#------------------------------------------------------------------------------ #$Date: 2016-02-14 04:40:26 +0000 (Sun, 14 Feb 2016) $ #$Revision: 176432 $ #$URL: svn://www.crystallography.net/cod/cif/2/23/89/2238944.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2238944 loop_ _publ_author_name 'Gjikaj, Mimoza' 'Pook, Niels-Patrick' 'Qarri, Flora' _publ_section_title ; \m-Hexathiometadiphosphato-bis[(1,4,7,10,13,16-hexaoxacyclooctadecane-\k^6^O)rubidium] acetonitrile disolvate ; _journal_coeditor_code WM2785 _journal_issue 12 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m689 _journal_paper_doi 10.1107/S1600536813032121 _journal_volume 69 _journal_year 2013 _chemical_formula_iupac '[Rb2 (P2 S6) (C12 H24 O6)2], 2C2 H3 N' _chemical_formula_moiety 'C24 H48 O12 P2 Rb2 S6, 2(C2 H3 N)' _chemical_formula_sum 'C28 H54 N2 O12 P2 Rb2 S6' _chemical_formula_weight 1035.98 _chemical_name_systematic '\m-Hexathiometadiphosphato-bis[(1,4,7,10,13,16-hexaoxacyclooctadecane-\k^6^O)rubidium] acetonitrile disolvate' _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 95.520(9) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 8.2261(9) _cell_length_b 17.1054(15) _cell_length_c 16.5895(18) _cell_measurement_reflns_used 41621 _cell_measurement_temperature 223(2) _cell_measurement_theta_max 25.68 _cell_measurement_theta_min 2.38 _cell_volume 2323.5(4) _computing_cell_refinement 'X-AREA (Stoe & Cie, 2002)' _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-AREA (Stoe & Cie, 2002)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 2012)' _computing_publication_material ; SHELXL97 (Sheldrick, 2008), PLATON (Spek, 2009) and publCIF (Westrip, 2010) ; _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _diffrn_ambient_temperature 223(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Stoe IPDSII' _diffrn_measurement_method \w-scans _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0923 _diffrn_reflns_av_sigmaI/netI 0.0526 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 26056 _diffrn_reflns_theta_full 25.68 _diffrn_reflns_theta_max 25.68 _diffrn_reflns_theta_min 2.38 _exptl_absorpt_coefficient_mu 2.496 _exptl_absorpt_correction_T_max 0.577 _exptl_absorpt_correction_T_min 0.490 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details '(X-SHAPE and X-RED; Stoe & Cie, 1999, 2001)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.481 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1064 _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _refine_diff_density_max 0.496 _refine_diff_density_min -0.283 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.148 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 343 _refine_ls_number_reflns 4400 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.148 _refine_ls_R_factor_all 0.0693 _refine_ls_R_factor_gt 0.0469 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0188P)^2^+1.1961P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0696 _refine_ls_wR_factor_ref 0.0742 _reflns_number_gt 3450 _reflns_number_total 4400 _reflns_threshold_expression I>2sigma(I) _iucr_refine_instructions_details ; TITL [Rb(C12H24O6)]2P2S6 * 2CH3CN CELL 0.71073 8.2261 17.1054 16.5895 90.000 95.520 90.000 ZERR 4 0.0009 0.0015 0.0018 0.000 0.009 0.000 LATT 1 SYMM -X,Y+1/2,-Z+1/2 SFAC C H N O P Rb S UNIT 56 108 4 24 4 4 12 SHEL 0.82 99 ACTA WGHT 0.0188 1.1961 FVAR 0.33729 MOLE 1 RB 6 0.016875 0.434251 -0.195895 11.00000 0.03859 0.03336 = 0.03045 0.00247 0.00526 -0.00168 S1 7 0.013823 0.359460 -0.389455 11.00000 0.06842 0.02883 = 0.03730 0.00207 0.00099 0.00616 S2 7 -0.207282 0.519946 -0.360484 11.00000 0.03542 0.04316 = 0.03489 -0.00273 0.00993 0.00330 S3 7 0.146018 0.536702 -0.448116 11.00000 0.03325 0.04288 = 0.02818 0.00049 0.00224 -0.00581 P 5 -0.057388 0.464162 -0.426191 11.00000 0.03228 0.02861 = 0.02634 0.00099 0.00430 0.00019 O1 4 0.267382 0.541357 -0.236399 11.00000 0.03467 0.03985 = 0.04871 0.00297 0.00549 -0.00432 O2 4 0.019952 0.602930 -0.148896 11.00000 0.04262 0.03796 = 0.04395 0.00306 0.00459 0.00199 O3 4 -0.216860 0.501475 -0.091879 11.00000 0.04155 0.03895 = 0.04124 0.00179 0.00361 0.00222 O4 4 -0.116111 0.345062 -0.064966 11.00000 0.03606 0.03745 = 0.04528 0.00271 0.00724 -0.00532 O5 4 0.132544 0.277891 -0.146835 11.00000 0.04595 0.03489 = 0.04274 0.00793 0.00482 0.00054 O6 4 0.366257 0.384393 -0.199932 11.00000 0.04009 0.04174 = 0.04326 0.00480 0.00633 -0.00027 C1 1 0.262798 0.621160 -0.212302 11.00000 0.05802 0.03798 = 0.05826 -0.00187 0.01337 -0.01717 C2 1 0.089259 0.646136 -0.210353 11.00000 0.06291 0.03381 = 0.04838 0.00460 0.00845 -0.00320 C3 1 -0.142842 0.626878 -0.138901 11.00000 0.05646 0.03420 = 0.05866 -0.00146 0.00336 0.00528 C4 1 -0.204387 0.582442 -0.070711 11.00000 0.04494 0.04689 = 0.05255 -0.01133 0.00826 0.00503 C5 1 -0.266142 0.455135 -0.027402 11.00000 0.04485 0.05877 = 0.05737 0.01140 0.02327 0.01083 C6 1 -0.274411 0.371014 -0.052696 11.00000 0.03590 0.05971 = 0.06841 0.01883 0.01613 -0.00450 C7 1 -0.106024 0.262571 -0.079590 11.00000 0.05946 0.03261 = 0.05018 0.00545 0.00726 -0.01018 C8 1 0.067449 0.240430 -0.080033 11.00000 0.05821 0.02701 = 0.04600 0.00463 0.00931 -0.00188 C9 1 0.300258 0.259308 -0.150726 11.00000 0.04656 0.03961 = 0.05040 0.00715 0.00206 0.01130 C10 1 0.362502 0.303313 -0.218844 11.00000 0.05150 0.04244 = 0.04964 -0.00094 0.00854 0.01004 C11 1 0.426631 0.429565 -0.263012 11.00000 0.03718 0.05717 = 0.05713 0.01472 0.01397 0.00357 C12 1 0.430013 0.513768 -0.238861 11.00000 0.03453 0.05614 = 0.06395 0.01407 0.00870 -0.00796 N13 3 -0.515882 0.242206 -0.411637 11.00000 0.08639 0.05835 = 0.08067 0.00942 0.01055 0.01238 C14 1 -0.516400 0.302240 -0.440744 11.00000 0.04316 0.05417 = 0.04571 -0.00773 0.00292 0.00624 C15 1 -0.520132 0.378823 -0.477783 11.00000 0.06465 0.05009 = 0.05774 0.00270 -0.00169 -0.00952 H1A 2 0.323622 0.633474 -0.160355 11.00000 0.05396 H1B 2 0.322516 0.652339 -0.251645 11.00000 0.07277 H2A 2 0.025831 0.638981 -0.261427 11.00000 0.04419 H2B 2 0.098006 0.701524 -0.196882 11.00000 0.06208 H3A 2 -0.145922 0.682728 -0.125231 11.00000 0.06493 H3B 2 -0.212020 0.618379 -0.192208 11.00000 0.05007 H4A 2 -0.302749 0.602680 -0.056439 11.00000 0.05434 H4B 2 -0.129386 0.590200 -0.018331 11.00000 0.05596 H5A 2 -0.372739 0.473243 -0.015669 11.00000 0.07733 H5B 2 -0.178775 0.463481 0.018701 11.00000 0.05253 H6A 2 -0.308216 0.341525 -0.008229 11.00000 0.04742 H6B 2 -0.341358 0.366843 -0.106405 11.00000 0.06194 H7A 2 -0.142832 0.236526 -0.036060 11.00000 0.04144 H7B 2 -0.179434 0.252761 -0.132009 11.00000 0.07709 H8A 2 0.078117 0.188605 -0.082751 11.00000 0.04072 H8B 2 0.136700 0.259117 -0.026846 11.00000 0.04986 H9A 2 0.319219 0.203681 -0.157563 11.00000 0.05615 H9B 2 0.363877 0.271234 -0.097132 11.00000 0.04634 H10A 2 0.300344 0.296073 -0.266833 11.00000 0.05028 H10B 2 0.470080 0.286595 -0.229059 11.00000 0.05430 H11A 2 0.537088 0.412532 -0.269470 11.00000 0.05388 H11B 2 0.353075 0.420431 -0.314144 11.00000 0.06107 H12A 2 0.485150 0.519750 -0.185863 11.00000 0.05194 H12B 2 0.480030 0.542871 -0.282291 11.00000 0.05074 H15A 2 -0.450597 0.411164 -0.445989 11.00000 0.09088 H15B 2 -0.493277 0.373882 -0.530976 11.00000 0.08288 H15C 2 -0.629721 0.396195 -0.485376 11.00000 0.11313 MOLE 2 L.S. 10 BOND $H FMAP 2 PLAN -1 HKLF 4 REM REM R1 = 0.0469 for 3450 Fo > 4sig(Fo) and 0.0693 for all 4400 data REM 343 parameters refined using 0 restraints END ; _cod_data_source_file wm2785.cif _cod_data_source_block I _cod_original_sg_symbol_Hall '-P 2yn' _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2238944 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' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_symmetry_multiplicity Rb Rb 0.01688(5) 0.43425(2) -0.19589(2) 0.03401(10) Uani d 1 1 S S1 0.01382(16) 0.35946(6) -0.38945(6) 0.0451(3) Uani d 1 1 S S2 -0.20728(13) 0.51995(6) -0.36048(6) 0.0374(2) Uani d 1 1 S S3 0.14602(13) 0.53670(6) -0.44812(5) 0.0348(2) Uani d 1 1 P P -0.05739(12) 0.46416(5) -0.42619(5) 0.0290(2) Uani d 1 1 O O1 0.2674(4) 0.54136(15) -0.23640(16) 0.0410(6) Uani d 1 1 O O2 0.0200(4) 0.60293(16) -0.14890(16) 0.0415(7) Uani d 1 1 O O3 -0.2169(4) 0.50147(15) -0.09188(15) 0.0406(6) Uani d 1 1 O O4 -0.1161(3) 0.34506(15) -0.06497(16) 0.0394(6) Uani d 1 1 O O5 0.1325(4) 0.27789(15) -0.14684(15) 0.0412(7) Uani d 1 1 O O6 0.3663(4) 0.38439(16) -0.19993(16) 0.0416(7) Uani d 1 1 C C1 0.2628(7) 0.6212(3) -0.2123(3) 0.0509(12) Uani d 1 1 C C2 0.0893(7) 0.6461(3) -0.2104(3) 0.0482(11) Uani d 1 1 C C3 -0.1428(7) 0.6269(3) -0.1389(3) 0.0499(11) Uani d 1 1 C C4 -0.2044(7) 0.5824(3) -0.0707(3) 0.0479(11) Uani d 1 1 C C5 -0.2661(7) 0.4551(3) -0.0274(3) 0.0525(12) Uani d 1 1 C C6 -0.2744(6) 0.3710(3) -0.0527(3) 0.0540(12) Uani d 1 1 C C7 -0.1060(6) 0.2626(2) -0.0796(3) 0.0473(11) Uani d 1 1 C C8 0.0674(6) 0.2404(2) -0.0800(3) 0.0435(10) Uani d 1 1 C C9 0.3003(6) 0.2593(3) -0.1507(3) 0.0457(10) Uani d 1 1 C C10 0.3625(7) 0.3033(3) -0.2188(3) 0.0476(11) Uani d 1 1 C C11 0.4266(6) 0.4296(3) -0.2630(3) 0.0499(11) Uani d 1 1 C C12 0.4300(6) 0.5138(3) -0.2389(3) 0.0513(11) Uani d 1 1 N N13 -0.5159(6) 0.2422(3) -0.4116(3) 0.0750(13) Uani d 1 1 C C14 -0.5164(6) 0.3022(3) -0.4407(3) 0.0478(10) Uani d 1 1 C C15 -0.5201(8) 0.3788(3) -0.4778(4) 0.0580(13) Uani d 1 1 H H1A 0.324(6) 0.633(3) -0.160(3) 0.054(13) Uiso d 1 1 H H1B 0.323(7) 0.652(3) -0.252(3) 0.073(16) Uiso d 1 1 H H2A 0.026(5) 0.639(2) -0.261(3) 0.044(12) Uiso d 1 1 H H2B 0.098(6) 0.702(3) -0.197(3) 0.062(14) Uiso d 1 1 H H3A -0.146(6) 0.683(3) -0.125(3) 0.065(14) Uiso d 1 1 H H3B -0.212(6) 0.618(2) -0.192(3) 0.050(13) Uiso d 1 1 H H4A -0.303(6) 0.603(3) -0.056(3) 0.054(13) Uiso d 1 1 H H4B -0.129(6) 0.590(3) -0.018(3) 0.056(13) Uiso d 1 1 H H5A -0.373(7) 0.473(3) -0.016(3) 0.077(17) Uiso d 1 1 H H5B -0.179(6) 0.463(2) 0.019(3) 0.052(13) Uiso d 1 1 H H6A -0.308(5) 0.342(2) -0.008(3) 0.047(12) Uiso d 1 1 H H6B -0.341(6) 0.367(3) -0.106(3) 0.062(15) Uiso d 1 1 H H7A -0.143(5) 0.237(2) -0.036(2) 0.041(11) Uiso d 1 1 H H7B -0.179(7) 0.253(3) -0.132(3) 0.077(17) Uiso d 1 1 H H8A 0.078(5) 0.189(3) -0.083(2) 0.041(11) Uiso d 1 1 H H8B 0.137(5) 0.259(2) -0.027(3) 0.050(12) Uiso d 1 1 H H9A 0.319(6) 0.204(3) -0.158(3) 0.056(13) Uiso d 1 1 H H9B 0.364(5) 0.271(2) -0.097(3) 0.046(12) Uiso d 1 1 H H10A 0.300(6) 0.296(3) -0.267(3) 0.050(13) Uiso d 1 1 H H10B 0.470(6) 0.287(3) -0.229(3) 0.054(13) Uiso d 1 1 H H11A 0.537(6) 0.413(3) -0.269(3) 0.054(13) Uiso d 1 1 H H11B 0.353(6) 0.420(3) -0.314(3) 0.061(14) Uiso d 1 1 H H12A 0.485(6) 0.520(3) -0.186(3) 0.052(13) Uiso d 1 1 H H12B 0.480(6) 0.543(2) -0.282(3) 0.051(13) Uiso d 1 1 H H15A -0.451(8) 0.411(4) -0.446(4) 0.09(2) Uiso d 1 1 H H15B -0.493(7) 0.374(3) -0.531(4) 0.083(18) Uiso d 1 1 H H15C -0.630(9) 0.396(4) -0.485(4) 0.11(3) Uiso d 1 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Rb 0.0386(2) 0.03336(18) 0.03045(17) -0.00168(18) 0.00526(13) 0.00247(16) S1 0.0684(8) 0.0288(5) 0.0373(5) 0.0062(5) 0.0010(5) 0.0021(4) S2 0.0354(6) 0.0432(5) 0.0349(5) 0.0033(4) 0.0099(4) -0.0027(4) S3 0.0333(5) 0.0429(5) 0.0282(4) -0.0058(4) 0.0022(4) 0.0005(4) P 0.0323(6) 0.0286(4) 0.0263(4) 0.0002(4) 0.0043(4) 0.0010(4) O1 0.0347(16) 0.0398(15) 0.0487(15) -0.0043(12) 0.0055(12) 0.0030(12) O2 0.0426(18) 0.0380(15) 0.0440(15) 0.0020(13) 0.0046(13) 0.0031(12) O3 0.0415(17) 0.0390(15) 0.0412(15) 0.0022(13) 0.0036(12) 0.0018(12) O4 0.0361(17) 0.0375(15) 0.0453(15) -0.0053(12) 0.0072(12) 0.0027(12) O5 0.0460(18) 0.0349(14) 0.0427(15) 0.0005(13) 0.0048(13) 0.0079(11) O6 0.0401(17) 0.0418(15) 0.0433(15) -0.0003(13) 0.0063(13) 0.0048(12) C1 0.058(3) 0.038(2) 0.058(3) -0.017(2) 0.013(2) -0.002(2) C2 0.063(3) 0.034(2) 0.048(3) -0.003(2) 0.008(2) 0.0046(19) C3 0.056(3) 0.034(2) 0.059(3) 0.005(2) 0.003(2) -0.001(2) C4 0.045(3) 0.047(3) 0.053(3) 0.005(2) 0.008(2) -0.0113(19) C5 0.045(3) 0.059(3) 0.057(3) 0.011(2) 0.023(2) 0.011(2) C6 0.036(3) 0.060(3) 0.068(3) -0.004(2) 0.016(2) 0.019(3) C7 0.059(3) 0.033(2) 0.050(3) -0.010(2) 0.007(2) 0.0054(19) C8 0.058(3) 0.027(2) 0.046(2) -0.002(2) 0.009(2) 0.0046(17) C9 0.047(3) 0.040(2) 0.050(3) 0.011(2) 0.002(2) 0.0071(19) C10 0.052(3) 0.042(2) 0.050(3) 0.010(2) 0.009(2) -0.0009(19) C11 0.037(3) 0.057(3) 0.057(3) 0.004(2) 0.014(2) 0.015(2) C12 0.035(3) 0.056(3) 0.064(3) -0.008(2) 0.009(2) 0.014(2) N13 0.086(4) 0.058(3) 0.081(3) 0.012(3) 0.011(3) 0.009(2) C14 0.043(3) 0.054(3) 0.046(2) 0.006(2) 0.003(2) -0.008(2) C15 0.065(4) 0.050(3) 0.058(3) -0.010(3) -0.002(3) 0.003(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rb Rb -0.9393 2.9676 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle O1 Rb O5 . . 115.13(8) O1 Rb O3 . . 114.25(8) O5 Rb O3 . . 114.06(7) O1 Rb O4 . . 145.48(8) O5 Rb O4 . . 57.07(8) O3 Rb O4 . . 57.31(7) O1 Rb O2 . . 57.26(8) O5 Rb O2 . . 144.60(8) O3 Rb O2 . . 57.22(8) O4 Rb O2 . . 107.56(7) O1 Rb O6 . . 57.92(8) O5 Rb O6 . . 57.38(8) O3 Rb O6 . . 143.65(8) O4 Rb O6 . . 107.03(7) O2 Rb O6 . . 107.20(8) O1 Rb S1 . . 87.72(6) O5 Rb S1 . . 83.87(5) O3 Rb S1 . . 138.08(6) O4 Rb S1 . . 121.53(6) O2 Rb S1 . . 126.82(5) O6 Rb S1 . . 78.21(6) O1 Rb S2 . . 83.44(6) O5 Rb S2 . . 137.62(6) O3 Rb S2 . . 88.20(6) O4 Rb S2 . . 126.26(6) O2 Rb S2 . . 77.75(6) O6 Rb S2 . . 122.65(5) S1 Rb S2 . . 57.93(3) P S1 Rb . . 85.75(4) P S2 Rb . . 85.25(4) P S3 P 3_564 . 87.88(5) S1 P S2 . . 117.02(6) S1 P S3 . 3_564 111.07(6) S2 P S3 . 3_564 111.69(6) S1 P S3 . . 111.50(7) S2 P S3 . . 110.75(6) S3 P S3 3_564 . 92.12(5) S1 P Rb . . 63.64(4) S2 P Rb . . 64.06(4) S3 P Rb 3_564 . 166.70(5) S3 P Rb . . 101.17(4) C12 O1 C1 . . 112.1(4) C12 O1 Rb . . 119.4(2) C1 O1 Rb . . 120.3(3) C2 O2 C3 . . 112.3(3) C2 O2 Rb . . 108.0(2) C3 O2 Rb . . 108.9(2) C5 O3 C4 . . 112.0(3) C5 O3 Rb . . 118.3(2) C4 O3 Rb . . 119.2(2) C6 O4 C7 . . 113.8(3) C6 O4 Rb . . 110.9(2) C7 O4 Rb . . 110.6(2) C9 O5 C8 . . 111.9(3) C9 O5 Rb . . 118.8(2) C8 O5 Rb . . 119.3(2) C10 O6 C11 . . 111.6(3) C10 O6 Rb . . 106.3(3) C11 O6 Rb . . 105.3(2) O1 C1 C2 . . 109.4(4) O1 C1 H1A . . 115(3) C2 C1 H1A . . 109(3) O1 C1 H1B . . 107(3) C2 C1 H1B . . 113(3) H1A C1 H1B . . 103(4) O2 C2 C1 . . 108.5(4) O2 C2 H2A . . 110(3) C1 C2 H2A . . 113(3) Rb C2 H2A . . 82(2) O2 C2 H2B . . 112(3) C1 C2 H2B . . 103(3) Rb C2 H2B . . 162(3) H2A C2 H2B . . 110(4) O2 C3 C4 . . 109.5(4) O2 C3 H3A . . 111(3) C4 C3 H3A . . 108(3) Rb C3 H3A . . 160(3) O2 C3 H3B . . 108(3) C4 C3 H3B . . 113(3) Rb C3 H3B . . 80(2) H3A C3 H3B . . 108(4) O3 C4 C3 . . 109.2(4) O3 C4 H4A . . 112(3) C3 C4 H4A . . 112(3) O3 C4 H4B . . 111(3) C3 C4 H4B . . 111(3) H4A C4 H4B . . 102(4) O3 C5 C6 . . 109.5(4) O3 C5 H5A . . 108(3) C6 C5 H5A . . 110(3) O3 C5 H5B . . 105(3) C6 C5 H5B . . 111(3) H5A C5 H5B . . 113(4) O4 C6 C5 . . 109.0(4) O4 C6 H6A . . 107(3) C5 C6 H6A . . 107(3) Rb C6 H6A . . 155(3) O4 C6 H6B . . 107(3) C5 C6 H6B . . 109(3) Rb C6 H6B . . 78(3) H6A C6 H6B . . 118(4) O4 C7 C8 . . 108.9(4) O4 C7 H7A . . 108(3) C8 C7 H7A . . 106(3) Rb C7 H7A . . 156(3) O4 C7 H7B . . 105(3) C8 C7 H7B . . 116(3) Rb C7 H7B . . 82(3) H7A C7 H7B . . 112(4) O5 C8 C7 . . 108.9(4) O5 C8 H8A . . 111(3) C7 C8 H8A . . 111(3) O5 C8 H8B . . 108(2) C7 C8 H8B . . 111(2) H8A C8 H8B . . 107(3) O5 C9 C10 . . 109.1(4) O5 C9 H9A . . 113(3) C10 C9 H9A . . 110(3) O5 C9 H9B . . 110(2) C10 C9 H9B . . 112(2) H9A C9 H9B . . 103(4) O6 C10 C9 . . 109.1(4) O6 C10 H10A . . 109(3) C9 C10 H10A . . 113(3) Rb C10 H10A . . 78(3) O6 C10 H10B . . 109(3) C9 C10 H10B . . 112(3) Rb C10 H10B . . 160(3) H10A C10 H10B . . 105(4) O6 C11 C12 . . 108.9(4) O6 C11 H11A . . 108(3) C12 C11 H11A . . 109(3) Rb C11 H11A . . 160(3) O6 C11 H11B . . 108(3) C12 C11 H11B . . 112(3) Rb C11 H11B . . 76(3) H11A C11 H11B . . 111(4) O1 C12 C11 . . 109.5(4) O1 C12 H12A . . 108(3) C11 C12 H12A . . 110(3) O1 C12 H12B . . 108(3) C11 C12 H12B . . 107(2) H12A C12 H12B . . 115(4) N13 C14 C15 . . 179.0(6) C14 C15 H15A . . 108(4) C14 C15 H15B . . 109(4) H15A C15 H15B . . 114(5) C14 C15 H15C . . 109(4) H15A C15 H15C . . 115(6) H15B C15 H15C . . 102(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance Rb O1 . 2.885(3) Rb O5 . 2.928(3) Rb O3 . 2.939(3) Rb O4 . 2.949(3) Rb O2 . 2.988(3) Rb O6 . 3.005(3) Rb S1 . 3.4544(11) Rb S2 . 3.4692(11) S1 P . 1.9630(13) S2 P . 1.9692(13) S3 P 3_564 2.1418(13) S3 P . 2.1421(14) P S3 3_564 2.1419(13) O1 C12 . 1.423(6) O1 C1 . 1.424(5) O2 C2 . 1.422(5) O2 C3 . 1.425(6) O3 C5 . 1.421(5) O3 C4 . 1.430(5) O4 C6 . 1.409(5) O4 C7 . 1.435(5) O5 C9 . 1.423(5) O5 C8 . 1.428(5) O6 C10 . 1.422(5) O6 C11 . 1.428(5) C1 C2 . 1.493(7) C1 H1A . 0.98(5) C1 H1B . 1.01(5) C2 H2A . 0.96(4) C2 H2B . 0.97(5) C3 C4 . 1.491(7) C3 H3A . 0.98(5) C3 H3B . 1.01(5) C4 H4A . 0.93(5) C4 H4B . 1.02(5) C5 C6 . 1.499(7) C5 H5A . 0.97(6) C5 H5B . 1.01(5) C6 H6A . 0.96(4) C6 H6B . 1.00(5) C7 C8 . 1.477(7) C7 H7A . 0.92(4) C7 H7B . 1.02(5) C8 H8A . 0.89(4) C8 H8B . 1.05(4) C9 C10 . 1.489(6) C9 H9A . 0.97(5) C9 H9B . 1.01(4) C10 H10A . 0.91(5) C10 H10B . 0.96(5) C11 C12 . 1.495(7) C11 H11A . 0.97(5) C11 H11B . 1.01(5) C12 H12A . 0.95(5) C12 H12B . 1.00(4) N13 C14 . 1.135(6) C14 C15 . 1.446(7) C15 H15A . 0.92(7) C15 H15B . 0.93(6) C15 H15C . 0.95(7)