# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1951 data_global # 1. SUBMISSION DETAILS _publ_contact_author ; Dr. Gerd W. Rabe Technische Universitat Munchen Anorganisch-chemisches Institut Lichtenbergstr. 4 85747 Garching (Germany) ; _publ_contact_author_phone '+49-89-3209-3085' _publ_contact_author_fax '+49-89-3209-3125' _publ_contact_author_email 'gwrabe@lrz.tu-muenchen.de' _publ_requested_journal 'J. Chem. Soc. Dalton Trans.' # 2. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis and X-ray Crystal Structure Determination of Two Monomeric Alkali Metal Phosphide Derivatives: [MP(H)t-Bu(3)Mes](18-crown-6)(M=K, Rb) ; loop_ _publ_author_name _publ_author_address 'Rabe, Gerd W.' ; Technische Universitat Munchen Anorganisch-chemisches Institut Lichtenbergstr. 4 85747 Garching (Germany) ; 'Rheingold, A. L.' ; University of Delaware Department of Chemistry and Biochemistry Academy Street Newark, DE 19716 U. S. A. ; 'Liable-Sands, L. M.' ; University of Delaware Department of Chemistry and Biochemistry Academy Street Newark, DE 19716 U. S. A. ; 'Guzei, I. A.' ; University of Delaware Department of Chemistry and Biochemistry Academy Street Newark, DE 19716 U. S. A. ; # 3. Results data_raba _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C30 H54 O6 P Rb' _chemical_formula_weight 627.17 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rb' 'Rb' -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 40.3994(5) _cell_length_b 9.16400(10) _cell_length_c 19.2861(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.2640(10) _cell_angle_gamma 90.00 _cell_volume 6854.36(13) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.216 _exptl_crystal_density_method ? _exptl_crystal_F_000 2672 _exptl_absorpt_coefficient_mu 1.527 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'Siemens P4/CCD' _diffrn_measurement_method 'phi, omega' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10877 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0732 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 52 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.05 _diffrn_reflns_theta_max 28.13 _reflns_number_total 6972 _reflns_number_observed 5108 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens/SMART' _computing_cell_refinement 'Siemens/SAINT' _computing_data_reduction 'Siemens/SAINT' _computing_structure_solution 'SHELXS-5.03 (Sheldrick, 1994)' _computing_structure_refinement 'SHELXL-5.03 (Sheldrick, 1994)' _computing_molecular_graphics 'XP-5.03' _computing_publication_material 'XCIF' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 7 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1000P)^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 'idealized contributions' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6965 _refine_ls_number_parameters 345 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0808 _refine_ls_R_factor_obs 0.0530 _refine_ls_wR_factor_all 0.1781 _refine_ls_wR_factor_obs 0.1449 _refine_ls_goodness_of_fit_all 1.025 _refine_ls_goodness_of_fit_obs 1.051 _refine_ls_restrained_S_all 1.100 _refine_ls_restrained_S_obs 1.051 _refine_ls_shift/esd_max -0.033 _refine_ls_shift/esd_mean 0.001 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Rb1 Rb 0.159476(9) 0.58300(4) 0.10493(2) 0.03065(13) Uani 1 d . . P1 P 0.14876(2) 0.27037(12) 0.20544(5) 0.0333(3) Uani 1 d D . O1 O 0.10012(7) 0.7259(3) -0.0014(2) 0.0413(7) Uani 1 d . . O2 O 0.15371(8) 0.5934(3) -0.0517(2) 0.0448(8) Uani 1 d . . O3 O 0.22118(7) 0.6270(3) 0.0421(2) 0.0463(7) Uani 1 d . . O4 O 0.23148(7) 0.6118(3) 0.1937(2) 0.0461(8) Uani 1 d . . O5 O 0.17870(8) 0.7475(3) 0.2459(2) 0.0430(7) Uani 1 d . . O6 O 0.11076(7) 0.7571(3) 0.1502(2) 0.0396(7) Uani 1 d . . C1 C 0.09351(12) 0.6274(6) -0.0608(3) 0.0528(13) Uani 1 d . . H1A H 0.07064(12) 0.6481(6) -0.0947(3) 0.063 Uiso 1 calc R . H1B H 0.09344(12) 0.5258(6) -0.0433(3) 0.063 Uiso 1 calc R . C2 C 0.12127(13) 0.6452(6) -0.0988(2) 0.0568(14) Uani 1 d . . H2A H 0.11518(13) 0.5886(6) -0.1443(2) 0.068 Uiso 1 calc R . H2B H 0.12336(13) 0.7493(6) -0.1107(2) 0.068 Uiso 1 calc R . C3 C 0.18211(12) 0.6397(5) -0.0768(2) 0.0453(11) Uani 1 d . . H3A H 0.18404(12) 0.7474(5) -0.0742(2) 0.054 Uiso 1 calc R . H3B H 0.17834(12) 0.6099(5) -0.1278(2) 0.054 Uiso 1 calc R . C4 C 0.21469(13) 0.5720(5) -0.0307(3) 0.0488(12) Uani 1 d . . H4A H 0.21230(13) 0.4645(5) -0.0309(3) 0.059 Uiso 1 calc R . H4B H 0.23422(13) 0.5968(5) -0.0502(3) 0.059 Uiso 1 calc R . C5 C 0.25147(11) 0.5627(6) 0.0901(3) 0.0520(12) Uani 1 d . . H5A H 0.27127(11) 0.5733(6) 0.0697(3) 0.062 Uiso 1 calc R . H5B H 0.24758(11) 0.4574(6) 0.0962(3) 0.062 Uiso 1 calc R . C6 C 0.25909(11) 0.6384(6) 0.1617(3) 0.0595(14) Uani 1 d . . H6A H 0.28106(11) 0.6014(6) 0.1940(3) 0.071 Uiso 1 calc R . H6B H 0.26153(11) 0.7445(6) 0.1551(3) 0.071 Uiso 1 calc R . C7 C 0.23768(12) 0.6792(6) 0.2624(3) 0.0581(14) Uani 1 d . . H7A H 0.24279(12) 0.7841(6) 0.2586(3) 0.070 Uiso 1 calc R . H7B H 0.25784(12) 0.6333(6) 0.2969(3) 0.070 Uiso 1 calc R . C8 C 0.20612(13) 0.6622(6) 0.2894(3) 0.0564(13) Uani 1 d . . H8A H 0.19919(13) 0.5583(6) 0.2870(3) 0.068 Uiso 1 calc R . H8B H 0.21148(13) 0.6944(6) 0.3403(3) 0.068 Uiso 1 calc R . C9 C 0.14820(13) 0.7461(6) 0.2698(2) 0.0527(12) Uani 1 d . . H9A H 0.15323(13) 0.7894(6) 0.3187(2) 0.063 Uiso 1 calc R . H9B H 0.14050(13) 0.6442(6) 0.2725(2) 0.063 Uiso 1 calc R . C10 C 0.12040(13) 0.8308(5) 0.2187(3) 0.0496(12) Uani 1 d . . H10A H 0.10017(13) 0.8389(5) 0.2380(3) 0.060 Uiso 1 calc R . H10B H 0.12867(13) 0.9304(5) 0.2128(3) 0.060 Uiso 1 calc R . C11 C 0.08287(11) 0.8271(5) 0.0979(3) 0.0466(11) Uani 1 d . . H11A H 0.09029(11) 0.9237(5) 0.0848(3) 0.056 Uiso 1 calc R . H11B H 0.06311(11) 0.8415(5) 0.1181(3) 0.056 Uiso 1 calc R . C12 C 0.07250(10) 0.7298(5) 0.0320(3) 0.0480(12) Uani 1 d . . H12A H 0.06765(10) 0.6301(5) 0.0463(3) 0.058 Uiso 1 calc R . H12B H 0.05132(10) 0.7682(5) -0.0026(3) 0.058 Uiso 1 calc R . C13 C 0.11686(8) 0.2340(4) 0.1178(2) 0.0219(7) Uani 1 d . . C14 C 0.07974(8) 0.2608(4) 0.1061(2) 0.0236(7) Uani 1 d . . C15 C 0.05751(9) 0.2477(4) 0.0353(2) 0.0272(8) Uani 1 d . . H15A H 0.03365(9) 0.2656(4) 0.0285(2) 0.033 Uiso 1 calc R . C16 C 0.06809(8) 0.2104(4) -0.0251(2) 0.0242(7) Uani 1 d . . C17 C 0.10282(8) 0.1750(4) -0.0130(2) 0.0252(7) Uani 1 d . . H17A H 0.11052(8) 0.1455(4) -0.0531(2) 0.030 Uiso 1 calc R . C18 C 0.12723(8) 0.1806(4) 0.0558(2) 0.0230(7) Uani 1 d . . C19 C 0.16394(8) 0.1203(4) 0.0584(2) 0.0279(8) Uani 1 d . . C20 C 0.16509(11) 0.0480(6) -0.0137(3) 0.0531(13) Uani 1 d . . H20A H 0.14827(11) -0.0317(6) -0.0255(3) 0.080 Uiso 1 calc R . H20B H 0.18825(11) 0.0093(6) -0.0087(3) 0.080 Uiso 1 calc R . H20C H 0.15948(11) 0.1209(6) -0.0524(3) 0.080 Uiso 1 calc R . C21 C 0.17488(10) -0.0029(4) 0.1158(2) 0.0389(10) Uani 1 d . . H21A H 0.15721(10) -0.0794(4) 0.1058(2) 0.058 Uiso 1 calc R . H21B H 0.17740(10) 0.0376(4) 0.1640(2) 0.058 Uiso 1 calc R . H21C H 0.19691(10) -0.0446(4) 0.1136(2) 0.058 Uiso 1 calc R . C22 C 0.19124(9) 0.2440(4) 0.0721(2) 0.0362(9) Uani 1 d . . H22A H 0.19177(9) 0.2943(4) 0.1173(2) 0.054 Uiso 1 calc R . H22B H 0.18520(9) 0.3137(4) 0.0320(2) 0.054 Uiso 1 calc R . H22C H 0.21398(9) 0.2021(4) 0.0758(2) 0.054 Uiso 1 calc R . C23 C 0.06254(9) 0.2976(4) 0.1674(2) 0.0289(8) Uani 1 d . . C24 C 0.02225(10) 0.3024(6) 0.1392(2) 0.0489(12) Uani 1 d . . H24A H 0.01526(10) 0.3763(6) 0.1012(2) 0.073 Uiso 1 calc R . H24B H 0.01270(10) 0.3272(6) 0.1792(2) 0.073 Uiso 1 calc R . H24C H 0.01358(10) 0.2067(6) 0.1196(2) 0.073 Uiso 1 calc R . C25 C 0.07023(11) 0.1789(5) 0.2261(2) 0.0403(10) Uani 1 d . . H25A H 0.06340(11) 0.0835(5) 0.2038(2) 0.060 Uiso 1 calc R . H25B H 0.05724(11) 0.1994(5) 0.2610(2) 0.060 Uiso 1 calc R . H25C H 0.09497(11) 0.1783(5) 0.2510(2) 0.060 Uiso 1 calc R . C26 C 0.07280(11) 0.4513(5) 0.1994(2) 0.0389(10) Uani 1 d . . H26A H 0.06751(11) 0.5236(5) 0.1604(2) 0.058 Uiso 1 calc R . H26B H 0.09755(11) 0.4532(5) 0.2241(2) 0.058 Uiso 1 calc R . H26C H 0.05982(11) 0.4743(5) 0.2340(2) 0.058 Uiso 1 calc R . C27 C 0.04246(9) 0.1963(4) -0.1016(2) 0.0318(9) Uani 1 d . . C28 C 0.0213(2) 0.0610(9) -0.1056(5) 0.054(2) Uiso 0.60 d P 1 H28A H 0.0107(2) 0.0605(9) -0.0657(5) 0.081 Uiso 0.60 calc PR 1 H28B H 0.0362(2) -0.0249(9) -0.1019(5) 0.081 Uiso 0.60 calc PR 1 H28C H 0.0033(2) 0.0587(9) -0.1517(5) 0.081 Uiso 0.60 calc PR 1 C29 C 0.0599(2) 0.2061(9) -0.1616(4) 0.049(2) Uiso 0.60 d P 1 H29A H 0.0734(2) 0.2965(9) -0.1564(4) 0.074 Uiso 0.60 calc PR 1 H29B H 0.0424(2) 0.2058(9) -0.2085(4) 0.074 Uiso 0.60 calc PR 1 H29C H 0.0753(2) 0.1222(9) -0.1588(4) 0.074 Uiso 0.60 calc PR 1 C30 C 0.0160(2) 0.3308(8) -0.1138(4) 0.044(2) Uiso 0.60 d P 1 H30A H 0.0287(2) 0.4226(8) -0.1116(4) 0.066 Uiso 0.60 calc PR 1 H30B H 0.0041(2) 0.3302(8) -0.0759(4) 0.066 Uiso 0.60 calc PR 1 H30C H -0.0010(2) 0.3217(8) -0.1611(4) 0.066 Uiso 0.60 calc PR 1 C28' C 0.0486(3) 0.0347(14) -0.1355(7) 0.050(3) Uiso 0.40 d P 2 H28D H 0.0726(3) 0.0267(14) -0.1368(7) 0.075 Uiso 0.40 calc PR 2 H28E H 0.0332(3) 0.0253(14) -0.1845(7) 0.075 Uiso 0.40 calc PR 2 H28F H 0.0436(3) -0.0430(14) -0.1050(7) 0.075 Uiso 0.40 calc PR 2 C29' C 0.0504(3) 0.3053(13) -0.1542(6) 0.045(3) Uiso 0.40 d P 2 H29D H 0.0749(3) 0.2997(13) -0.1519(6) 0.067 Uiso 0.40 calc PR 2 H29E H 0.0449(3) 0.4041(13) -0.1413(6) 0.067 Uiso 0.40 calc PR 2 H29F H 0.0364(3) 0.2825(13) -0.2033(6) 0.067 Uiso 0.40 calc PR 2 C30' C 0.0052(3) 0.1980(13) -0.1018(7) 0.049(3) Uiso 0.40 d P 2 H30D H 0.0016(3) 0.1260(13) -0.0671(7) 0.073 Uiso 0.40 calc PR 2 H30E H -0.0093(3) 0.1737(13) -0.1503(7) 0.073 Uiso 0.40 calc PR 2 H30F H -0.0008(3) 0.2953(13) -0.0882(7) 0.073 Uiso 0.40 calc PR 2 H1P H 0.1307(12) 0.3289(83) 0.2511(27) 0.150(29) Uiso 1 d 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 Rb1 0.0386(2) 0.0303(2) 0.0242(2) 0.00188(15) 0.01062(14) 0.00436(14) P1 0.0350(5) 0.0400(6) 0.0220(5) -0.0013(4) 0.0030(4) -0.0068(4) O1 0.0393(15) 0.045(2) 0.037(2) 0.0055(13) 0.0068(12) -0.0100(12) O2 0.061(2) 0.050(2) 0.0270(15) 0.0014(13) 0.0184(13) -0.0176(14) O3 0.048(2) 0.051(2) 0.049(2) -0.0016(15) 0.0270(14) -0.0028(14) O4 0.040(2) 0.054(2) 0.042(2) 0.0036(15) 0.0057(13) -0.0107(13) O5 0.059(2) 0.044(2) 0.029(2) 0.0011(13) 0.0176(13) -0.0102(13) O6 0.051(2) 0.031(2) 0.042(2) -0.0014(12) 0.0222(13) -0.0015(12) C1 0.050(3) 0.060(3) 0.040(3) 0.002(2) -0.002(2) -0.018(2) C2 0.071(3) 0.065(3) 0.026(2) 0.000(2) 0.001(2) -0.017(3) C3 0.077(3) 0.041(3) 0.028(2) 0.001(2) 0.030(2) -0.008(2) C4 0.074(3) 0.041(3) 0.049(3) 0.001(2) 0.046(2) -0.009(2) C5 0.035(2) 0.057(3) 0.072(3) -0.002(3) 0.026(2) -0.010(2) C6 0.035(2) 0.068(3) 0.075(4) 0.009(3) 0.015(2) -0.013(2) C7 0.053(3) 0.080(4) 0.032(3) 0.003(2) -0.005(2) -0.012(2) C8 0.069(3) 0.062(3) 0.031(2) 0.006(2) 0.002(2) -0.011(3) C9 0.073(3) 0.061(3) 0.032(2) -0.013(2) 0.026(2) -0.021(2) C10 0.067(3) 0.038(3) 0.060(3) -0.017(2) 0.046(2) -0.011(2) C11 0.045(2) 0.041(3) 0.061(3) 0.009(2) 0.026(2) 0.007(2) C12 0.034(2) 0.057(3) 0.053(3) 0.016(2) 0.011(2) -0.003(2) C13 0.026(2) 0.018(2) 0.023(2) 0.0014(13) 0.0095(13) -0.0016(12) C14 0.030(2) 0.023(2) 0.022(2) -0.0030(13) 0.0133(13) -0.0033(13) C15 0.025(2) 0.034(2) 0.024(2) -0.002(2) 0.0101(13) -0.0006(14) C16 0.028(2) 0.027(2) 0.018(2) 0.0009(14) 0.0079(13) -0.0015(13) C17 0.032(2) 0.026(2) 0.021(2) -0.0001(14) 0.0127(14) -0.0010(13) C18 0.026(2) 0.023(2) 0.024(2) 0.0015(13) 0.0128(13) -0.0024(12) C19 0.025(2) 0.032(2) 0.030(2) -0.001(2) 0.0136(14) 0.0004(14) C20 0.039(2) 0.079(4) 0.043(3) -0.016(2) 0.015(2) 0.015(2) C21 0.032(2) 0.029(2) 0.056(3) 0.007(2) 0.014(2) 0.004(2) C22 0.027(2) 0.040(2) 0.045(2) 0.013(2) 0.016(2) 0.002(2) C23 0.033(2) 0.034(2) 0.025(2) -0.005(2) 0.0167(14) -0.0016(15) C24 0.031(2) 0.084(4) 0.037(2) -0.016(2) 0.019(2) -0.004(2) C25 0.051(2) 0.043(3) 0.036(2) -0.005(2) 0.028(2) -0.009(2) C26 0.052(2) 0.039(2) 0.032(2) -0.006(2) 0.023(2) 0.001(2) C27 0.029(2) 0.041(2) 0.024(2) -0.001(2) 0.0058(14) -0.005(2) _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 Rb1 O6 2.853(3) . ? Rb1 O4 2.945(3) . ? Rb1 O2 2.966(3) . ? Rb1 O1 2.986(3) . ? Rb1 O5 3.014(3) . ? Rb1 O3 3.088(3) . ? Rb1 P1 3.5529(11) . ? Rb1 C8 3.602(5) . ? Rb1 C13 3.674(3) . ? P1 C13 1.847(3) . ? O1 C1 1.422(6) . ? O1 C12 1.437(5) . ? O2 C3 1.429(5) . ? O2 C2 1.449(6) . ? O3 C5 1.437(6) . ? O3 C4 1.446(5) . ? O4 C7 1.419(6) . ? O4 C6 1.439(6) . ? O5 C8 1.421(5) . ? O5 C9 1.431(6) . ? O6 C11 1.435(5) . ? O6 C10 1.438(5) . ? C1 C2 1.511(7) . ? C3 C4 1.501(7) . ? C5 C6 1.497(8) . ? C7 C8 1.513(7) . ? C9 C10 1.488(7) . ? C11 C12 1.513(7) . ? C13 C18 1.457(5) . ? C13 C14 1.473(5) . ? C14 C15 1.414(5) . ? C14 C23 1.566(5) . ? C15 C16 1.392(5) . ? C16 C17 1.395(5) . ? C16 C27 1.552(5) . ? C17 C18 1.415(5) . ? C18 C19 1.570(5) . ? C19 C22 1.551(5) . ? C19 C20 1.552(6) . ? C19 C21 1.556(5) . ? C23 C25 1.538(6) . ? C23 C26 1.547(5) . ? C23 C24 1.565(5) . ? C27 C28 1.495(9) . ? C27 C30' 1.503(12) . ? C27 C29 1.518(9) . ? C27 C29' 1.520(12) . ? C27 C30 1.606(8) . ? C27 C28' 1.664(13) . ? 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 O6 Rb1 O4 115.18(9) . . ? O6 Rb1 O2 115.42(9) . . ? O4 Rb1 O2 111.87(9) . . ? O6 Rb1 O1 58.33(8) . . ? O4 Rb1 O1 146.35(8) . . ? O2 Rb1 O1 57.81(9) . . ? O6 Rb1 O5 58.00(8) . . ? O4 Rb1 O5 57.83(9) . . ? O2 Rb1 O5 146.08(8) . . ? O1 Rb1 O5 110.79(8) . . ? O6 Rb1 O3 138.48(8) . . ? O4 Rb1 O3 56.09(9) . . ? O2 Rb1 O3 55.80(8) . . ? O1 Rb1 O3 104.74(8) . . ? O5 Rb1 O3 104.86(8) . . ? O6 Rb1 P1 94.83(6) . . ? O4 Rb1 P1 90.37(6) . . ? O2 Rb1 P1 126.50(6) . . ? O1 Rb1 P1 122.09(6) . . ? O5 Rb1 P1 87.19(6) . . ? O3 Rb1 P1 123.66(6) . . ? O6 Rb1 C8 78.48(11) . . ? O4 Rb1 C8 41.35(11) . . ? O2 Rb1 C8 150.41(10) . . ? O1 Rb1 C8 133.43(11) . . ? O5 Rb1 C8 22.65(10) . . ? O3 Rb1 C8 96.00(10) . . ? P1 Rb1 C8 74.55(8) . . ? O6 Rb1 C13 95.15(8) . . ? O4 Rb1 C13 116.36(8) . . ? O2 Rb1 C13 101.07(8) . . ? O1 Rb1 C13 97.28(7) . . ? O5 Rb1 C13 112.43(8) . . ? O3 Rb1 C13 125.81(8) . . ? P1 Rb1 C13 29.55(5) . . ? C8 Rb1 C13 103.55(10) . . ? C13 P1 Rb1 78.85(11) . . ? C1 O1 C12 112.5(3) . . ? C1 O1 Rb1 102.0(2) . . ? C12 O1 Rb1 106.1(2) . . ? C3 O2 C2 111.2(3) . . ? C3 O2 Rb1 120.8(2) . . ? C2 O2 Rb1 116.6(3) . . ? C5 O3 C4 111.9(4) . . ? C5 O3 Rb1 109.2(3) . . ? C4 O3 Rb1 112.9(2) . . ? C7 O4 C6 111.8(3) . . ? C7 O4 Rb1 118.0(3) . . ? C6 O4 Rb1 121.6(3) . . ? C8 O5 C9 113.9(4) . . ? C8 O5 Rb1 102.6(3) . . ? C9 O5 Rb1 105.0(2) . . ? C11 O6 C10 113.2(4) . . ? C11 O6 Rb1 120.5(3) . . ? C10 O6 Rb1 120.8(2) . . ? O1 C1 C2 108.9(4) . . ? O2 C2 C1 109.0(4) . . ? O2 C3 C4 109.3(3) . . ? O3 C4 C3 108.8(4) . . ? O3 C5 C6 108.8(4) . . ? O4 C6 C5 109.5(4) . . ? O4 C7 C8 109.3(4) . . ? O5 C8 C7 109.5(4) . . ? O5 C8 Rb1 54.8(2) . . ? C7 C8 Rb1 86.6(3) . . ? O5 C9 C10 109.9(4) . . ? O6 C10 C9 108.9(4) . . ? O6 C11 C12 107.8(4) . . ? O1 C12 C11 109.0(3) . . ? C18 C13 C14 116.4(3) . . ? C18 C13 P1 121.6(2) . . ? C14 C13 P1 121.9(3) . . ? C18 C13 Rb1 89.4(2) . . ? C14 C13 Rb1 108.7(2) . . ? P1 C13 Rb1 71.60(10) . . ? C15 C14 C13 118.5(3) . . ? C15 C14 C23 116.8(3) . . ? C13 C14 C23 124.6(3) . . ? C16 C15 C14 124.7(3) . . ? C15 C16 C17 116.6(3) . . ? C15 C16 C27 122.5(3) . . ? C17 C16 C27 120.8(3) . . ? C16 C17 C18 123.6(3) . . ? C17 C18 C13 119.8(3) . . ? C17 C18 C19 114.9(3) . . ? C13 C18 C19 125.3(3) . . ? C22 C19 C20 105.5(3) . . ? C22 C19 C21 111.2(3) . . ? C20 C19 C21 104.7(3) . . ? C22 C19 C18 111.6(3) . . ? C20 C19 C18 112.8(3) . . ? C21 C19 C18 110.8(3) . . ? C25 C23 C26 111.9(3) . . ? C25 C23 C24 104.6(3) . . ? C26 C23 C24 104.4(3) . . ? C25 C23 C14 111.3(3) . . ? C26 C23 C14 111.8(3) . . ? C24 C23 C14 112.4(3) . . ? C28 C27 C29 113.0(5) . . ? C30' C27 C29' 112.9(7) . . ? C28 C27 C16 109.7(4) . . ? C30' C27 C16 113.7(6) . . ? C29 C27 C16 113.0(4) . . ? C29' C27 C16 111.8(5) . . ? C28 C27 C30 106.4(5) . . ? C29 C27 C30 106.1(5) . . ? C16 C27 C30 108.3(4) . . ? C30' C27 C28' 105.4(6) . . ? C29' C27 C28' 104.0(7) . . ? C16 C27 C28' 108.3(5) . . ? _refine_diff_density_max 0.743 _refine_diff_density_min -0.886 _refine_diff_density_rms 0.097 data_rabx _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C30 H54 K O6 P' _chemical_formula_weight 580.80 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 40.7745(2) _cell_length_b 9.0007(2) _cell_length_c 19.1484(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.6550(10) _cell_angle_gamma 90.00 _cell_volume 6732.6(2) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6608 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.146 _exptl_crystal_density_method ? _exptl_crystal_F_000 2528 _exptl_absorpt_coefficient_mu 0.242 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'Siemens P4/CCD' _diffrn_measurement_method 'phi, omega' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10746 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0741 _diffrn_reflns_limit_h_min -54 _diffrn_reflns_limit_h_max 54 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.04 _diffrn_reflns_theta_max 28.39 _reflns_number_total 6861 _reflns_number_observed 4742 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-5.03 (Sheldrick, 1994)' _computing_structure_refinement 'SHELXL-5.03 (Sheldrick, 1994)' _computing_molecular_graphics XP _computing_publication_material XCIF _refine_special_details ; Refinement on F^2^ for ALL reflections except for 5 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0800P)^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 'idealized contributions' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6856 _refine_ls_number_parameters 371 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0881 _refine_ls_R_factor_obs 0.0572 _refine_ls_wR_factor_all 0.1809 _refine_ls_wR_factor_obs 0.1509 _refine_ls_goodness_of_fit_all 1.146 _refine_ls_goodness_of_fit_obs 1.230 _refine_ls_restrained_S_all 1.214 _refine_ls_restrained_S_obs 1.230 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group K1 K 0.664028(13) 0.89538(6) 0.60809(3) 0.0368(2) Uani 1 d . . P1 P 0.64977(2) 1.21214(8) 0.69966(4) 0.0383(2) Uani 1 d . . O21 O 0.68195(5) 0.7511(2) 0.74860(10) 0.0491(5) Uani 1 d . . O22 O 0.61517(5) 0.7439(2) 0.65313(11) 0.0445(5) Uani 1 d . . O23 O 0.60356(5) 0.7846(2) 0.50337(11) 0.0481(5) Uani 1 d . . O24 O 0.65619(5) 0.9094(2) 0.45314(10) 0.0506(5) Uani 1 d . . O25 O 0.72277(5) 0.8725(2) 0.54440(11) 0.0493(5) Uani 1 d . . O26 O 0.73309(5) 0.8856(2) 0.69518(11) 0.0510(5) Uani 1 d . . C1 C 0.57992(6) 1.2353(3) 0.60484(12) 0.0282(5) Uani 1 d . . C2 C 0.55703(6) 1.2528(3) 0.53503(13) 0.0314(5) Uani 1 d . . H2A H 0.53369(6) 1.2346(3) 0.52912(13) 0.038 Uiso 1 calc R . C3 C 0.56673(6) 1.2950(3) 0.47428(13) 0.0306(5) Uani 1 d . . C4 C 0.60092(5) 1.3263(3) 0.48554(12) 0.0292(5) Uani 1 d . . H4A H 0.60796(5) 1.3585(3) 0.44541(12) 0.035 Uiso 1 calc R . C5 C 0.62578(5) 1.3133(2) 0.55266(12) 0.0259(5) Uani 1 d . . C6 C 0.61631(5) 1.2565(2) 0.61505(12) 0.0254(5) Uani 1 d . . C7 C 0.56370(6) 1.1981(3) 0.66764(13) 0.0349(6) Uani 1 d . . C8 C 0.57324(8) 1.0405(3) 0.6981(2) 0.0463(7) Uani 1 d . . H8A H 0.56670(8) 0.9689(3) 0.6587(2) 0.070 Uiso 1 calc R . H8B H 0.56129(8) 1.0184(3) 0.7340(2) 0.070 Uiso 1 calc R . H8C H 0.59774(8) 1.0349(3) 0.7209(2) 0.070 Uiso 1 calc R . C9 C 0.57348(8) 1.3163(3) 0.7277(2) 0.0501(7) Uani 1 d . . H9A H 0.56710(8) 1.4138(3) 0.7065(2) 0.075 Uiso 1 calc R . H9B H 0.59799(8) 1.3132(3) 0.7507(2) 0.075 Uiso 1 calc R . H9C H 0.56154(8) 1.2968(3) 0.7638(2) 0.075 Uiso 1 calc R . C10 C 0.52414(7) 1.1992(4) 0.6415(2) 0.0618(9) Uani 1 d . . H10A H 0.51615(7) 1.1262(4) 0.6032(2) 0.093 Uiso 1 calc R . H10B H 0.51617(7) 1.2970(4) 0.6230(2) 0.093 Uiso 1 calc R . H10C H 0.51528(7) 1.1750(4) 0.6821(2) 0.093 Uiso 1 calc R . C11 C 0.54070(6) 1.3136(3) 0.39814(14) 0.0417(7) Uani 1 d . . C12 C 0.50348(11) 1.3071(8) 0.3999(3) 0.060(2) Uani 0.60 d P 1 H12A H 0.49985(11) 1.3805(8) 0.4341(3) 0.091 Uiso 0.60 calc PR 1 H12B H 0.49857(11) 1.2089(8) 0.4152(3) 0.091 Uiso 0.60 calc PR 1 H12C H 0.48840(11) 1.3278(8) 0.3517(3) 0.091 Uiso 0.60 calc PR 1 C13 C 0.54638(14) 1.4719(7) 0.3663(3) 0.060(2) Uani 0.60 d P 1 H13A H 0.54243(14) 1.5493(7) 0.3982(3) 0.090 Uiso 0.60 calc PR 1 H13B H 0.53050(14) 1.4839(7) 0.3181(3) 0.090 Uiso 0.60 calc PR 1 H13C H 0.56967(14) 1.4789(7) 0.3632(3) 0.090 Uiso 0.60 calc PR 1 C14 C 0.5474(2) 1.2022(9) 0.3459(3) 0.073(2) Uani 0.60 d P 1 H14A H 0.5711(2) 1.2087(9) 0.3458(3) 0.109 Uiso 0.60 calc PR 1 H14B H 0.5326(2) 1.2225(9) 0.2973(3) 0.109 Uiso 0.60 calc PR 1 H14C H 0.5428(2) 1.1031(9) 0.3607(3) 0.109 Uiso 0.60 calc PR 1 C12' C 0.5161(2) 1.1703(12) 0.3849(5) 0.074(3) Uani 0.40 d P 2 H12D H 0.5295(2) 1.0816(12) 0.3842(5) 0.111 Uiso 0.40 calc PR 2 H12E H 0.4986(2) 1.1801(12) 0.3386(5) 0.111 Uiso 0.40 calc PR 2 H12F H 0.5054(2) 1.1626(12) 0.4239(5) 0.111 Uiso 0.40 calc PR 2 C13' C 0.5196(3) 1.4416(15) 0.3984(6) 0.114(6) Uani 0.40 d P 2 H13D H 0.5102(3) 1.4355(15) 0.4394(6) 0.171 Uiso 0.40 calc PR 2 H13E H 0.5011(3) 1.4447(15) 0.3533(6) 0.171 Uiso 0.40 calc PR 2 H13F H 0.5334(3) 1.5309(15) 0.4026(6) 0.171 Uiso 0.40 calc PR 2 C14' C 0.5577(3) 1.3061(17) 0.3370(5) 0.086(4) Uani 0.40 d P 2 H14D H 0.5713(3) 1.2162(17) 0.3421(5) 0.128 Uiso 0.40 calc PR 2 H14E H 0.5724(3) 1.3920(17) 0.3398(5) 0.128 Uiso 0.40 calc PR 2 H14F H 0.5402(3) 1.3055(17) 0.2904(5) 0.128 Uiso 0.40 calc PR 2 C15 C 0.66245(5) 1.3697(3) 0.55475(13) 0.0306(5) Uani 1 d . . C16 C 0.67409(6) 1.4945(3) 0.6114(2) 0.0430(7) Uani 1 d . . H16A H 0.67408(6) 1.4580(3) 0.6590(2) 0.065 Uiso 1 calc R . H16B H 0.65851(6) 1.5780(3) 0.5980(2) 0.065 Uiso 1 calc R . H16C H 0.69701(6) 1.5260(3) 0.6128(2) 0.065 Uiso 1 calc R . C17 C 0.66343(7) 1.4395(5) 0.4822(2) 0.0680(11) Uani 1 d . . H17A H 0.64724(7) 1.5211(5) 0.4701(2) 0.102 Uiso 1 calc R . H17B H 0.65736(7) 1.3652(5) 0.4440(2) 0.102 Uiso 1 calc R . H17C H 0.68630(7) 1.4764(5) 0.4867(2) 0.102 Uiso 1 calc R . C18 C 0.68869(6) 1.2427(3) 0.5692(2) 0.0447(7) Uani 1 d . . H18A H 0.68924(6) 1.1941(3) 0.6147(2) 0.067 Uiso 1 calc R . H18B H 0.71117(6) 1.2826(3) 0.5723(2) 0.067 Uiso 1 calc R . H18C H 0.68224(6) 1.1714(3) 0.5297(2) 0.067 Uiso 1 calc R . C21 C 0.65228(9) 0.7564(4) 0.7730(2) 0.0599(9) Uani 1 d . . H21A H 0.64511(9) 0.8599(4) 0.7750(2) 0.072 Uiso 1 calc R . H21B H 0.65740(9) 0.7145(4) 0.8222(2) 0.072 Uiso 1 calc R . C22 C 0.62421(9) 0.6706(4) 0.7225(2) 0.0586(9) Uani 1 d . . H22A H 0.63180(9) 0.5688(4) 0.7175(2) 0.070 Uiso 1 calc R . H22B H 0.60435(9) 0.6661(4) 0.7416(2) 0.070 Uiso 1 calc R . C23 C 0.58653(7) 0.6791(4) 0.6012(2) 0.0565(8) Uani 1 d . . H23A H 0.56745(7) 0.6677(4) 0.6224(2) 0.068 Uiso 1 calc R . H23B H 0.59260(7) 0.5807(4) 0.5868(2) 0.068 Uiso 1 calc R . C24 C 0.57640(7) 0.7790(4) 0.5365(2) 0.0589(9) Uani 1 d . . H24A H 0.55555(7) 0.7414(4) 0.5014(2) 0.071 Uiso 1 calc R . H24B H 0.57171(7) 0.8790(4) 0.5515(2) 0.071 Uiso 1 calc R . C25 C 0.59692(8) 0.8862(4) 0.4438(2) 0.0599(9) Uani 1 d . . H25A H 0.59734(8) 0.9884(4) 0.4616(2) 0.072 Uiso 1 calc R . H25B H 0.57425(8) 0.8669(4) 0.4100(2) 0.072 Uiso 1 calc R . C26 C 0.62367(8) 0.8663(4) 0.4058(2) 0.0596(9) Uani 1 d . . H26A H 0.62444(8) 0.7620(4) 0.3916(2) 0.071 Uiso 1 calc R . H26B H 0.61816(8) 0.9271(4) 0.3615(2) 0.071 Uiso 1 calc R . C27 C 0.68326(9) 0.8617(4) 0.4260(2) 0.0550(8) Uani 1 d . . H27A H 0.67898(9) 0.8935(4) 0.3752(2) 0.066 Uiso 1 calc R . H27B H 0.68478(9) 0.7531(4) 0.4276(2) 0.066 Uiso 1 calc R . C28 C 0.71613(8) 0.9279(4) 0.4718(2) 0.0554(8) Uani 1 d . . H28A H 0.73493(8) 0.9009(4) 0.4519(2) 0.067 Uiso 1 calc R . H28B H 0.71431(8) 1.0364(4) 0.4718(2) 0.067 Uiso 1 calc R . C29 C 0.75236(7) 0.9382(4) 0.5924(2) 0.0593(9) Uani 1 d . . H29A H 0.74829(7) 1.0441(4) 0.5983(2) 0.071 Uiso 1 calc R . H29B H 0.77176(7) 0.9286(4) 0.5721(2) 0.071 Uiso 1 calc R . C30 C 0.76041(7) 0.8621(4) 0.6646(2) 0.0652(10) Uani 1 d . . H30A H 0.76353(7) 0.7554(4) 0.6585(2) 0.078 Uiso 1 calc R . H30B H 0.78168(7) 0.9021(4) 0.6972(2) 0.078 Uiso 1 calc R . C31 C 0.73980(8) 0.8186(4) 0.7651(2) 0.0662(10) Uani 1 d . . H31A H 0.75989(8) 0.8648(4) 0.7989(2) 0.079 Uiso 1 calc R . H31B H 0.74449(8) 0.7124(4) 0.7618(2) 0.079 Uiso 1 calc R . C32 C 0.70913(9) 0.8392(4) 0.7921(2) 0.0641(9) Uani 1 d . . H32B H 0.71449(9) 0.8087(4) 0.8433(2) 0.077 Uiso 1 calc R . H32A H 0.70241(9) 0.9441(4) 0.7887(2) 0.077 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K1 0.0410(3) 0.0353(4) 0.0328(3) -0.0004(2) 0.0084(2) -0.0041(2) P1 0.0352(4) 0.0432(4) 0.0304(3) 0.0043(3) -0.0003(2) 0.0045(3) O21 0.0644(13) 0.0472(13) 0.0373(11) -0.0019(9) 0.0172(9) 0.0111(9) O22 0.0510(11) 0.0308(11) 0.0563(13) -0.0008(9) 0.0229(9) -0.0018(8) O23 0.0426(11) 0.0490(13) 0.0483(12) -0.0055(9) 0.0059(8) 0.0092(8) O24 0.0645(13) 0.0516(13) 0.0353(10) -0.0028(9) 0.0137(9) 0.0115(9) O25 0.0500(11) 0.0470(13) 0.0567(12) 0.0020(10) 0.0248(9) 0.0026(9) O26 0.0390(10) 0.0601(14) 0.0474(11) -0.0053(10) 0.0020(8) 0.0104(9) C1 0.0308(12) 0.0256(13) 0.0292(12) 0.0007(9) 0.0099(9) 0.0041(9) C2 0.0224(11) 0.0346(15) 0.0365(13) 0.0027(10) 0.0075(9) 0.0004(9) C3 0.0304(12) 0.0293(14) 0.0293(12) 0.0032(10) 0.0040(9) 0.0009(9) C4 0.0313(12) 0.0289(13) 0.0281(12) 0.0030(10) 0.0097(9) 0.0002(9) C5 0.0252(11) 0.0235(12) 0.0298(12) -0.0017(9) 0.0092(8) 0.0022(8) C6 0.0286(11) 0.0217(13) 0.0260(11) -0.0017(9) 0.0081(8) 0.0030(8) C7 0.0345(13) 0.039(2) 0.0361(13) 0.0054(11) 0.0169(10) 0.0043(10) C8 0.063(2) 0.035(2) 0.046(2) 0.0062(13) 0.0241(13) -0.0046(13) C9 0.072(2) 0.039(2) 0.050(2) 0.0023(13) 0.0355(15) 0.0079(14) C10 0.036(2) 0.097(3) 0.060(2) 0.021(2) 0.0257(13) 0.006(2) C11 0.0371(14) 0.051(2) 0.0300(13) 0.0034(12) -0.0014(10) 0.0028(11) C12 0.032(2) 0.087(5) 0.051(3) 0.013(3) -0.007(2) -0.002(3) C13 0.047(3) 0.066(4) 0.056(3) 0.030(3) -0.003(2) 0.002(3) C14 0.072(4) 0.093(6) 0.037(3) -0.014(3) -0.010(3) 0.031(4) C12' 0.059(5) 0.085(7) 0.056(5) 0.013(5) -0.018(4) -0.024(5) C13' 0.122(10) 0.103(10) 0.070(7) -0.024(6) -0.048(7) 0.080(8) C14' 0.083(7) 0.126(11) 0.035(5) 0.008(6) -0.004(4) -0.015(7) C15 0.0238(11) 0.0335(15) 0.0366(13) -0.0009(10) 0.0119(9) -0.0010(9) C16 0.0330(13) 0.029(2) 0.068(2) -0.0102(13) 0.0151(12) -0.0049(10) C17 0.040(2) 0.109(3) 0.056(2) 0.024(2) 0.0151(14) -0.019(2) C18 0.0319(13) 0.039(2) 0.064(2) -0.0175(13) 0.0156(12) 0.0033(11) C21 0.085(2) 0.062(2) 0.040(2) 0.011(2) 0.030(2) 0.018(2) C22 0.078(2) 0.045(2) 0.071(2) 0.020(2) 0.050(2) 0.012(2) C23 0.043(2) 0.051(2) 0.084(2) -0.018(2) 0.033(2) -0.0083(13) C24 0.036(2) 0.064(2) 0.072(2) -0.021(2) 0.0082(14) 0.0019(13) C25 0.058(2) 0.059(2) 0.047(2) -0.005(2) -0.0090(14) 0.0163(15) C26 0.074(2) 0.064(2) 0.0325(15) 0.0021(15) 0.0010(14) 0.015(2) C27 0.085(2) 0.048(2) 0.041(2) 0.0001(14) 0.0335(15) 0.009(2) C28 0.078(2) 0.046(2) 0.058(2) 0.0033(15) 0.046(2) 0.0080(15) C29 0.034(2) 0.064(2) 0.084(2) 0.000(2) 0.0230(15) 0.0057(13) C30 0.036(2) 0.076(3) 0.081(2) -0.005(2) 0.0106(15) 0.0144(15) C31 0.060(2) 0.076(2) 0.045(2) -0.004(2) -0.0128(14) 0.015(2) C32 0.086(2) 0.070(2) 0.0266(14) -0.0066(15) 0.0004(14) 0.010(2) _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 K1 O22 2.749(2) . ? K1 O26 2.833(2) . ? K1 O23 2.874(2) . ? K1 O21 2.887(2) . ? K1 O24 2.894(2) . ? K1 O25 2.990(2) . ? K1 P1 3.4822(9) . ? P1 C6 1.838(2) . ? O21 C21 1.417(4) . ? O21 C32 1.422(4) . ? O22 C23 1.424(3) . ? O22 C22 1.434(4) . ? O23 C24 1.426(4) . ? O23 C25 1.427(4) . ? O24 C27 1.415(4) . ? O24 C26 1.429(4) . ? O25 C29 1.419(4) . ? O25 C28 1.427(4) . ? O26 C30 1.414(4) . ? O26 C31 1.421(4) . ? C1 C2 1.403(3) . ? C1 C6 1.452(3) . ? C1 C7 1.566(3) . ? C2 C3 1.385(3) . ? C3 C4 1.378(3) . ? C3 C11 1.547(3) . ? C4 C5 1.395(3) . ? C5 C6 1.450(3) . ? C5 C15 1.569(3) . ? C7 C9 1.533(4) . ? C7 C8 1.541(4) . ? C7 C10 1.546(4) . ? C11 C13' 1.438(9) . ? C11 C14 1.496(7) . ? C11 C14' 1.522(12) . ? C11 C12 1.529(6) . ? C11 C13 1.593(6) . ? C11 C12' 1.608(9) . ? C15 C17 1.536(4) . ? C15 C18 1.536(3) . ? C15 C16 1.538(3) . ? C21 C22 1.485(5) . ? C23 C24 1.491(5) . ? C25 C26 1.484(5) . ? C27 C28 1.499(5) . ? C29 C30 1.493(5) . ? C31 C32 1.496(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O22 K1 O26 119.16(6) . . ? O22 K1 O23 59.53(6) . . ? O26 K1 O23 155.38(6) . . ? O22 K1 O21 59.80(6) . . ? O26 K1 O21 59.60(6) . . ? O23 K1 O21 115.57(6) . . ? O22 K1 O24 117.79(6) . . ? O26 K1 O24 113.81(6) . . ? O23 K1 O24 58.63(6) . . ? O21 K1 O24 154.04(6) . . ? O22 K1 O25 146.21(6) . . ? O26 K1 O25 57.36(6) . . ? O23 K1 O25 108.60(6) . . ? O21 K1 O25 109.32(6) . . ? O24 K1 O25 56.69(6) . . ? O22 K1 P1 90.43(4) . . ? O26 K1 P1 90.59(4) . . ? O23 K1 P1 113.68(4) . . ? O21 K1 P1 86.17(4) . . ? O24 K1 P1 119.69(4) . . ? O25 K1 P1 122.04(4) . . ? C6 P1 K1 85.57(7) . . ? C21 O21 C32 112.6(2) . . ? C21 O21 K1 106.3(2) . . ? C32 O21 K1 104.0(2) . . ? C23 O22 C22 113.6(2) . . ? C23 O22 K1 120.5(2) . . ? C22 O22 K1 120.1(2) . . ? C24 O23 C25 112.6(2) . . ? C24 O23 K1 108.8(2) . . ? C25 O23 K1 105.3(2) . . ? C27 O24 C26 111.4(2) . . ? C27 O24 K1 119.7(2) . . ? C26 O24 K1 116.6(2) . . ? C29 O25 C28 112.0(2) . . ? C29 O25 K1 109.8(2) . . ? C28 O25 K1 115.0(2) . . ? C30 O26 C31 111.4(2) . . ? C30 O26 K1 121.9(2) . . ? C31 O26 K1 117.3(2) . . ? C2 C1 C6 119.3(2) . . ? C2 C1 C7 116.3(2) . . ? C6 C1 C7 124.4(2) . . ? C3 C2 C1 124.0(2) . . ? C4 C3 C2 116.4(2) . . ? C4 C3 C11 121.0(2) . . ? C2 C3 C11 122.5(2) . . ? C3 C4 C5 124.2(2) . . ? C4 C5 C6 119.6(2) . . ? C4 C5 C15 115.6(2) . . ? C6 C5 C15 124.7(2) . . ? C5 C6 C1 116.0(2) . . ? C5 C6 P1 119.8(2) . . ? C1 C6 P1 124.2(2) . . ? C9 C7 C8 111.8(2) . . ? C9 C7 C10 105.1(2) . . ? C8 C7 C10 104.8(2) . . ? C9 C7 C1 110.5(2) . . ? C8 C7 C1 111.8(2) . . ? C10 C7 C1 112.4(2) . . ? C13' C11 C14' 116.2(9) . . ? C14 C11 C12 111.2(4) . . ? C13' C11 C3 109.4(4) . . ? C14 C11 C3 110.5(3) . . ? C14' C11 C3 112.3(4) . . ? C12 C11 C3 113.1(3) . . ? C14 C11 C13 105.6(5) . . ? C12 C11 C13 107.3(4) . . ? C3 C11 C13 108.8(3) . . ? C13' C11 C12' 107.3(8) . . ? C14' C11 C12' 104.1(7) . . ? C3 C11 C12' 106.9(3) . . ? C17 C15 C18 105.7(2) . . ? C17 C15 C16 104.9(2) . . ? C18 C15 C16 111.0(2) . . ? C17 C15 C5 112.4(2) . . ? C18 C15 C5 111.9(2) . . ? C16 C15 C5 110.7(2) . . ? O21 C21 C22 109.9(3) . . ? O22 C22 C21 108.0(3) . . ? O22 C23 C24 108.1(3) . . ? O23 C24 C23 109.0(2) . . ? O23 C25 C26 108.5(2) . . ? O24 C26 C25 109.6(2) . . ? O24 C27 C28 109.0(2) . . ? O25 C28 C27 108.7(2) . . ? O25 C29 C30 109.2(3) . . ? O26 C30 C29 108.9(2) . . ? O26 C31 C32 108.6(2) . . ? O21 C32 C31 108.4(3) . . ? _refine_diff_density_max 0.689 _refine_diff_density_min -0.387 _refine_diff_density_rms 0.068