(2) 6_655 1_655 ? Se3 K Se1 69.80(3) 2_655 1_655 ? Se1 K Se1 161.82(4) . 1_655 ? Se3 K Se1 121.72(4) 6_665 1_655 ? Se3 K Se2 87.24(3) . 5 ? Se2 K Se2 67.77(3) . 5 ? Se2 K Se2 169.65(4) 5_665 5 ? Se3 K Se2 59.63(3) 6_655 5 ? Se3 K Se2 94.28(3) 2_655 5 ? Se1 K Se2 59.62(2) . 5 ? Se3 K Se2 118.13(4) 6_665 5 ? Se1 K Se2 119.97(4) 1_655 5 ? Se3 K K 128.39(5) . 5 ? Se2 K K 57.51(3) . 5 ? Se2 K K 126.00(4) 5_665 5 ? Se3 K K 49.10(3) 6_655 5 ? Se3 K K 48.60(2) 2_655 5 ? Se1 K K 95.39(2) . 5 ? Se3 K K 130.07(4) 6_665 5 ? Se1 K K 94.85(2) 1_655 5 ? Se2 K K 45.83(2) 5 5 ? Se3 K K 50.83(3) . 6_655 ? Se2 K K 132.38(5) . 6_655 ? Se2 K K 123.81(5) 5_665 6_655 ? Se3 K K 42.313(10) 6_655 6_655 ? Se3 K K 112.36(3) 2_655 6_655 ? Se1 K K 96.91(4) . 6_655 ? Se3 K K 136.90(4) 6_665 6_655 ? Se1 K K 69.11(3) 1_655 6_655 ? Se2 K K 64.94(3) 5 6_655 ? K K K 84.90(3) 5 6_655 ? Se3 K K 43.76(3) . 6_665 ? Se2 K K 104.24(4) . 6_665 ? Se2 K K 78.88(3) 5_665 6_665 ? Se3 K K 136.85(4) 6_655 6_665 ? Se3 K K 151.09(4) 2_655 6_665 ? Se1 K K 54.68(2) . 6_665 ? Se3 K K 42.355(9) 6_665 6_665 ? Se1 K K 113.16(4) 1_655 6_665 ? Se2 K K 107.04(4) 5 6_665 ? K K K 149.87(4) 5 6_665 ? K K K 94.56(4) 6_655 6_665 ? Se2 P Se3 117.92(5) 3_554 . ? Se2 P P 106.65(4) 3_554 4 ? Se3 P P 111.41(3) . 4 ? Se2 P Se1 112.30(5) 3_554 6 ? Se3 P Se1 111.91(5) . 6 ? P P Se1 93.89(6) 4 6 ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.778 _refine_diff_density_min -1.178 _refine_diff_density_rms 0.269 #=============================================END data_K2P2Se6_173K _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 660 _chemical_formula_moiety 'P2 Se6, 2(K)' _chemical_formula_sum 'K2 P2 Se6' _chemical_formula_weight 613.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'P' 'P' 0.1023 0.0942 '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' '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 P3(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' _cell_length_a 14.4916(7) _cell_length_b 14.4916(7) _cell_length_c 18.7999(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3419.2(4) _cell_formula_units_Z 12 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2494 _cell_measurement_theta_min 3.25 _cell_measurement_theta_max 26.23 _exptl_crystal_description rod _exptl_crystal_colour 'Orange red' _exptl_crystal_size_max 0.162 _exptl_crystal_size_mid 0.048 _exptl_crystal_size_min 0.048 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.578 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3264 _exptl_absorpt_coefficient_mu 20.209 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.09804 _exptl_absorpt_correction_T_max 0.38357 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 0.3 _diffrn_standards_interval_time 30 _diffrn_standards_decay_% ? _diffrn_reflns_number 21703 _diffrn_reflns_av_R_equivalents 0.0653 _diffrn_reflns_av_sigmaI/netI 0.1105 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 28.29 _reflns_number_total 10294 _reflns_number_gt 5037 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.1d (Crystal Impact Gbr, 2006)' _computing_publication_material 'Bruker SMART' _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^)+(0.0328P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000271(19) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.25(1) _refine_ls_number_reflns 10294 _refine_ls_number_parameters 365 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1492 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1143 _refine_ls_wR_factor_gt 0.0817 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.974 _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 1.3688(5) 0.9676(5) 0.0645(4) 0.0135(13) Uani 1 1 d . . . Se2 Se 0.6125(5) 1.2292(5) 0.0332(4) 0.0171(13) Uani 1 1 d . . . Se3 Se 0.6208(6) 0.9822(6) 0.0147(4) 0.0255(16) Uani 1 1 d . . . Se4 Se 1.1357(5) 0.4907(6) 0.2239(3) 0.0202(13) Uani 1 1 d . . . Se5 Se 0.8603(6) 1.2651(5) 0.2076(4) 0.0190(14) Uani 1 1 d . . . Se6 Se 0.9132(6) 0.5372(5) 0.1757(4) 0.0205(15) Uani 1 1 d . . . Se7 Se 0.8756(5) 0.4608(5) 0.0627(4) 0.0136(13) Uani 1 1 d . . . Se8 Se 1.1483(5) 0.5153(6) 0.0166(4) 0.0288(15) Uani 1 1 d . . . Se9 Se 1.0967(6) 0.7344(6) 0.0324(4) 0.0206(16) Uani 1 1 d . . . Se10 Se 0.6399(5) 0.5185(5) 0.2246(3) 0.0193(13) Uani 1 1 d . . . Se11 Se 1.3824(6) 1.2740(5) 0.2041(4) 0.0183(15) Uani 1 1 d . . . Se12 Se 1.4013(6) 1.5368(6) 0.1759(3) 0.0168(14) Uani 1 1 d . . . Se13 Se 0.3654(5) 0.4607(5) 0.0622(4) 0.0137(13) Uani 1 1 d . . . Se14 Se 0.6081(6) 0.7255(5) 0.0350(4) 0.0168(14) Uani 1 1 d . . . Se15 Se 0.6201(5) 0.4810(5) 0.0146(4) 0.0221(15) Uani 1 1 d . . . Se16 Se 1.3598(6) 0.7670(5) 0.2049(4) 0.0172(14) Uani 1 1 d . . . Se17 Se 0.6374(5) 0.9920(5) 0.2247(3) 0.0182(14) Uani 1 1 d . . . Se18 Se 1.4164(6) 1.0437(5) 0.1775(4) 0.0181(14) Uani 1 1 d . . . Se19 Se 0.8701(5) 0.9560(5) 0.0639(4) 0.0147(13) Uani 1 1 d . . . Se20 Se 0.0925(6) 0.2310(6) 0.0355(4) 0.0220(15) Uani 1 1 d . . . Se21 Se 0.9879(6) 1.1305(5) 0.3494(4) 0.0299(17) Uani 1 1 d . . . Se22 Se 1.1402(5) 1.0149(5) 0.2256(3) 0.0185(13) Uani 1 1 d . . . Se23 Se 0.8845(6) 0.7708(5) 0.2070(4) 0.0192(14) Uani 1 1 d . . . Se24 Se 0.8997(6) 1.0310(5) 0.1781(4) 0.0166(14) Uani 1 1 d . . . K1 K 0.6431(12) 0.7647(11) 0.2114(8) 0.026(3) Uani 1 1 d . . . K2 K 1.1398(12) 1.2618(12) 0.2087(8) 0.030(4) Uani 1 1 d . . . K3 K 1.1393(11) 0.7869(11) 0.2066(8) 0.028(3) Uani 1 1 d . . . K4 K 0.8517(11) 0.7101(11) 0.0339(7) 0.026(3) Uani 1 1 d . . . K5 K 0.7876(12) 0.6401(11) 0.3684(7) 0.025(3) Uani 1 1 d . . . K6 K 0.3789(11) 0.2345(10) 0.0306(7) 0.019(3) Uani 1 1 d . . . K7 K 0.6404(11) 0.2918(9) 0.2050(7) 0.028(3) Uani 1 1 d . . . K8 K 0.3815(11) 0.7381(10) 0.0314(7) 0.025(3) Uani 1 1 d . . . P1 P 0.5302(13) 1.0629(12) 0.0079(9) 0.011(3) Uani 1 1 d . . . P2 P 0.9693(13) 0.4295(13) 0.2324(9) 0.012(3) Uani 1 1 d . . . P3 P 1.0372(12) 0.5712(13) 0.0091(8) 0.013(3) Uani 1 1 d . . . P4 P 1.4711(13) 1.4389(13) 0.2312(8) 0.012(3) Uani 1 1 d . . . P5 P 0.5276(12) 0.5597(13) 0.0086(9) 0.011(3) Uani 1 1 d . . . P6 P 1.4701(12) 0.9309(11) 0.2316(8) 0.011(3) Uani 1 1 d . . . P7 P 1.0319(13) 1.0677(12) 0.0105(9) 0.015(3) Uani 1 1 d . . . P8 P 0.9724(12) 0.9355(12) 0.2344(8) 0.012(3) 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 Se1 0.007(3) 0.018(3) 0.013(3) 0.001(2) -0.001(2) 0.005(2) Se2 0.021(3) 0.010(2) 0.017(3) 0.001(2) -0.005(2) 0.006(2) Se3 0.022(3) 0.027(3) 0.030(3) -0.001(3) -0.004(2) 0.015(3) Se4 0.013(3) 0.032(3) 0.014(3) -0.006(2) 0.000(2) 0.010(3) Se5 0.032(3) 0.010(3) 0.015(3) -0.002(2) -0.004(2) 0.010(2) Se6 0.034(4) 0.019(3) 0.013(3) 0.004(2) 0.003(3) 0.017(3) Se7 0.012(3) 0.017(3) 0.013(3) 0.001(2) 0.000(2) 0.008(2) Se8 0.025(3) 0.035(3) 0.035(3) -0.006(3) -0.007(3) 0.021(3) Se9 0.030(4) 0.015(3) 0.012(3) -0.001(2) -0.004(2) 0.008(3) Se10 0.008(3) 0.027(3) 0.014(2) 0.001(2) -0.001(2) 0.003(2) Se11 0.030(3) 0.014(3) 0.012(3) -0.005(2) -0.006(2) 0.012(2) Se12 0.025(3) 0.021(3) 0.007(3) 0.002(2) 0.003(2) 0.013(3) Se13 0.007(3) 0.016(3) 0.018(3) 0.001(2) 0.002(2) 0.005(2) Se14 0.024(3) 0.011(3) 0.016(3) 0.001(2) -0.005(2) 0.010(2) Se15 0.019(3) 0.025(3) 0.026(3) 0.004(3) -0.001(2) 0.013(3) Se16 0.031(3) 0.009(3) 0.014(3) -0.001(2) -0.005(3) 0.011(2) Se17 0.013(3) 0.026(3) 0.013(2) -0.005(2) -0.002(2) 0.008(2) Se18 0.032(3) 0.017(3) 0.010(3) 0.004(2) 0.006(3) 0.016(3) Se19 0.010(3) 0.013(2) 0.017(3) -0.001(2) 0.000(2) 0.002(2) Se20 0.028(3) 0.019(3) 0.014(3) -0.001(2) -0.007(2) 0.007(2) Se21 0.039(4) 0.015(3) 0.035(3) -0.003(2) 0.005(3) 0.013(3) Se22 0.008(2) 0.026(3) 0.015(2) -0.003(2) -0.001(2) 0.004(2) Se23 0.029(3) 0.014(3) 0.016(3) -0.006(2) -0.008(3) 0.012(2) Se24 0.025(3) 0.017(3) 0.010(3) 0.005(2) 0.006(2) 0.013(2) K1 0.020(6) 0.027(7) 0.031(7) 0.000(5) -0.002(5) 0.012(5) K2 0.021(6) 0.026(8) 0.034(7) -0.006(5) -0.017(5) 0.006(5) K3 0.019(6) 0.016(6) 0.040(8) -0.002(5) -0.014(5) 0.001(5) K4 0.036(7) 0.045(7) 0.006(5) -0.007(5) -0.010(5) 0.027(6) K5 0.042(8) 0.029(6) 0.011(6) -0.007(5) 0.005(5) 0.024(6) K6 0.033(7) 0.023(6) 0.004(6) -0.003(4) 0.000(5) 0.017(6) K7 0.025(6) 0.017(6) 0.031(7) -0.003(5) -0.010(5) 0.003(5) K8 0.040(7) 0.024(7) 0.012(5) -0.002(4) -0.011(5) 0.018(6) P1 0.014(7) 0.014(7) 0.005(8) 0.004(5) 0.002(5) 0.006(6) P2 0.021(7) 0.018(7) 0.007(7) -0.003(5) -0.005(5) 0.018(5) P3 0.017(8) 0.016(7) 0.009(7) 0.009(5) 0.006(5) 0.011(6) P4 0.009(7) 0.018(7) 0.014(7) -0.008(6) -0.003(6) 0.010(6) P5 0.009(6) 0.017(7) 0.007(7) 0.008(5) 0.005(5) 0.007(5) P6 0.011(6) 0.007(6) 0.014(8) -0.008(5) -0.005(5) 0.005(5) P7 0.019(7) 0.010(7) 0.016(7) 0.008(6) 0.003(6) 0.009(6) P8 0.007(6) 0.011(7) 0.017(7) -0.007(6) -0.006(5) 0.004(5) _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 2.297(17) 1_655 ? Se1 Se18 2.334(13) . ? Se1 K8 3.478(14) 1_655 ? Se1 K6 3.849(15) 1_665 ? Se2 P1 2.141(17) . ? Se2 K7 3.325(15) 1_565 ? Se2 K6 3.423(16) 1_565 ? Se2 K7 3.470(15) 3_674 ? Se2 K5 3.606(15) 3_674 ? Se3 P1 2.154(17) . ? Se3 K3 3.317(17) 3_674 ? Se3 K5 3.367(16) 3_674 ? Se3 K8 3.518(15) . ? Se4 P2 2.118(17) . ? Se4 K8 3.346(14) 2_765 ? Se4 K2 3.360(16) 1_545 ? Se5 P2 2.151(17) 1_565 ? Se5 K5 3.321(15) 3_674 ? Se5 K6 3.344(15) 2_665 ? Se5 K7 3.398(15) 1_565 ? Se6 Se7 2.330(8) . ? Se6 P2 2.346(17) . ? Se6 K3 3.509(16) . ? Se6 K7 3.811(14) . ? Se7 P3 2.305(17) . ? Se7 K5 3.484(15) 3_664 ? Se7 K4 3.836(15) . ? Se8 P3 2.138(17) . ? Se8 K8 3.318(14) 1_655 ? Se8 K1 3.363(17) 3_664 ? Se9 P3 2.119(18) . ? Se9 K3 3.348(17) . ? Se9 K4 3.388(15) . ? Se9 K2 3.393(17) 3_674 ? Se10 P4 2.123(17) 1_445 ? Se10 K7 3.309(14) . ? Se10 K5 3.351(15) . ? Se10 K1 3.554(14) . ? Se11 P4 2.133(18) . ? Se11 K6 3.307(15) 1_665 ? Se11 K2 3.433(17) . ? Se11 K4 3.510(16) 2_765 ? Se11 K7 3.616(15) 1_665 ? Se12 Se13 2.342(7) 1_665 ? Se12 P4 2.356(17) . ? Se12 K1 3.473(16) 1_665 ? Se12 K2 3.940(16) . ? Se13 P5 2.286(17) . ? Se13 Se12 2.342(7) 1_445 ? Se13 K6 3.433(15) . ? Se14 P5 2.140(17) . ? Se14 K1 3.361(17) . ? Se14 K8 3.380(15) . ? Se14 K3 3.505(16) 3_674 ? Se14 K4 3.646(15) . ? Se15 P5 2.155(16) . ? Se15 K4 3.359(15) . ? Se15 K7 3.363(15) 3_664 ? Se15 K6 3.547(14) . ? Se16 P6 2.157(15) . ? Se16 K8 3.325(15) 1_655 ? Se16 K3 3.348(15) . ? Se16 K8 3.420(15) 2_765 ? Se17 P6 2.129(16) 1_455 ? Se17 K6 3.329(16) 2_665 ? Se17 K1 3.345(14) . ? Se18 P6 2.363(17) . ? Se18 K7 3.473(14) 1_665 ? Se18 K3 3.915(16) . ? Se19 P7 2.309(17) . ? Se19 Se24 2.347(12) . ? Se19 K4 3.483(15) . ? Se19 K5 3.888(16) 3_674 ? Se20 P7 2.125(17) 1_445 ? Se20 K2 3.311(17) 1_445 ? Se20 K5 3.352(15) 3_564 ? Se20 K1 3.391(16) 3_564 ? Se21 P7 2.126(17) 2_765 ? Se21 K6 3.339(15) 2_665 ? Se21 K2 3.358(17) . ? Se22 P8 2.113(16) . ? Se22 K3 3.317(16) . ? Se22 K4 3.345(14) 2_765 ? Se22 K2 3.595(16) . ? Se23 P8 2.131(16) . ? Se23 K4 3.341(14) . ? Se23 K1 3.456(16) . ? Se23 K5 3.481(15) . ? Se23 K3 3.582(15) . ? Se24 P8 2.368(17) . ? Se24 K2 3.462(16) . ? Se24 K1 3.842(17) . ? K1 Se8 3.363(17) 2_655 ? K1 Se20 3.391(16) 2_665 ? K1 Se12 3.473(16) 1_445 ? K1 K5 4.49(2) . ? K1 K4 4.83(2) . ? K1 K8 4.95(2) . ? K2 Se20 3.310(17) 1_665 ? K2 Se4 3.360(16) 1_565 ? K2 Se9 3.393(17) 2_765 ? K2 K4 4.52(2) 2_765 ? K2 K6 4.97(2) 1_665 ? K2 K5 5.05(2) 3_674 ? K3 Se3 3.317(17) 2_765 ? K3 Se14 3.505(16) 2_765 ? K3 K8 4.473(16) 2_765 ? K3 K4 4.951(18) . ? K4 Se22 3.345(14) 3_674 ? K4 Se11 3.509(16) 3_674 ? K4 K2 4.52(2) 3_674 ? K5 Se5 3.321(15) 2_765 ? K5 Se20 3.352(15) 2_665 ? K5 Se3 3.367(15) 2_765 ? K5 Se7 3.484(15) 2_655 ? K5 Se2 3.606(15) 2_765 ? K5 Se19 3.888(16) 2_765 ? K5 K7 4.95(2) 2_655 ? K5 K2 5.052(19) 2_765 ? K6 Se11 3.307(15) 1_445 ? K6 Se17 3.329(16) 3_564 ? K6 Se5 3.344(15) 3_564 ? K6 Se21 3.339(15) 3_564 ? K6 Se2 3.423(16) 1_545 ? K6 Se1 3.849(15) 1_445 ? K6 K7 4.544(16) 3_664 ? K6 K7 4.76(2) . ? K6 K2 4.97(2) 1_445 ? K7 Se2 3.325(15) 1_545 ? K7 Se15 3.363(15) 2_655 ? K7 Se5 3.398(15) 1_545 ? K7 Se2 3.470(15) 2_765 ? K7 Se18 3.473(14) 1_445 ? K7 Se11 3.616(15) 1_445 ? K7 K6 4.544(16) 2_655 ? K7 K5 4.95(2) 3_664 ? K8 Se8 3.318(14) 1_455 ? K8 Se4 3.346(14) 3_674 ? K8 Se16 3.325(14) 1_455 ? K8 Se16 3.420(15) 3_674 ? K8 Se1 3.478(14) 1_455 ? K8 K3 4.473(16) 3_674 ? P1 P2 2.227(17) 3_674 ? P1 Se1 2.297(17) 1_455 ? P2 Se5 2.150(17) 1_545 ? P2 P1 2.227(17) 2_765 ? P3 P4 2.27(3) 3_674 ? P4 Se10 2.123(17) 1_665 ? P4 P3 2.27(3) 2_765 ? P5 P6 2.236(18) 3_674 ? P6 Se17 2.129(16) 1_655 ? P6 P5 2.236(18) 2_765 ? P7 Se21 2.126(17) 3_674 ? P7 Se20 2.125(17) 1_665 ? P7 P8 2.23(3) 3_674 ? P8 P7 2.23(3) 2_765 ? 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 Se18 99.6(5) 1_655 . ? P1 Se1 K8 88.1(5) 1_655 1_655 ? Se18 Se1 K8 118.0(4) . 1_655 ? P1 Se1 K6 78.7(5) 1_655 1_665 ? Se18 Se1 K6 79.8(3) . 1_665 ? K8 Se1 K6 159.7(3) 1_655 1_665 ? P1 Se2 K7 116.5(5) . 1_565 ? P1 Se2 K6 91.2(5) . 1_565 ? K7 Se2 K6 89.7(4) 1_565 1_565 ? P1 Se2 K7 105.4(5) . 3_674 ? K7 Se2 K7 137.5(3) 1_565 3_674 ? K6 Se2 K7 82.5(3) 1_565 3_674 ? P1 Se2 K5 86.5(5) . 3_674 ? K7 Se2 K5 91.1(4) 1_565 3_674 ? K6 Se2 K5 177.7(4) 1_565 3_674 ? K7 Se2 K5 98.4(4) 3_674 3_674 ? P1 Se3 K3 120.4(6) . 3_674 ? P1 Se3 K5 92.6(5) . 3_674 ? K3 Se3 K5 107.1(4) 3_674 3_674 ? P1 Se3 K8 89.4(5) . . ? K3 Se3 K8 81.7(3) 3_674 . ? K5 Se3 K8 168.2(4) 3_674 . ? P2 Se4 K8 110.4(6) . 2_765 ? P2 Se4 K2 99.8(5) . 1_545 ? K8 Se4 K2 116.5(4) 2_765 1_545 ? P2 Se5 K5 112.9(6) 1_565 3_674 ? P2 Se5 K6 105.7(6) 1_565 2_665 ? K5 Se5 K6 141.3(5) 3_674 2_665 ? P2 Se5 K7 95.1(5) 1_565 1_565 ? K5 Se5 K7 94.9(4) 3_674 1_565 ? K6 Se5 K7 84.8(4) 2_665 1_565 ? Se7 Se6 P2 100.1(5) . . ? Se7 Se6 K3 121.1(4) . . ? P2 Se6 K3 98.9(5) . . ? Se7 Se6 K7 78.6(3) . . ? P2 Se6 K7 81.7(5) . . ? K3 Se6 K7 159.5(4) . . ? P3 Se7 Se6 98.8(5) . . ? P3 Se7 K5 101.0(5) . 3_664 ? Se6 Se7 K5 120.4(3) . 3_664 ? P3 Se7 K4 79.9(5) . . ? Se6 Se7 K4 77.9(3) . . ? K5 Se7 K4 160.9(3) 3_664 . ? P3 Se8 K8 103.3(6) . 1_655 ? P3 Se8 K1 110.8(5) . 3_664 ? K8 Se8 K1 116.3(4) 1_655 3_664 ? P3 Se9 K3 112.4(5) . . ? P3 Se9 K4 93.8(5) . . ? K3 Se9 K4 94.6(4) . . ? P3 Se9 K2 107.1(5) . 3_674 ? K3 Se9 K2 140.4(5) . 3_674 ? K4 Se9 K2 83.6(4) . 3_674 ? P4 Se10 K7 92.3(5) 1_445 . ? P4 Se10 K5 119.9(5) 1_445 . ? K7 Se10 K5 107.1(4) . . ? P4 Se10 K1 89.0(5) 1_445 . ? K7 Se10 K1 169.6(4) . . ? K5 Se10 K1 81.0(4) . . ? P4 Se11 K6 112.2(6) . 1_665 ? P4 Se11 K2 94.6(5) . . ? K6 Se11 K2 95.1(4) 1_665 . ? P4 Se11 K4 104.8(5) . 2_765 ? K6 Se11 K4 143.0(4) 1_665 2_765 ? K2 Se11 K4 81.3(4) . 2_765 ? P4 Se11 K7 84.1(5) . 1_665 ? K6 Se11 K7 86.7(4) 1_665 1_665 ? K2 Se11 K7 178.0(4) . 1_665 ? K4 Se11 K7 97.7(4) 2_765 1_665 ? Se13 Se12 P4 100.4(5) 1_665 . ? Se13 Se12 K1 120.3(4) 1_665 1_665 ? P4 Se12 K1 87.4(5) . 1_665 ? Se13 Se12 K2 78.0(3) 1_665 . ? P4 Se12 K2 78.9(5) . . ? K1 Se12 K2 159.2(4) 1_665 . ? P5 Se13 Se12 101.0(5) . 1_445 ? P5 Se13 K6 89.5(5) . . ? Se12 Se13 K6 120.2(4) 1_445 . ? P5 Se14 K1 111.7(6) . . ? P5 Se14 K8 93.2(5) . . ? K1 Se14 K8 94.5(4) . . ? P5 Se14 K3 105.7(6) . 3_674 ? K1 Se14 K3 142.5(4) . 3_674 ? K8 Se14 K3 81.0(3) . 3_674 ? P5 Se14 K4 86.1(5) . . ? K1 Se14 K4 86.9(4) . . ? K8 Se14 K4 178.5(4) . . ? K3 Se14 K4 97.9(4) 3_674 . ? P5 Se15 K4 93.5(5) . . ? P5 Se15 K7 121.2(6) . 3_664 ? K4 Se15 K7 105.9(4) . 3_664 ? P5 Se15 K6 88.7(5) . . ? K4 Se15 K6 168.8(4) . . ? K7 Se15 K6 82.2(3) 3_664 . ? P6 Se16 K8 107.6(5) . 1_655 ? P6 Se16 K3 96.7(5) . . ? K8 Se16 K3 100.0(4) 1_655 . ? P6 Se16 K8 104.9(5) . 2_765 ? K8 Se16 K8 146.8(3) 1_655 2_765 ? K3 Se16 K8 82.7(4) . 2_765 ? P6 Se17 K6 111.7(5) 1_455 2_665 ? P6 Se17 K1 100.3(5) 1_455 . ? K6 Se17 K1 115.6(4) 2_665 . ? Se1 Se18 P6 100.8(5) . . ? Se1 Se18 K7 121.8(4) . 1_665 ? P6 Se18 K7 101.0(5) . 1_665 ? Se1 Se18 K3 76.0(3) . . ? P6 Se18 K3 79.5(4) . . ? K7 Se18 K3 161.2(4) 1_665 . ? P7 Se19 Se24 100.7(5) . . ? P7 Se19 K4 100.3(5) . . ? Se24 Se19 K4 121.6(4) . . ? P7 Se19 K5 78.4(5) . 3_674 ? Se24 Se19 K5 76.6(3) . 3_674 ? K4 Se19 K5 161.3(3) . 3_674 ? P7 Se20 K2 108.1(6) 1_445 1_445 ? P7 Se20 K5 94.3(5) 1_445 3_564 ? K2 Se20 K5 98.6(4) 1_445 3_564 ? P7 Se20 K1 106.1(6) 1_445 3_564 ? K2 Se20 K1 145.5(5) 1_445 3_564 ? K5 Se20 K1 83.5(4) 3_564 3_564 ? P7 Se21 K6 104.0(6) 2_765 2_665 ? P7 Se21 K2 111.9(6) 2_765 . ? K6 Se21 K2 114.1(5) 2_665 . ? P8 Se22 K3 92.0(5) . . ? P8 Se22 K4 119.4(5) . 2_765 ? K3 Se22 K4 108.1(4) . 2_765 ? P8 Se22 K2 88.6(5) . . ? K3 Se22 K2 168.8(4) . . ? K4 Se22 K2 81.2(4) 2_765 . ? P8 Se23 K4 117.2(6) . . ? P8 Se23 K1 93.1(5) . . ? K4 Se23 K1 90.5(4) . . ? P8 Se23 K5 104.5(5) . . ? K4 Se23 K5 137.8(4) . . ? K1 Se23 K5 80.6(4) . . ? P8 Se23 K3 84.7(5) . . ? K4 Se23 K3 91.2(4) . . ? K1 Se23 K3 177.7(4) . . ? K5 Se23 K3 99.2(4) . . ? Se19 Se24 P8 99.8(5) . . ? Se19 Se24 K2 117.5(4) . . ? P8 Se24 K2 88.0(5) . . ? Se19 Se24 K1 79.8(3) . . ? P8 Se24 K1 80.2(5) . . ? K2 Se24 K1 160.7(4) . . ? Se17 K1 Se8 98.9(4) . 2_655 ? Se17 K1 Se14 99.5(4) . . ? Se8 K1 Se14 131.8(5) 2_655 . ? Se17 K1 Se20 78.5(4) . 2_665 ? Se8 K1 Se20 68.4(3) 2_655 2_665 ? Se14 K1 Se20 159.4(6) . 2_665 ? Se17 K1 Se23 120.0(5) . . ? Se8 K1 Se23 115.4(4) 2_655 . ? Se14 K1 Se23 92.6(4) . . ? Se20 K1 Se23 71.5(3) 2_665 . ? Se17 K1 Se12 116.1(4) . 1_445 ? Se8 K1 Se12 62.1(3) 2_655 1_445 ? Se14 K1 Se12 69.8(3) . 1_445 ? Se20 K1 Se12 129.8(5) 2_665 1_445 ? Se23 K1 Se12 123.2(4) . 1_445 ? Se17 K1 Se10 171.5(5) . . ? Se8 K1 Se10 73.4(3) 2_655 . ? Se14 K1 Se10 88.5(4) . . ? Se20 K1 Se10 95.1(4) 2_665 . ? Se23 K1 Se10 62.1(3) . . ? Se12 K1 Se10 63.8(3) 1_445 . ? Se17 K1 Se24 60.8(3) . . ? Se8 K1 Se24 137.7(5) 2_655 . ? Se14 K1 Se24 89.8(4) . . ? Se20 K1 Se24 71.1(3) 2_665 . ? Se23 K1 Se24 60.7(3) . . ? Se12 K1 Se24 159.0(5) 1_445 . ? Se10 K1 Se24 122.7(4) . . ? Se17 K1 K5 126.4(4) . . ? Se8 K1 K5 65.5(3) 2_655 . ? Se14 K1 K5 130.0(5) . . ? Se20 K1 K5 47.9(3) 2_665 . ? Se23 K1 K5 49.9(3) . . ? Se12 K1 K5 101.3(3) 1_445 . ? Se10 K1 K5 47.5(3) . . ? Se24 K1 K5 95.7(3) . . ? Se17 K1 K4 122.6(4) . . ? Se8 K1 K4 138.4(4) 2_655 . ? Se14 K1 K4 49.0(2) . . ? Se20 K1 K4 114.8(4) 2_665 . ? Se23 K1 K4 43.8(3) . . ? Se12 K1 K4 97.4(3) 1_445 . ? Se10 K1 K4 65.1(3) . . ? Se24 K1 K4 71.4(3) . . ? K5 K1 K4 86.1(4) . . ? Se17 K1 K8 74.5(3) . . ? Se8 K1 K8 101.9(4) 2_655 . ? Se14 K1 K8 42.9(2) . . ? Se20 K1 K8 149.5(4) 2_665 . ? Se23 K1 K8 135.3(4) . . ? Se12 K1 K8 54.9(3) 1_445 . ? Se10 K1 K8 110.1(3) . . ? Se24 K1 K8 106.6(3) . . ? K5 K1 K8 155.7(3) . . ? K4 K1 K8 91.9(3) . . ? Se20 K2 Se4 96.5(4) 1_665 1_565 ? Se20 K2 Se21 131.7(5) 1_665 . ? Se4 K2 Se21 99.3(5) 1_565 . ? Se20 K2 Se9 160.8(6) 1_665 2_765 ? Se4 K2 Se9 76.9(4) 1_565 2_765 ? Se21 K2 Se9 67.5(3) . 2_765 ? Se20 K2 Se11 96.9(5) 1_665 . ? Se4 K2 Se11 118.3(5) 1_565 . ? Se21 K2 Se11 114.4(5) . . ? Se9 K2 Se11 71.5(4) 2_765 . ? Se20 K2 Se24 70.5(3) 1_665 . ? Se4 K2 Se24 117.6(5) 1_565 . ? Se21 K2 Se24 61.7(3) . . ? Se9 K2 Se24 128.6(5) 2_765 . ? Se11 K2 Se24 123.7(5) . . ? Se20 K2 Se22 93.2(4) 1_665 . ? Se4 K2 Se22 170.0(5) 1_565 . ? Se21 K2 Se22 72.1(4) . . ? Se9 K2 Se22 94.7(4) 2_765 . ? Se11 K2 Se22 62.7(3) . . ? Se24 K2 Se22 63.5(3) . . ? Se20 K2 Se12 90.7(4) 1_665 . ? Se4 K2 Se12 59.8(3) 1_565 . ? Se21 K2 Se12 136.3(5) . . ? Se9 K2 Se12 70.3(3) 2_765 . ? Se11 K2 Se12 60.1(3) . . ? Se24 K2 Se12 160.9(5) . . ? Se22 K2 Se12 122.8(4) . . ? Se20 K2 K4 134.7(5) 1_665 2_765 ? Se4 K2 K4 125.0(4) 1_565 2_765 ? Se21 K2 K4 64.4(3) . 2_765 ? Se9 K2 K4 48.1(3) 2_765 2_765 ? Se11 K2 K4 50.1(3) . 2_765 ? Se24 K2 K4 100.5(4) . 2_765 ? Se22 K2 K4 47.0(3) . 2_765 ? Se12 K2 K4 95.1(3) . 2_765 ? Se20 K2 K6 55.5(3) 1_665 1_665 ? Se4 K2 K6 119.5(4) 1_565 1_665 ? Se21 K2 K6 140.4(4) . 1_665 ? Se9 K2 K6 111.9(5) 2_765 1_665 ? Se11 K2 K6 41.5(3) . 1_665 ? Se24 K2 K6 102.4(3) . 1_665 ? Se22 K2 K6 68.4(3) . 1_665 ? Se12 K2 K6 67.6(3) . 1_665 ? K4 K2 K6 85.7(4) 2_765 1_665 ? Se20 K2 K5 41.0(2) 1_665 3_674 ? Se4 K2 K5 77.0(4) 1_565 3_674 ? Se21 K2 K5 99.7(4) . 3_674 ? Se9 K2 K5 148.3(5) 2_765 3_674 ? Se11 K2 K5 137.9(5) . 3_674 ? Se24 K2 K5 52.9(3) . 3_674 ? Se22 K2 K5 109.1(3) . 3_674 ? Se12 K2 K5 110.5(3) . 3_674 ? K4 K2 K5 153.2(3) 2_765 3_674 ? K6 K2 K5 96.4(3) 1_665 3_674 ? Se22 K3 Se3 107.2(5) . 2_765 ? Se22 K3 Se9 103.9(4) . . ? Se3 K3 Se9 131.2(5) 2_765 . ? Se22 K3 Se16 123.9(5) . . ? Se3 K3 Se16 99.9(4) 2_765 . ? Se9 K3 Se16 92.7(4) . . ? Se22 K3 Se14 77.8(3) . 2_765 ? Se3 K3 Se14 64.7(3) 2_765 2_765 ? Se9 K3 Se14 160.3(5) . 2_765 ? Se16 K3 Se14 71.0(3) . 2_765 ? Se22 K3 Se6 125.6(4) . . ? Se3 K3 Se6 62.9(3) 2_765 . ? Se9 K3 Se6 68.4(3) . . ? Se16 K3 Se6 110.4(4) . . ? Se14 K3 Se6 126.9(5) 2_765 . ? Se22 K3 Se23 63.6(3) . . ? Se3 K3 Se23 76.1(3) 2_765 . ? Se9 K3 Se23 85.4(3) . . ? Se16 K3 Se23 172.5(5) . . ? Se14 K3 Se23 112.2(4) 2_765 . ? Se6 K3 Se23 62.1(3) . . ? Se22 K3 Se18 65.0(3) . . ? Se3 K3 Se18 133.5(4) 2_765 . ? Se9 K3 Se18 93.7(4) . . ? Se16 K3 Se18 60.7(3) . . ? Se14 K3 Se18 68.9(3) 2_765 . ? Se6 K3 Se18 160.4(5) . . ? Se23 K3 Se18 126.6(4) . . ? Se22 K3 K8 125.9(4) . 2_765 ? Se3 K3 K8 51.1(3) 2_765 2_765 ? Se9 K3 K8 128.0(4) . 2_765 ? Se16 K3 K8 49.3(3) . 2_765 ? Se14 K3 K8 48.3(2) 2_765 2_765 ? Se6 K3 K8 90.8(4) . 2_765 ? Se23 K3 K8 127.2(4) . 2_765 ? Se18 K3 K8 94.5(3) . 2_765 ? Se22 K3 K4 83.0(3) . . ? Se3 K3 K4 105.4(4) 2_765 . ? Se9 K3 K4 43.0(2) . . ? Se16 K3 K4 135.0(4) . . ? Se14 K3 K4 154.0(4) 2_765 . ? Se6 K3 K4 54.0(3) . . ? Se23 K3 K4 42.4(3) . . ? Se18 K3 K4 118.0(3) . . ? K8 K3 K4 144.8(4) 2_765 . ? Se23 K4 Se22 130.5(5) . 3_674 ? Se23 K4 Se15 107.8(4) . . ? Se22 K4 Se15 106.3(4) 3_674 . ? Se23 K4 Se9 88.7(4) . . ? Se22 K4 Se9 99.6(4) 3_674 . ? Se15 K4 Se9 125.4(5) . . ? Se23 K4 Se19 69.2(3) . . ? Se22 K4 Se19 62.2(3) 3_674 . ? Se15 K4 Se19 123.8(4) . . ? Se9 K4 Se19 110.8(4) . . ? Se23 K4 Se11 157.3(5) . 3_674 ? Se22 K4 Se11 64.5(3) 3_674 3_674 ? Se15 K4 Se11 78.5(3) . 3_674 ? Se9 K4 Se11 70.6(3) . 3_674 ? Se19 K4 Se11 126.1(4) . 3_674 ? Se23 K4 Se14 89.6(4) . . ? Se22 K4 Se14 75.5(3) 3_674 . ? Se15 K4 Se14 62.7(3) . . ? Se9 K4 Se14 171.8(5) . . ? Se19 K4 Se14 61.2(3) . . ? Se11 K4 Se14 112.2(4) 3_674 . ? Se23 K4 Se7 92.4(3) . . ? Se22 K4 Se7 134.1(4) 3_674 . ? Se15 K4 Se7 66.4(3) . . ? Se9 K4 Se7 61.0(3) . . ? Se19 K4 Se7 160.7(4) . . ? Se11 K4 Se7 69.7(3) 3_674 . ? Se14 K4 Se7 127.1(4) . . ? Se23 K4 K2 122.7(5) . 3_674 ? Se22 K4 K2 51.8(3) 3_674 3_674 ? Se15 K4 K2 127.0(4) . 3_674 ? Se9 K4 K2 48.2(3) . 3_674 ? Se19 K4 K2 90.5(3) . 3_674 ? Se11 K4 K2 48.6(3) 3_674 3_674 ? Se14 K4 K2 127.3(4) . 3_674 ? Se7 K4 K2 94.7(3) . 3_674 ? Se23 K4 K1 45.7(2) . . ? Se22 K4 K1 108.2(4) 3_674 . ? Se15 K4 K1 80.7(4) . . ? Se9 K4 K1 134.3(4) . . ? Se19 K4 K1 56.9(3) . . ? Se11 K4 K1 154.6(4) 3_674 . ? Se14 K4 K1 44.1(3) . . ? Se7 K4 K1 114.6(3) . . ? K2 K4 K1 147.1(3) 3_674 . ? Se23 K4 K3 46.3(2) . . ? Se22 K4 K3 125.2(3) 3_674 . ? Se15 K4 K3 127.3(3) . . ? Se9 K4 K3 42.4(3) . . ? Se19 K4 K3 92.2(3) . . ? Se11 K4 K3 112.2(4) 3_674 . ? Se14 K4 K3 135.6(4) . . ? Se7 K4 K3 69.9(3) . . ? K2 K4 K3 84.0(4) 3_674 . ? K1 K4 K3 92.1(3) . . ? Se5 K5 Se20 93.7(4) 2_765 2_665 ? Se5 K5 Se10 131.4(5) 2_765 . ? Se20 K5 Se10 99.7(4) 2_665 . ? Se5 K5 Se3 104.0(4) 2_765 2_765 ? Se20 K5 Se3 124.1(5) 2_665 2_765 ? Se10 K5 Se3 106.2(4) . 2_765 ? Se5 K5 Se23 161.6(5) 2_765 . ? Se20 K5 Se23 71.6(3) 2_665 . ? Se10 K5 Se23 63.9(3) . . ? Se3 K5 Se23 76.9(3) 2_765 . ? Se5 K5 Se7 69.0(3) 2_765 2_655 ? Se20 K5 Se7 110.9(4) 2_665 2_655 ? Se10 K5 Se7 62.5(3) . 2_655 ? Se3 K5 Se7 125.0(4) 2_765 2_655 ? Se23 K5 Se7 125.9(4) . 2_655 ? Se5 K5 Se2 85.3(4) 2_765 2_765 ? Se20 K5 Se2 172.6(5) 2_665 2_765 ? Se10 K5 Se2 75.7(3) . 2_765 ? Se3 K5 Se2 63.2(3) 2_765 2_765 ? Se23 K5 Se2 110.7(4) . 2_765 ? Se7 K5 Se2 61.9(3) 2_655 2_765 ? Se5 K5 Se19 94.2(4) 2_765 2_765 ? Se20 K5 Se19 61.0(3) 2_665 2_765 ? Se10 K5 Se19 133.0(4) . 2_765 ? Se3 K5 Se19 65.1(3) 2_765 2_765 ? Se23 K5 Se19 69.3(3) . 2_765 ? Se7 K5 Se19 161.5(4) 2_655 2_765 ? Se2 K5 Se19 126.4(4) 2_765 2_765 ? Se5 K5 K1 127.8(5) 2_765 . ? Se20 K5 K1 48.6(3) 2_665 . ? Se10 K5 K1 51.5(3) . . ? Se3 K5 K1 126.2(4) 2_765 . ? Se23 K5 K1 49.4(3) . . ? Se7 K5 K1 90.2(3) 2_655 . ? Se2 K5 K1 127.2(4) 2_765 . ? Se19 K5 K1 94.6(3) 2_765 . ? Se5 K5 K7 43.1(2) 2_765 2_655 ? Se20 K5 K7 136.0(4) 2_665 2_655 ? Se10 K5 K7 104.9(4) . 2_655 ? Se3 K5 K7 82.9(3) 2_765 2_655 ? Se23 K5 K7 152.3(4) . 2_655 ? Se7 K5 K7 54.1(2) 2_655 2_655 ? Se2 K5 K7 42.2(3) 2_765 2_655 ? Se19 K5 K7 118.5(3) 2_765 2_655 ? K1 K5 K7 144.2(3) . 2_655 ? Se5 K5 K2 53.5(2) 2_765 2_765 ? Se20 K5 K2 40.4(3) 2_665 2_765 ? Se10 K5 K2 127.5(4) . 2_765 ? Se3 K5 K2 123.8(4) 2_765 2_765 ? Se23 K5 K2 110.4(4) . 2_765 ? Se7 K5 K2 96.3(3) 2_655 2_765 ? Se2 K5 K2 138.7(4) 2_765 2_765 ? Se19 K5 K2 66.6(3) 2_765 2_765 ? K1 K5 K2 84.0(4) . 2_765 ? K7 K5 K2 96.5(3) 2_655 2_765 ? Se11 K6 Se17 132.5(5) 1_445 3_564 ? Se11 K6 Se5 160.5(5) 1_445 3_564 ? Se17 K6 Se5 66.6(3) 3_564 3_564 ? Se11 K6 Se21 99.6(4) 1_445 3_564 ? Se17 K6 Se21 97.5(4) 3_564 3_564 ? Se5 K6 Se21 78.7(3) 3_564 3_564 ? Se11 K6 Se2 93.5(4) 1_445 1_545 ? Se17 K6 Se2 113.9(4) 3_564 1_545 ? Se5 K6 Se2 71.8(3) 3_564 1_545 ? Se21 K6 Se2 121.9(4) 3_564 1_545 ? Se11 K6 Se13 70.6(3) 1_445 . ? Se17 K6 Se13 62.0(3) 3_564 . ? Se5 K6 Se13 128.0(5) 3_564 . ? Se21 K6 Se13 114.5(5) 3_564 . ? Se2 K6 Se13 123.2(4) 1_545 . ? Se11 K6 Se15 89.3(4) 1_445 . ? Se17 K6 Se15 72.4(3) 3_564 . ? Se5 K6 Se15 94.7(4) 3_564 . ? Se21 K6 Se15 169.6(5) 3_564 . ? Se2 K6 Se15 62.4(3) 1_545 . ? Se13 K6 Se15 63.3(3) . . ? Se11 K6 Se1 90.0(4) 1_445 1_445 ? Se17 K6 Se1 136.8(4) 3_564 1_445 ? Se5 K6 Se1 71.8(3) 3_564 1_445 ? Se21 K6 Se1 62.5(3) 3_564 1_445 ? Se2 K6 Se1 61.1(3) 1_545 1_445 ? Se13 K6 Se1 160.0(4) . 1_445 ? Se15 K6 Se1 123.3(4) . 1_445 ? Se11 K6 K7 130.1(4) 1_445 3_664 ? Se17 K6 K7 64.8(3) 3_564 3_664 ? Se5 K6 K7 48.1(3) 3_564 3_664 ? Se21 K6 K7 126.8(4) 3_564 3_664 ? Se2 K6 K7 49.2(3) 1_545 3_664 ? Se13 K6 K7 100.7(4) . 3_664 ? Se15 K6 K7 47.2(3) . 3_664 ? Se1 K6 K7 95.7(4) 1_445 3_664 ? Se11 K6 K7 49.3(2) 1_445 . ? Se17 K6 K7 137.9(4) 3_564 . ? Se5 K6 K7 115.8(5) 3_564 . ? Se21 K6 K7 124.6(4) 3_564 . ? Se2 K6 K7 44.3(3) 1_545 . ? Se13 K6 K7 97.8(3) . . ? Se15 K6 K7 65.5(3) . . ? Se1 K6 K7 71.9(3) 1_445 . ? K7 K6 K7 85.8(3) 3_664 . ? Se11 K6 K2 43.4(2) 1_445 1_445 ? Se17 K6 K2 102.3(4) 3_564 1_445 ? Se5 K6 K2 148.2(4) 3_564 1_445 ? Se21 K6 K2 73.3(3) 3_564 1_445 ? Se2 K6 K2 136.7(4) 1_545 1_445 ? Se13 K6 K2 55.4(3) . 1_445 ? Se15 K6 K2 110.6(3) . 1_445 ? Se1 K6 K2 106.9(3) 1_445 1_445 ? K7 K6 K2 155.7(3) 3_664 1_445 ? K7 K6 K2 92.8(2) . 1_445 ? Se10 K7 Se2 108.6(4) . 1_545 ? Se10 K7 Se15 107.7(4) . 2_655 ? Se2 K7 Se15 130.1(4) 1_545 2_655 ? Se10 K7 Se5 125.4(4) . 1_545 ? Se2 K7 Se5 88.6(4) 1_545 1_545 ? Se15 K7 Se5 97.2(4) 2_655 1_545 ? Se10 K7 Se2 78.2(3) . 2_765 ? Se2 K7 Se2 157.4(5) 1_545 2_765 ? Se15 K7 Se2 63.8(3) 2_655 2_765 ? Se5 K7 Se2 70.6(3) 1_545 2_765 ? Se10 K7 Se18 125.4(4) . 1_445 ? Se2 K7 Se18 69.5(3) 1_545 1_445 ? Se15 K7 Se18 61.8(3) 2_655 1_445 ? Se5 K7 Se18 109.2(4) 1_545 1_445 ? Se2 K7 Se18 125.0(4) 2_765 1_445 ? Se10 K7 Se11 63.7(3) . 1_445 ? Se2 K7 Se11 89.7(4) 1_545 1_445 ? Se15 K7 Se11 77.0(3) 2_655 1_445 ? Se5 K7 Se11 170.8(4) 1_545 1_445 ? Se2 K7 Se11 112.2(4) 2_765 1_445 ? Se18 K7 Se11 61.8(3) 1_445 1_445 ? Se10 K7 Se6 66.8(3) . . ? Se2 K7 Se6 92.4(4) 1_545 . ? Se15 K7 Se6 133.4(4) 2_655 . ? Se5 K7 Se6 60.9(3) 1_545 . ? Se2 K7 Se6 70.0(3) 2_765 . ? Se18 K7 Se6 160.2(4) 1_445 . ? Se11 K7 Se6 128.2(4) 1_445 . ? Se10 K7 K6 126.4(4) . 2_655 ? Se2 K7 K6 122.2(4) 1_545 2_655 ? Se15 K7 K6 50.7(3) 2_655 2_655 ? Se5 K7 K6 47.1(3) 1_545 2_655 ? Se2 K7 K6 48.3(3) 2_765 2_655 ? Se18 K7 K6 89.8(3) 1_445 2_655 ? Se11 K7 K6 127.7(4) 1_445 2_655 ? Se6 K7 K6 93.6(4) . 2_655 ? Se10 K7 K6 81.6(3) . . ? Se2 K7 K6 46.0(2) 1_545 . ? Se15 K7 K6 109.1(4) 2_655 . ? Se5 K7 K6 134.4(4) 1_545 . ? Se2 K7 K6 154.6(4) 2_765 . ? Se18 K7 K6 57.7(3) 1_445 . ? Se11 K7 K6 43.9(3) 1_445 . ? Se6 K7 K6 115.3(3) . . ? K6 K7 K6 147.2(3) 2_655 . ? Se10 K7 K5 127.8(3) . 3_664 ? Se2 K7 K5 46.7(2) 1_545 3_664 ? Se15 K7 K5 122.9(3) 2_655 3_664 ? Se5 K7 K5 41.9(3) 1_545 3_664 ? Se2 K7 K5 111.7(4) 2_765 3_664 ? Se18 K7 K5 91.7(3) 1_445 3_664 ? Se11 K7 K5 136.1(4) 1_445 3_664 ? Se6 K7 K5 69.4(3) . 3_664 ? K6 K7 K5 82.8(3) 2_655 3_664 ? K6 K7 K5 92.7(3) . 3_664 ? Se8 K8 Se4 97.3(4) 1_455 3_674 ? Se8 K8 Se16 95.2(4) 1_455 1_455 ? Se4 K8 Se16 131.6(4) 3_674 1_455 ? Se8 K8 Se14 119.6(4) 1_455 . ? Se4 K8 Se14 115.2(4) 3_674 . ? Se16 K8 Se14 98.2(4) 1_455 . ? Se8 K8 Se16 78.0(3) 1_455 3_674 ? Se4 K8 Se16 66.3(3) 3_674 3_674 ? Se16 K8 Se16 162.0(4) 1_455 3_674 ? Se14 K8 Se16 71.6(3) . 3_674 ? Se8 K8 Se1 115.5(4) 1_455 1_455 ? Se4 K8 Se1 62.8(3) 3_674 1_455 ? Se16 K8 Se1 69.5(3) 1_455 1_455 ? Se14 K8 Se1 124.4(4) . 1_455 ? Se16 K8 Se1 128.5(4) 3_674 1_455 ? Se8 K8 Se3 169.6(4) 1_455 . ? Se4 K8 Se3 72.8(3) 3_674 . ? Se16 K8 Se3 94.0(4) 1_455 . ? Se14 K8 Se3 63.9(3) . . ? Se16 K8 Se3 94.7(4) 3_674 . ? Se1 K8 Se3 63.3(3) 1_455 . ? Se8 K8 K3 125.9(4) 1_455 3_674 ? Se4 K8 K3 64.5(3) 3_674 3_674 ? Se16 K8 K3 136.0(4) 1_455 3_674 ? Se14 K8 K3 50.7(3) . 3_674 ? Se16 K8 K3 47.9(3) 3_674 3_674 ? Se1 K8 K3 100.7(4) 1_455 3_674 ? Se3 K8 K3 47.2(3) . 3_674 ? Se8 K8 K1 120.0(3) 1_455 . ? Se4 K8 K1 142.2(4) 3_674 . ? Se16 K8 K1 55.7(2) 1_455 . ? Se14 K8 K1 42.6(3) . . ? Se16 K8 K1 113.3(4) 3_674 . ? Se1 K8 K1 102.0(3) 1_455 . ? Se3 K8 K1 69.6(3) . . ? K3 K8 K1 87.1(4) 3_674 . ? Se2 P1 Se3 116.8(8) . . ? Se2 P1 P2 112.3(9) . 3_674 ? Se3 P1 P2 106.1(9) . 3_674 ? Se2 P1 Se1 113.6(7) . 1_455 ? Se3 P1 Se1 111.1(7) . 1_455 ? P2 P1 Se1 94.6(7) 3_674 1_455 ? Se4 P2 Se5 120.0(7) . 1_545 ? Se4 P2 P1 107.5(9) . 2_765 ? Se5 P2 P1 110.1(9) 1_545 2_765 ? Se4 P2 Se6 112.8(8) . . ? Se5 P2 Se6 109.4(7) 1_545 . ? P1 P2 Se6 94.0(6) 2_765 . ? Se9 P3 Se8 116.5(8) . . ? Se9 P3 P4 111.7(6) . 3_674 ? Se8 P3 P4 106.0(7) . 3_674 ? Se9 P3 Se7 112.9(7) . . ? Se8 P3 Se7 113.9(7) . . ? P4 P3 Se7 93.2(8) 3_674 . ? Se11 P4 Se10 118.7(7) . 1_665 ? Se11 P4 P3 110.5(7) . 2_765 ? Se10 P4 P3 107.3(7) 1_665 2_765 ? Se11 P4 Se12 111.7(7) . . ? Se10 P4 Se12 111.9(8) 1_665 . ? P3 P4 Se12 93.9(8) 2_765 . ? Se14 P5 Se15 116.6(7) . . ? Se14 P5 P6 111.9(9) . 3_674 ? Se15 P5 P6 105.7(8) . 3_674 ? Se14 P5 Se13 114.5(7) . . ? Se15 P5 Se13 111.2(7) . . ? P6 P5 Se13 94.5(6) 3_674 . ? Se17 P6 Se16 120.4(7) 1_655 . ? Se17 P6 P5 105.8(8) 1_655 2_765 ? Se16 P6 P5 110.7(9) . 2_765 ? Se17 P6 Se18 112.7(7) 1_655 . ? Se16 P6 Se18 110.0(7) . . ? P5 P6 Se18 93.7(6) 2_765 . ? Se21 P7 Se20 116.2(8) 3_674 1_665 ? Se21 P7 P8 105.7(8) 3_674 3_674 ? Se20 P7 P8 112.1(6) 1_665 3_674 ? Se21 P7 Se19 114.0(7) 3_674 . ? Se20 P7 Se19 113.2(7) 1_665 . ? P8 P7 Se19 93.0(9) 3_674 . ? Se22 P8 Se23 118.2(8) . . ? Se22 P8 P7 107.8(7) . 2_765 ? Se23 P8 P7 111.5(7) . 2_765 ? Se22 P8 Se24 112.0(7) . . ? Se23 P8 Se24 110.8(7) . . ? P7 P8 Se24 94.0(9) 2_765 . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.658 _refine_diff_density_min -1.630 _refine_diff_density_rms 0.309 #=============================================END data_try3ti _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 637 _chemical_formula_moiety 'P2 Se6, 2(Rb)' _chemical_formula_sum 'P2 Rb2 Se6' _chemical_formula_weight 706.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source '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' 'Rb' 'Rb' -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P3(1)21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' 'y, x, -z' 'x-y, -y, -z+2/3' '-x, -x+y, -z+1/3' _cell_length_a 7.2982(5) _cell_length_b 7.2982(5) _cell_length_c 19.0019(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 876.51(11) _cell_formula_units_Z 3 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6460 _cell_measurement_theta_min 3.21 _cell_measurement_theta_max 33.59 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.059 _exptl_crystal_size_mid 0.040 _exptl_crystal_size_min 0.035 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.016 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 924 _exptl_absorpt_coefficient_mu 27.272 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.4322 _exptl_absorpt_correction_T_max 0.5763 _exptl_absorpt_process_details 'Using XRED & XSHAPE' _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 'STOE IPDS II' _diffrn_measurement_method 'incremental omega oscillation 1.0\%' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count 1.0 _diffrn_standards_interval_time 5 _diffrn_standards_decay_% ? _diffrn_reflns_number 9968 _diffrn_reflns_av_R_equivalents 0.0827 _diffrn_reflns_av_sigmaI/netI 0.0629 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 30.99 _reflns_number_total 1866 _reflns_number_gt 1669 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-Area 1.39 (STOE & Cie Gmbh, 2006)' _computing_cell_refinement 'X-Area 1.39 (STOE & Cie Gmbh, 2006)' _computing_data_reduction 'X-Area 1.39 (STOE & Cie Gmbh, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.1d (Crystal Impact Gbr, 2006)' _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^)+(0.0092P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.08(3) _refine_ls_number_reflns 1866 _refine_ls_number_parameters 49 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0474 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.0470 _refine_ls_wR_factor_gt 0.0456 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.976 _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 Rb Rb 0.58483(11) 0.27084(11) 0.24789(3) 0.00940(14) Uani 1 1 d . . . Se1 Se 0.08566(11) 0.24876(12) 0.22068(3) 0.00607(12) Uani 1 1 d . . . Se2 Se 0.31057(12) 0.25455(12) 0.39627(3) 0.01016(15) Uani 1 1 d . . . Se3 Se 0.42716(12) 0.20351(11) 0.07489(3) 0.00730(13) Uani 1 1 d . . . P P 0.0979(3) 0.0238(3) 0.05360(7) 0.0049(3) 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 Rb 0.0104(3) 0.0137(4) 0.0073(2) -0.0019(3) -0.0020(2) 0.0084(3) Se1 0.0066(3) 0.0054(3) 0.0049(2) -0.0006(2) 0.0012(2) 0.0020(3) Se2 0.0045(4) 0.0124(4) 0.0105(3) -0.0028(3) -0.0002(3) 0.0018(3) Se3 0.0042(3) 0.0108(3) 0.0059(3) 0.0003(3) -0.0004(2) 0.0031(3) P 0.0042(8) 0.0053(8) 0.0042(6) 0.0006(6) 0.0001(6) 0.0016(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rb Se2 3.4252(10) . ? Rb Se3 3.4361(9) . ? Rb Se2 3.4778(11) 5_665 ? Rb Se3 3.5098(10) 2_655 ? Rb Se3 3.5716(11) 6_655 ? Rb Se1 3.6024(11) . ? Rb Se3 3.7392(11) 6_665 ? Rb Se1 3.7740(11) 1_655 ? Rb Se1 3.8596(10) 6_655 ? Rb Se2 3.8706(11) 5 ? Rb Rb 4.7187(14) 5 ? Rb Rb 4.8983(9) 6_665 ? Se1 Se1 2.3210(13) 6 ? Se1 P 2.3343(18) 6 ? Se1 Rb 3.7740(11) 1_455 ? Se1 Rb 3.8596(10) 6_665 ? Se2 P 2.123(2) 2 ? Se2 Rb 3.4778(11) 5_565 ? Se2 Rb 3.8706(11) 5 ? Se3 P 2.1231(19) . ? Se3 Rb 3.5098(10) 3_664 ? Se3 Rb 3.5716(11) 6_665 ? Se3 Rb 3.7392(11) 6_655 ? P Se2 2.123(2) 3_554 ? P P 2.242(3) 4 ? P Se1 2.3343(18) 6 ? 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 Se2 Rb Se3 129.38(3) . . ? Se2 Rb Se2 101.713(19) . 5_665 ? Se3 Rb Se2 110.72(3) . 5_665 ? Se2 Rb Se3 63.91(2) . 2_655 ? Se3 Rb Se3 161.58(3) . 2_655 ? Se2 Rb Se3 74.12(2) 5_665 2_655 ? Se2 Rb Se3 101.54(2) . 6_655 ? Se3 Rb Se3 94.13(2) . 6_655 ? Se2 Rb Se3 120.79(3) 5_665 6_655 ? Se3 Rb Se3 69.00(2) 2_655 6_655 ? Se2 Rb Se1 63.66(2) . . ? Se3 Rb Se1 66.264(18) . . ? Se2 Rb Se1 122.44(3) 5_665 . ? Se3 Rb Se1 127.23(2) 2_655 . ? Se3 Rb Se1 116.71(2) 6_655 . ? Se2 Rb Se3 71.85(2) . 6_665 ? Se3 Rb Se3 91.21(2) . 6_665 ? Se2 Rb Se3 60.66(2) 5_665 6_665 ? Se3 Rb Se3 106.190(19) 2_655 6_665 ? Se3 Rb Se3 173.27(3) 6_655 6_665 ? Se1 Rb Se3 61.95(2) . 6_665 ? Se2 Rb Se1 132.29(3) . 1_655 ? Se3 Rb Se1 97.18(2) . 1_655 ? Se2 Rb Se1 64.08(2) 5_665 1_655 ? Se3 Rb Se1 68.38(2) 2_655 1_655 ? Se3 Rb Se1 59.96(2) 6_655 1_655 ? Se1 Rb Se1 163.29(2) . 1_655 ? Se3 Rb Se1 123.40(2) 6_665 1_655 ? Se2 Rb Se1 162.52(3) . 6_655 ? Se3 Rb Se1 62.10(2) . 6_655 ? Se2 Rb Se1 83.01(2) 5_665 6_655 ? Se3 Rb Se1 102.02(3) 2_655 6_655 ? Se3 Rb Se1 62.26(2) 6_655 6_655 ? Se1 Rb Se1 127.916(19) . 6_655 ? Se3 Rb Se1 124.13(2) 6_665 6_655 ? Se1 Rb Se1 35.378(19) 1_655 6_655 ? Se2 Rb Se2 66.34(3) . 5 ? Se3 Rb Se2 82.37(2) . 5 ? Se2 Rb Se2 166.58(3) 5_665 5 ? Se3 Rb Se2 94.40(2) 2_655 5 ? Se3 Rb Se2 58.953(19) 6_655 5 ? Se1 Rb Se2 59.10(2) . 5 ? Se3 Rb Se2 117.90(3) 6_665 5 ? Se1 Rb Se2 118.69(3) 1_655 5 ? Se1 Rb Se2 106.61(2) 6_655 5 ? Se2 Rb Rb 53.964(18) . 5 ? Se3 Rb Rb 124.65(3) . 5 ? Se2 Rb Rb 122.77(2) 5_665 5 ? Se3 Rb Rb 48.777(16) 2_655 5 ? Se3 Rb Rb 47.657(15) 6_655 5 ? Se1 Rb Rb 94.050(16) . 5 ? Se3 Rb Rb 125.66(2) 6_665 5 ? Se1 Rb Rb 93.867(15) 1_655 5 ? Se1 Rb Rb 109.28(2) 6_655 5 ? Se2 Rb Rb 45.693(16) 5 5 ? Se2 Rb Rb 102.48(2) . 6_665 ? Se3 Rb Rb 46.80(2) . 6_665 ? Se2 Rb Rb 83.759(18) 5_665 6_665 ? Se3 Rb Rb 150.17(2) 2_655 6_665 ? Se3 Rb Rb 140.75(2) 6_655 6_665 ? Se1 Rb Rb 51.282(18) . 6_665 ? Se3 Rb Rb 44.409(10) 6_665 6_665 ? Se1 Rb Rb 119.33(3) 1_655 6_665 ? Se1 Rb Rb 94.73(2) 6_655 6_665 ? Se2 Rb Rb 104.31(3) 5 6_665 ? Rb Rb Rb 145.320(17) 5 6_665 ? Se1 Se1 P 101.14(5) 6 6 ? Se1 Se1 Rb 122.38(3) 6 . ? P Se1 Rb 91.91(5) 6 . ? Se1 Se1 Rb 74.33(3) 6 1_455 ? P Se1 Rb 84.15(5) 6 1_455 ? Rb Se1 Rb 163.30(2) . 1_455 ? Se1 Se1 Rb 70.30(3) 6 6_665 ? P Se1 Rb 163.84(5) 6 6_665 ? Rb Se1 Rb 81.979(17) . 6_665 ? Rb Se1 Rb 105.80(3) 1_455 6_665 ? P Se2 Rb 115.04(5) 2 . ? P Se2 Rb 93.54(5) 2 5_565 ? Rb Se2 Rb 110.71(2) . 5_565 ? P Se2 Rb 88.25(5) 2 5 ? Rb Se2 Rb 80.34(2) . 5 ? Rb Se2 Rb 166.58(3) 5_565 5 ? P Se3 Rb 117.73(5) . . ? P Se3 Rb 107.48(4) . 3_664 ? Rb Se3 Rb 134.38(3) . 3_664 ? P Se3 Rb 92.39(5) . 6_665 ? Rb Se3 Rb 88.67(2) . 6_665 ? Rb Se3 Rb 83.57(2) 3_664 6_665 ? P Se3 Rb 86.48(6) . 6_655 ? Rb Se3 Rb 86.00(2) . 6_655 ? Rb Se3 Rb 103.105(19) 3_664 6_655 ? Rb Se3 Rb 173.27(3) 6_665 6_655 ? Se2 P Se3 118.63(9) 3_554 . ? Se2 P P 107.48(6) 3_554 4 ? Se3 P P 111.05(5) . 4 ? Se2 P Se1 111.81(7) 3_554 6 ? Se3 P Se1 110.98(7) . 6 ? P P Se1 94.10(10) 4 6 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.014 _refine_diff_density_min -1.204 _refine_diff_density_rms 0.258