#Supplementary Material (ESI) for Dalton Transactions #This journal is (c) The Royal Society of Chemistry 2001 ---------- X-Sun-Charset: us-ascii X-Sun-Content-Lines: 1765 data_global _publ_contact_author ; Hey-Hawkins, Evamarie Institut f\"ur Anorganische Chemie Universit\"at Leipzig Johannisallee 29 04103 Leipzig Bundesrepublik Deutschland ; _publ_contact_author_phone '49 / 341 / 9736151' _publ_contact_author_fax '49 / 341 / 9736199' _publ_contact_author_email hey@rz.uni-leipzig.de _publ_requested_journal ; J. Chem. Soc., Dalton Trans. ; #------------------------------------------------------------------------------- _publ_section_title ; Syntheses and solid-state structures of [{K(THF)~2~(PHTipp)K(THF)(\m-THF)(PHTipp)}~x~]~2~ and [Rb(THF)(PHTipp)]~x~ (Tipp == 2,4,6-Pri3C6H2) ; loop_ _publ_author_name _publ_author_address ; Christoph, Frenzel ; ; Institut f\"ur Anorganische Chemie Universit\"at Leipzig Johannisallee 29 04103 Leipzig Bundesrepublik Deutschland ; ; Somoza Jr., Fernando ; ; Institut f\"ur Anorganische Chemie Universit\"at Leipzig Johannisallee 29 04103 Leipzig Bundesrepublik Deutschland ; ; Blaurock, Steffen ; ; Institut f\"ur Anorganische Chemie Universit\"at Leipzig Johannisallee 29 04103 Leipzig Bundesrepublik Deutschland ; ; Hey-Hawkins, Evamarie ; ; Institut f\"ur Anorganische Chemie Universit\"at Leipzig Johannisallee 29 04103 Leipzig Bundesrepublik Deutschland ; _journal_name_full ; Journal of the Chemical Society, Dalton Transactions ; _journal_volume ? _journal_page_first ? _journal_page_last ? _journal_year 2001 _ccdc_journal_depnumber ? #------------------------------------------------------------------------------# # DATA BLOCK # #------------------------------------------------------------------------------# data_c268 _database_code_CSD 165077 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H80 K2 O4 P2' _chemical_formula_weight 837.24 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' 'K' 'K' 0.2009 0.2494 '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' _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 34.9726(10) _cell_length_b 11.5969(3) _cell_length_c 28.4498(9) _cell_angle_alpha 90.00 _cell_angle_beta 115.202(2) _cell_angle_gamma 90.00 _cell_volume 10440.2(5) _cell_formula_units_Z 8 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.56 _cell_measurement_theta_max 25.24 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.065 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3648 _exptl_absorpt_coefficient_mu 0.278 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.8969 _exptl_absorpt_correction_T_max 0.9465 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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-Diffractometer (AXS-Bruker)' _diffrn_measurement_method 'omega-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20635 _diffrn_reflns_av_R_equivalents 0.0477 _diffrn_reflns_av_sigmaI/netI 0.0476 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.24 _reflns_number_total 8443 _reflns_number_gt 5549 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (AXS-Bruker)' _computing_cell_refinement 'SAINT (AXS-Bruker)' _computing_data_reduction 'SAINT (AXS-Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (AXS-Bruker)' _computing_publication_material ? _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^)+(0.0000P)^2^+32.1969P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8443 _refine_ls_number_parameters 518 _refine_ls_number_restraints 223 _refine_ls_R_factor_all 0.1239 _refine_ls_R_factor_gt 0.0825 _refine_ls_wR_factor_ref 0.1542 _refine_ls_wR_factor_gt 0.1414 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.103 _refine_ls_shift/su_max 0.270 _refine_ls_shift/su_mean 0.020 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 K1 K 0.05130(3) 0.77348(9) 0.32733(4) 0.0724(3) Uani 1 1 d . . . K2 K 0.14208(4) 0.27170(9) 0.37476(4) 0.0858(3) Uani 1 1 d . . . P1 P 0.11037(4) 1.00627(11) 0.34240(5) 0.0696(3) Uani 1 1 d . . . H1 H 0.1466 0.9573 0.3766 0.084 Uiso 1 1 calc R . . P2 P 0.09282(4) 0.51438(11) 0.36594(5) 0.0749(4) Uani 1 1 d . A . H2 H 0.0551 0.4635 0.3540 0.090 Uiso 1 1 calc R . . O1 O 0.03440(9) 0.7168(2) 0.22330(11) 0.0712(8) Uani 1 1 d D . . O2 O 0.03965(19) 0.8207(4) 0.41186(17) 0.154(2) Uani 1 1 d D B . O3 O 0.19226(15) 0.3235(3) 0.32868(18) 0.1276(15) Uani 1 1 d D A . O4 O 0.19009(13) 0.2303(3) 0.47467(14) 0.1064(12) Uani 1 1 d D A . C1 C 0.12546(13) 1.0077(4) 0.28810(16) 0.0620(11) Uani 1 1 d . . . C2 C 0.16011(14) 0.9435(4) 0.28709(18) 0.0717(12) Uani 1 1 d . B . C3 C 0.16734(15) 0.9441(4) 0.2432(2) 0.0839(14) Uani 1 1 d . . . H3 H 0.1905 0.9017 0.2438 0.101 Uiso 1 1 calc R B . C4 C 0.14273(17) 1.0032(5) 0.1981(2) 0.0844(14) Uani 1 1 d . B . C5 C 0.10964(16) 1.0681(4) 0.19942(18) 0.0818(14) Uani 1 1 d . . . H5 H 0.0926 1.1111 0.1699 0.098 Uiso 1 1 calc R B . C6 C 0.10071(14) 1.0720(4) 0.24286(17) 0.0672(12) Uani 1 1 d . B . C7 C 0.19012(16) 0.8741(5) 0.3342(2) 0.0896(16) Uani 1 1 d . . . H7 H 0.1732 0.8435 0.3519 0.108 Uiso 1 1 calc R B . C8 C 0.2117(2) 0.7711(6) 0.3217(3) 0.168(3) Uani 1 1 d . B . H8A H 0.1904 0.7208 0.2971 0.251 Uiso 1 1 calc R . . H8B H 0.2281 0.7287 0.3533 0.251 Uiso 1 1 calc R . . H8C H 0.2303 0.7987 0.3067 0.251 Uiso 1 1 calc R . . C9 C 0.22385(18) 0.9528(6) 0.3727(2) 0.141(3) Uani 1 1 d . B . H9A H 0.2104 1.0175 0.3812 0.211 Uiso 1 1 calc R . . H9B H 0.2421 0.9809 0.3573 0.211 Uiso 1 1 calc R . . H9C H 0.2406 0.9099 0.4041 0.211 Uiso 1 1 calc R . . C10 C 0.1501(2) 0.9970(6) 0.1493(2) 0.116(2) Uani 1 1 d . . . H10 H 0.1733 0.9400 0.1589 0.140 Uiso 1 1 calc R B . C11 C 0.1153(2) 0.9393(8) 0.1057(3) 0.169(3) Uani 1 1 d . B . H11A H 0.1062 0.8719 0.1185 0.254 Uiso 1 1 calc R . . H11B H 0.1250 0.9159 0.0799 0.254 Uiso 1 1 calc R . . H11C H 0.0917 0.9923 0.0901 0.254 Uiso 1 1 calc R . . C12 C 0.1694(3) 1.1019(6) 0.1397(3) 0.166(3) Uani 1 1 d . B . H12A H 0.1921 1.1276 0.1720 0.250 Uiso 1 1 calc R . . H12B H 0.1482 1.1620 0.1262 0.250 Uiso 1 1 calc R . . H12C H 0.1807 1.0851 0.1147 0.250 Uiso 1 1 calc R . . C13 C 0.06278(16) 1.1415(4) 0.23913(19) 0.0828(14) Uani 1 1 d . . . H13 H 0.0622 1.1379 0.2736 0.099 Uiso 1 1 calc R B . C14 C 0.0668(2) 1.2689(5) 0.2276(3) 0.130(2) Uani 1 1 d . B . H14A H 0.0422 1.3107 0.2256 0.195 Uiso 1 1 calc R . . H14B H 0.0689 1.2754 0.1947 0.195 Uiso 1 1 calc R . . H14C H 0.0920 1.3011 0.2551 0.195 Uiso 1 1 calc R . . C15 C 0.02130(17) 1.0920(6) 0.2000(3) 0.136(3) Uani 1 1 d . B . H15A H -0.0019 1.1390 0.1992 0.205 Uiso 1 1 calc R . . H15B H 0.0181 1.0138 0.2099 0.205 Uiso 1 1 calc R . . H15C H 0.0212 1.0914 0.1658 0.205 Uiso 1 1 calc R . . C16 C 0.10702(12) 0.5186(3) 0.43577(15) 0.0580(10) Uani 1 1 d . . . C17 C 0.08650(14) 0.4495(4) 0.45909(17) 0.0688(12) Uani 1 1 d . A . C18 C 0.09797(15) 0.4572(4) 0.51249(19) 0.0773(13) Uani 1 1 d . . . H18 H 0.0834 0.4121 0.5270 0.093 Uiso 1 1 calc R A . C19 C 0.13054(15) 0.5299(4) 0.54520(17) 0.0716(12) Uani 1 1 d . A . C20 C 0.15035(13) 0.5962(4) 0.52246(17) 0.0652(11) Uani 1 1 d . . . H20 H 0.1720 0.6462 0.5435 0.078 Uiso 1 1 calc R A . C21 C 0.13988(12) 0.5928(4) 0.46969(16) 0.0602(11) Uani 1 1 d . A . C22 C 0.05084(17) 0.3662(5) 0.4274(2) 0.0939(17) Uani 1 1 d . . . H22 H 0.0486 0.3673 0.3915 0.113 Uiso 1 1 calc R A . C23 C 0.0598(2) 0.2445(5) 0.4458(3) 0.156(3) Uani 1 1 d . A . H23A H 0.0872 0.2218 0.4478 0.234 Uiso 1 1 calc R . . H23B H 0.0382 0.1944 0.4216 0.234 Uiso 1 1 calc R . . H23C H 0.0600 0.2380 0.4799 0.234 Uiso 1 1 calc R . . C24 C 0.00887(17) 0.4047(6) 0.4241(3) 0.148(3) Uani 1 1 d . A . H24A H 0.0037 0.4838 0.4120 0.222 Uiso 1 1 calc R . . H24B H 0.0090 0.3996 0.4582 0.222 Uiso 1 1 calc R . . H24C H -0.0132 0.3555 0.4000 0.222 Uiso 1 1 calc R . . C25 C 0.14216(18) 0.5370(5) 0.60308(19) 0.0923(16) Uani 1 1 d . . . H25 H 0.1656 0.5935 0.6165 0.111 Uiso 1 1 calc R A . C26 C 0.16118(18) 0.4276(5) 0.6316(2) 0.1045(18) Uani 1 1 d . A . H26A H 0.1828 0.4006 0.6215 0.157 Uiso 1 1 calc R . . H26B H 0.1393 0.3693 0.6232 0.157 Uiso 1 1 calc R . . H26C H 0.1737 0.4420 0.6687 0.157 Uiso 1 1 calc R . . C27 C 0.10888(19) 0.5884(6) 0.6150(2) 0.124(2) Uani 1 1 d . A . H27A H 0.0986 0.6583 0.5948 0.186 Uiso 1 1 calc R . . H27B H 0.1203 0.6068 0.6517 0.186 Uiso 1 1 calc R . . H27C H 0.0858 0.5341 0.6064 0.186 Uiso 1 1 calc R . . C28 C 0.16472(13) 0.6687(4) 0.44911(18) 0.0719(12) Uani 1 1 d . . . H28 H 0.1461 0.6863 0.4124 0.086 Uiso 1 1 calc R A . C29 C 0.20301(15) 0.6031(5) 0.4501(2) 0.0976(17) Uani 1 1 d . A . H29A H 0.2186 0.6524 0.4368 0.146 Uiso 1 1 calc R . . H29B H 0.1935 0.5347 0.4285 0.146 Uiso 1 1 calc R . . H29C H 0.2212 0.5808 0.4855 0.146 Uiso 1 1 calc R . . C30 C 0.17909(18) 0.7837(4) 0.4776(2) 0.112(2) Uani 1 1 d . A . H30A H 0.1946 0.8270 0.4623 0.168 Uiso 1 1 calc R . . H30B H 0.1972 0.7694 0.5140 0.168 Uiso 1 1 calc R . . H30C H 0.1546 0.8277 0.4747 0.168 Uiso 1 1 calc R . . C31 C 0.03954(14) 0.5946(3) 0.21997(19) 0.0762(13) Uani 1 1 d D . . H31A H 0.0162 0.5628 0.1892 0.091 Uiso 1 1 calc R B . H31B H 0.0402 0.5557 0.2509 0.091 Uiso 1 1 calc R . . C32 C 0.0801(2) 0.5793(5) 0.2163(3) 0.129(2) Uani 1 1 d D B . H32A H 0.1027 0.5594 0.2503 0.155 Uiso 1 1 calc R . . H32B H 0.0779 0.5181 0.1915 0.155 Uiso 1 1 calc R . . C33 C 0.0886(2) 0.6885(6) 0.1987(4) 0.172(3) Uani 1 1 d DU . . H33A H 0.1186 0.7078 0.2176 0.206 Uiso 1 1 calc R B . H33B H 0.0817 0.6845 0.1616 0.206 Uiso 1 1 calc R . . C34 C 0.06327(18) 0.7752(4) 0.2078(2) 0.1039(18) Uani 1 1 d D B . H34A H 0.0812 0.8281 0.2352 0.125 Uiso 1 1 calc R . . H34B H 0.0477 0.8198 0.1760 0.125 Uiso 1 1 calc R . . C43 C 0.2049(7) 0.1143(8) 0.4898(6) 0.105(6) Uani 0.59(3) 1 d PD A 1 H43A H 0.2358 0.1103 0.5050 0.126 Uiso 0.59(3) 1 calc PR A 1 H43B H 0.1931 0.0612 0.4603 0.126 Uiso 0.59(3) 1 calc PR A 1 C44 C 0.1885(6) 0.0893(9) 0.5290(8) 0.103(5) Uani 0.59(3) 1 d PD A 1 H44A H 0.1607 0.0524 0.5127 0.124 Uiso 0.59(3) 1 calc PR A 1 H44B H 0.2078 0.0381 0.5561 0.124 Uiso 0.59(3) 1 calc PR A 1 C45 C 0.1855(7) 0.1990(12) 0.5508(6) 0.111(6) Uani 0.59(3) 1 d PD A 1 H45A H 0.1576 0.2072 0.5508 0.134 Uiso 0.59(3) 1 calc PR A 1 H45B H 0.2070 0.2046 0.5867 0.134 Uiso 0.59(3) 1 calc PR A 1 C46 C 0.1917(8) 0.2876(9) 0.5200(5) 0.118(11) Uani 0.59(3) 1 d PD A 1 H46A H 0.2191 0.3252 0.5388 0.141 Uiso 0.59(3) 1 calc PR A 1 H46B H 0.1694 0.3459 0.5106 0.141 Uiso 0.59(3) 1 calc PR A 1 C43' C 0.1895(11) 0.1118(8) 0.4893(6) 0.133(13) Uani 0.41(3) 1 d PD A 2 H43C H 0.2032 0.0623 0.4730 0.159 Uiso 0.41(3) 1 calc PR A 2 H43D H 0.1605 0.0851 0.4789 0.159 Uiso 0.41(3) 1 calc PR A 2 C44' C 0.2135(10) 0.111(2) 0.5468(6) 0.113(8) Uani 0.41(3) 1 d PD A 2 H44C H 0.2014 0.0544 0.5623 0.135 Uiso 0.41(3) 1 calc PR A 2 H44D H 0.2432 0.0912 0.5568 0.135 Uiso 0.41(3) 1 calc PR A 2 C45' C 0.2098(14) 0.226(2) 0.5635(6) 0.177(17) Uani 0.41(3) 1 d PD A 2 H45C H 0.1883 0.2277 0.5770 0.213 Uiso 0.41(3) 1 calc PR A 2 H45D H 0.2368 0.2504 0.5910 0.213 Uiso 0.41(3) 1 calc PR A 2 C46' C 0.1979(13) 0.2999(15) 0.5195(6) 0.099(11) Uani 0.41(3) 1 d PD A 2 H46C H 0.2207 0.3550 0.5249 0.119 Uiso 0.41(3) 1 calc PR A 2 H46D H 0.1725 0.3433 0.5145 0.119 Uiso 0.41(3) 1 calc PR A 2 C39 C 0.2119(6) 0.2355(9) 0.3113(8) 0.109(6) Uiso 0.412(18) 1 d PD A 1 H39A H 0.1913 0.1770 0.2909 0.131 Uiso 0.412(18) 1 calc PR A 1 H39B H 0.2347 0.1978 0.3408 0.131 Uiso 0.412(18) 1 calc PR A 1 C40 C 0.2289(6) 0.2974(13) 0.2788(7) 0.107(6) Uiso 0.412(18) 1 d PD A 1 H40A H 0.2586 0.2768 0.2891 0.129 Uiso 0.412(18) 1 calc PR A 1 H40B H 0.2127 0.2778 0.2420 0.129 Uiso 0.412(18) 1 calc PR A 1 C41 C 0.2251(7) 0.4182(13) 0.2870(9) 0.148(8) Uiso 0.412(18) 1 d PD A 1 H41A H 0.2516 0.4480 0.3139 0.178 Uiso 0.412(18) 1 calc PR A 1 H41B H 0.2183 0.4614 0.2549 0.178 Uiso 0.412(18) 1 calc PR A 1 C42 C 0.1916(7) 0.4299(12) 0.3032(11) 0.162(9) Uiso 0.412(18) 1 d PD A 1 H42A H 0.1969 0.4951 0.3271 0.194 Uiso 0.412(18) 1 calc PR A 1 H42B H 0.1644 0.4413 0.2733 0.194 Uiso 0.412(18) 1 calc PR A 1 C39' C 0.1986(5) 0.2568(9) 0.2898(5) 0.120(5) Uiso 0.588(18) 1 d PD A 2 H39C H 0.1738 0.2089 0.2702 0.144 Uiso 0.588(18) 1 calc PR A 2 H39D H 0.2233 0.2064 0.3061 0.144 Uiso 0.588(18) 1 calc PR A 2 C40' C 0.2053(6) 0.3408(12) 0.2553(5) 0.136(5) Uiso 0.588(18) 1 d PD A 2 H40C H 0.2328 0.3277 0.2546 0.163 Uiso 0.588(18) 1 calc PR A 2 H40D H 0.1832 0.3333 0.2199 0.163 Uiso 0.588(18) 1 calc PR A 2 C41' C 0.2040(6) 0.4529(10) 0.2754(5) 0.152(6) Uiso 0.588(18) 1 d PD A 2 H41C H 0.1783 0.4934 0.2522 0.182 Uiso 0.588(18) 1 calc PR A 2 H41D H 0.2285 0.4982 0.2779 0.182 Uiso 0.588(18) 1 calc PR A 2 C42' C 0.2046(4) 0.4398(6) 0.3257(4) 0.098(4) Uiso 0.588(18) 1 d PD A 2 H42C H 0.2330 0.4546 0.3529 0.118 Uiso 0.588(18) 1 calc PR A 2 H42D H 0.1848 0.4939 0.3300 0.118 Uiso 0.588(18) 1 calc PR A 2 C35 C 0.0272(7) 0.9293(10) 0.4245(5) 0.178(9) Uiso 0.459(11) 1 d PD B 1 H35A H -0.0019 0.9291 0.4212 0.214 Uiso 0.459(11) 1 calc PR B 1 H35B H 0.0314 0.9935 0.4048 0.214 Uiso 0.459(11) 1 calc PR B 1 C36 C 0.0597(7) 0.9261(13) 0.4802(7) 0.215(11) Uiso 0.459(11) 1 d PD B 1 H36A H 0.0882 0.9379 0.4826 0.258 Uiso 0.459(11) 1 calc PR B 1 H36B H 0.0540 0.9852 0.5010 0.258 Uiso 0.459(11) 1 calc PR B 1 C37 C 0.0553(6) 0.8126(12) 0.4972(4) 0.129(6) Uiso 0.459(11) 1 d PD B 1 H37A H 0.0821 0.7860 0.5247 0.155 Uiso 0.459(11) 1 calc PR B 1 H37B H 0.0337 0.8116 0.5106 0.155 Uiso 0.459(11) 1 calc PR B 1 C38 C 0.0431(5) 0.7419(8) 0.4525(4) 0.096(5) Uiso 0.459(11) 1 d PD B 1 H38A H 0.0160 0.7042 0.4446 0.115 Uiso 0.459(11) 1 calc PR B 1 H38B H 0.0645 0.6827 0.4574 0.115 Uiso 0.459(11) 1 calc PR B 1 C35' C 0.0547(4) 0.9288(7) 0.4362(4) 0.098(4) Uiso 0.541(11) 1 d PD B 2 H35C H 0.0498 0.9909 0.4109 0.118 Uiso 0.541(11) 1 calc PR B 2 H35D H 0.0846 0.9262 0.4605 0.118 Uiso 0.541(11) 1 calc PR B 2 C36' C 0.0262(5) 0.9383(10) 0.4637(6) 0.155(6) Uiso 0.541(11) 1 d PD B 2 H36C H 0.0392 0.9873 0.4946 0.186 Uiso 0.541(11) 1 calc PR B 2 H36D H -0.0012 0.9715 0.4406 0.186 Uiso 0.541(11) 1 calc PR B 2 C37' C 0.0208(5) 0.8229(11) 0.4782(5) 0.138(5) Uiso 0.541(11) 1 d PD B 2 H37C H 0.0426 0.8048 0.5130 0.165 Uiso 0.541(11) 1 calc PR B 2 H37D H -0.0070 0.8142 0.4785 0.165 Uiso 0.541(11) 1 calc PR B 2 C38' C 0.0245(7) 0.7482(10) 0.4406(6) 0.177(8) Uiso 0.541(11) 1 d PD B 2 H38C H -0.0030 0.7150 0.4180 0.213 Uiso 0.541(11) 1 calc PR B 2 H38D H 0.0444 0.6855 0.4575 0.213 Uiso 0.541(11) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K1 0.0834(7) 0.0667(6) 0.0661(6) -0.0071(5) 0.0311(5) -0.0143(5) K2 0.1049(8) 0.0639(7) 0.0902(8) 0.0061(6) 0.0432(7) -0.0025(6) P1 0.0771(8) 0.0634(7) 0.0706(8) 0.0003(6) 0.0335(6) -0.0059(6) P2 0.0844(8) 0.0714(8) 0.0578(7) 0.0058(6) 0.0196(6) 0.0027(7) O1 0.0752(19) 0.0650(19) 0.078(2) -0.0070(16) 0.0367(17) 0.0015(16) O2 0.306(7) 0.086(3) 0.118(3) -0.010(3) 0.137(4) -0.006(4) O3 0.177(4) 0.089(3) 0.167(4) -0.004(3) 0.122(4) -0.019(3) O4 0.146(3) 0.081(3) 0.084(3) 0.004(2) 0.041(2) 0.026(2) C1 0.061(3) 0.055(2) 0.067(3) -0.003(2) 0.024(2) -0.015(2) C2 0.065(3) 0.076(3) 0.079(3) 0.004(3) 0.035(3) -0.010(2) C3 0.072(3) 0.093(4) 0.090(4) 0.006(3) 0.037(3) 0.001(3) C4 0.084(3) 0.100(4) 0.080(3) -0.006(3) 0.045(3) -0.013(3) C5 0.089(4) 0.080(3) 0.067(3) 0.008(3) 0.024(3) -0.011(3) C6 0.067(3) 0.063(3) 0.069(3) 0.001(2) 0.027(2) -0.010(2) C7 0.073(3) 0.112(4) 0.087(4) 0.026(3) 0.037(3) 0.016(3) C8 0.201(8) 0.164(7) 0.161(7) 0.062(6) 0.099(6) 0.104(6) C9 0.082(4) 0.182(7) 0.121(5) 0.036(5) 0.009(4) -0.004(4) C10 0.119(5) 0.154(6) 0.090(4) -0.003(4) 0.058(4) -0.010(5) C11 0.189(8) 0.232(9) 0.104(5) -0.042(6) 0.079(6) -0.015(7) C12 0.276(10) 0.123(6) 0.187(8) 0.008(5) 0.182(8) -0.017(6) C13 0.089(4) 0.079(3) 0.075(3) 0.014(3) 0.031(3) 0.011(3) C14 0.167(6) 0.091(4) 0.137(6) 0.027(4) 0.069(5) 0.029(4) C15 0.076(4) 0.156(6) 0.152(6) -0.029(5) 0.025(4) 0.013(4) C16 0.055(2) 0.053(2) 0.062(3) 0.006(2) 0.022(2) 0.010(2) C17 0.066(3) 0.068(3) 0.066(3) -0.001(2) 0.023(2) -0.001(2) C18 0.079(3) 0.082(3) 0.082(3) 0.007(3) 0.044(3) -0.004(3) C19 0.076(3) 0.075(3) 0.061(3) -0.006(2) 0.027(2) 0.010(3) C20 0.060(3) 0.060(3) 0.069(3) -0.002(2) 0.022(2) 0.003(2) C21 0.053(2) 0.057(3) 0.062(3) 0.005(2) 0.017(2) 0.010(2) C22 0.089(4) 0.107(4) 0.079(3) -0.007(3) 0.030(3) -0.034(3) C23 0.130(6) 0.088(5) 0.215(8) -0.033(5) 0.040(6) -0.031(4) C24 0.073(4) 0.143(6) 0.187(7) -0.019(5) 0.016(4) -0.023(4) C25 0.109(4) 0.103(4) 0.071(3) -0.002(3) 0.044(3) 0.014(3) C26 0.130(5) 0.107(4) 0.075(3) 0.006(3) 0.042(3) 0.012(4) C27 0.132(5) 0.161(6) 0.101(4) 0.009(4) 0.071(4) 0.028(5) C28 0.062(3) 0.071(3) 0.073(3) 0.017(3) 0.020(2) 0.000(2) C29 0.079(3) 0.105(4) 0.115(4) 0.011(4) 0.047(3) 0.000(3) C30 0.117(5) 0.070(4) 0.143(5) 0.009(4) 0.049(4) -0.016(3) C31 0.086(3) 0.068(3) 0.078(3) -0.008(3) 0.037(3) -0.005(3) C32 0.149(6) 0.088(4) 0.199(7) 0.009(5) 0.121(6) 0.022(4) C33 0.166(6) 0.140(6) 0.279(8) -0.010(6) 0.160(6) -0.005(5) C34 0.116(4) 0.078(4) 0.146(5) -0.014(4) 0.083(4) -0.019(3) C43 0.119(10) 0.076(10) 0.120(14) 0.005(9) 0.053(9) 0.032(7) C44 0.117(12) 0.088(8) 0.111(13) -0.008(8) 0.054(11) -0.009(8) C45 0.168(14) 0.085(10) 0.105(11) -0.026(8) 0.080(11) -0.005(9) C46 0.14(2) 0.063(10) 0.13(2) -0.011(11) 0.039(13) 0.025(11) C43' 0.21(3) 0.088(18) 0.085(17) -0.006(13) 0.045(17) 0.055(15) C44' 0.123(19) 0.118(17) 0.095(14) 0.038(12) 0.045(13) 0.026(14) C45' 0.31(4) 0.085(16) 0.077(13) -0.012(12) 0.031(19) 0.02(2) C46' 0.079(14) 0.12(2) 0.10(2) -0.035(16) 0.036(14) -0.027(14) _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 O2 2.662(4) . ? K1 O1 2.795(3) 2 ? K1 O1 2.837(3) . ? K1 P2 3.3144(17) . ? K1 P1 3.3146(15) . ? K1 C35' 3.540(8) . ? K1 K1 4.335(2) 2 ? K2 O4 2.658(4) . ? K2 O3 2.668(4) . ? K2 P2 3.2532(17) . ? K2 P1 3.2685(16) 1_545 ? K2 C43' 3.493(14) . ? P1 C1 1.833(4) . ? P1 K2 3.2685(16) 1_565 ? P1 H1 1.3500 . ? P2 C16 1.832(4) . ? P2 H2 1.3500 . ? O1 C34 1.433(4) . ? O1 C31 1.436(4) . ? O1 K1 2.795(3) 2 ? O2 C35' 1.420(6) . ? O2 C38' 1.425(7) . ? O2 C35 1.428(7) . ? O2 C38 1.438(7) . ? O3 C42 1.427(7) . ? O3 C42' 1.430(6) . ? O3 C39 1.432(7) . ? O3 C39' 1.443(6) . ? O4 C46 1.430(7) . ? O4 C46' 1.433(7) . ? O4 C43' 1.437(7) . ? O4 C43 1.439(7) . ? C1 C6 1.419(6) . ? C1 C2 1.433(6) . ? C2 C3 1.376(6) . ? C2 C7 1.533(6) . ? C3 C4 1.383(7) . ? C3 H3 0.9400 . ? C4 C5 1.394(7) . ? C4 C10 1.518(7) . ? C5 C6 1.398(6) . ? C5 H5 0.9400 . ? C6 C13 1.516(6) . ? C7 C9 1.524(8) . ? C7 C8 1.534(8) . ? C7 H7 0.9900 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 C12 1.473(8) . ? C10 C11 1.476(8) . ? C10 H10 0.9900 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 H11C 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C13 C15 1.516(7) . ? C13 C14 1.534(7) . ? C13 H13 0.9900 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 C17 1.415(6) . ? C16 C21 1.431(5) . ? C17 C18 1.399(6) . ? C17 C22 1.531(6) . ? C18 C19 1.404(6) . ? C18 H18 0.9400 . ? C19 C20 1.368(6) . ? C19 C25 1.521(6) . ? C20 C21 1.386(6) . ? C20 H20 0.9400 . ? C21 C28 1.518(6) . ? C22 C23 1.492(8) . ? C22 C24 1.498(7) . ? C22 H22 0.9900 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C25 C27 1.471(7) . ? C25 C26 1.501(7) . ? C25 H25 0.9900 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C28 C30 1.531(6) . ? C28 C29 1.530(6) . ? C28 H28 0.9900 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 H30C 0.9700 . ? C31 C32 1.478(6) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C32 C33 1.438(6) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C33 C34 1.433(6) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C43 C44 1.485(9) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C44 C45 1.437(8) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C45 C46 1.426(9) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C43' C44' 1.487(9) . ? C43' H43C 0.9800 . ? C43' H43D 0.9800 . ? C44' C45' 1.437(9) . ? C44' H44C 0.9800 . ? C44' H44D 0.9800 . ? C45' C46' 1.428(9) . ? C45' H45C 0.9800 . ? C45' H45D 0.9800 . ? C46' H46C 0.9800 . ? C46' H46D 0.9800 . ? C39 C40 1.480(9) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C40 C41 1.436(9) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C41 C42 1.433(9) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C39' C40' 1.470(8) . ? C39' H39C 0.9800 . ? C39' H39D 0.9800 . ? C40' C41' 1.428(8) . ? C40' H40C 0.9800 . ? C40' H40D 0.9800 . ? C41' C42' 1.431(8) . ? C41' H41C 0.9800 . ? C41' H41D 0.9800 . ? C42' H42C 0.9800 . ? C42' H42D 0.9800 . ? C35 C36 1.508(9) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 C37 1.434(9) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 C38 1.417(8) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C35' C36' 1.512(8) . ? C35' H35C 0.9800 . ? C35' H35D 0.9800 . ? C36' C37' 1.436(8) . ? C36' H36C 0.9800 . ? C36' H36D 0.9800 . ? C37' C38' 1.423(8) . ? C37' H37C 0.9800 . ? C37' H37D 0.9800 . ? C38' H38C 0.9800 . ? C38' H38D 0.9800 . ? 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 O2 K1 O1 88.34(15) . 2 ? O2 K1 O1 161.11(15) . . ? O1 K1 O1 72.94(10) 2 . ? O2 K1 P2 95.80(11) . . ? O1 K1 P2 100.36(7) 2 . ? O1 K1 P2 90.17(7) . . ? O2 K1 P1 92.43(11) . . ? O1 K1 P1 136.95(7) 2 . ? O1 K1 P1 99.50(7) . . ? P2 K1 P1 122.31(4) . . ? O2 K1 C35' 20.94(14) . . ? O1 K1 C35' 101.51(19) 2 . ? O1 K1 C35' 160.9(2) . . ? P2 K1 C35' 108.94(19) . . ? P1 K1 C35' 71.68(13) . . ? O2 K1 K1 122.56(14) . 2 ? O1 K1 K1 40.04(6) 2 2 ? O1 K1 K1 39.33(6) . 2 ? P2 K1 K1 113.14(3) . 2 ? P1 K1 K1 109.41(3) . 2 ? C35' K1 K1 126.3(2) . 2 ? O4 K2 O3 108.54(15) . . ? O4 K2 P2 108.15(9) . . ? O3 K2 P2 101.83(10) . . ? O4 K2 P1 96.60(9) . 1_545 ? O3 K2 P1 106.78(10) . 1_545 ? P2 K2 P1 133.47(5) . 1_545 ? O4 K2 C43' 22.1(2) . . ? O3 K2 C43' 115.3(6) . . ? P2 K2 C43' 123.8(4) . . ? P1 K2 C43' 74.5(2) 1_545 . ? C1 P1 K2 92.54(13) . 1_565 ? C1 P1 K1 106.58(13) . . ? K2 P1 K1 157.15(5) 1_565 . ? C1 P1 H1 95.3 . . ? K2 P1 H1 95.3 1_565 . ? K1 P1 H1 95.3 . . ? C16 P2 K2 92.84(13) . . ? C16 P2 K1 102.32(13) . . ? K2 P2 K1 162.31(5) . . ? C16 P2 H2 94.0 . . ? K2 P2 H2 94.0 . . ? K1 P2 H2 94.0 . . ? C34 O1 C31 108.7(3) . . ? C34 O1 K1 118.1(3) . 2 ? C31 O1 K1 109.6(2) . 2 ? C34 O1 K1 110.6(3) . . ? C31 O1 K1 108.7(2) . . ? K1 O1 K1 100.63(9) 2 . ? C35' O2 C38' 113.1(7) . . ? C35' O2 C35 35.7(8) . . ? C38' O2 C35 98.4(11) . . ? C35' O2 C38 106.4(7) . . ? C38' O2 C38 24.1(10) . . ? C35 O2 C38 106.7(7) . . ? C35' O2 K1 117.0(4) . . ? C38' O2 K1 129.5(6) . . ? C35 O2 K1 126.2(7) . . ? C38 O2 K1 127.1(5) . . ? C42 O3 C42' 24.9(12) . . ? C42 O3 C39 110.3(7) . . ? C42' O3 C39 116.7(7) . . ? C42 O3 C39' 92.8(9) . . ? C42' O3 C39' 108.1(6) . . ? C39 O3 C39' 25.7(8) . . ? C42 O3 K2 125.0(6) . . ? C42' O3 K2 121.4(4) . . ? C39 O3 K2 121.5(5) . . ? C39' O3 K2 127.2(5) . . ? C46 O4 C46' 11(2) . . ? C46 O4 C43' 100.6(11) . . ? C46' O4 C43' 107.6(8) . . ? C46 O4 C43 107.1(7) . . ? C46' O4 C43 110.6(13) . . ? C43' O4 C43 21.3(18) . . ? C46 O4 K2 130.1(8) . . ? C46' O4 K2 130.1(11) . . ? C43' O4 K2 113.7(7) . . ? C43 O4 K2 118.1(8) . . ? C6 C1 C2 116.7(4) . . ? C6 C1 P1 119.1(3) . . ? C2 C1 P1 124.2(3) . . ? C3 C2 C1 119.9(4) . . ? C3 C2 C7 118.4(4) . . ? C1 C2 C7 121.6(4) . . ? C2 C3 C4 124.1(5) . . ? C2 C3 H3 117.9 . . ? C4 C3 H3 117.9 . . ? C3 C4 C5 116.0(5) . . ? C3 C4 C10 122.9(5) . . ? C5 C4 C10 121.0(5) . . ? C4 C5 C6 122.8(5) . . ? C4 C5 H5 118.6 . . ? C6 C5 H5 118.6 . . ? C5 C6 C1 120.3(4) . . ? C5 C6 C13 118.2(4) . . ? C1 C6 C13 121.4(4) . . ? C9 C7 C2 110.3(5) . . ? C9 C7 C8 109.0(5) . . ? C2 C7 C8 115.2(5) . . ? C9 C7 H7 107.3 . . ? C2 C7 H7 107.3 . . ? C8 C7 H7 107.3 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 C11 119.9(6) . . ? C12 C10 C4 113.6(6) . . ? C11 C10 C4 112.9(5) . . ? C12 C10 H10 102.5 . . ? C11 C10 H10 102.5 . . ? C4 C10 H10 102.5 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C6 C13 C15 112.6(4) . . ? C6 C13 C14 111.7(5) . . ? C15 C13 C14 110.8(5) . . ? C6 C13 H13 107.2 . . ? C15 C13 H13 107.2 . . ? C14 C13 H13 107.1 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 116.5(4) . . ? C17 C16 P2 122.4(3) . . ? C21 C16 P2 121.1(3) . . ? C18 C17 C16 120.3(4) . . ? C18 C17 C22 117.7(4) . . ? C16 C17 C22 122.0(4) . . ? C17 C18 C19 122.3(4) . . ? C17 C18 H18 118.9 . . ? C19 C18 H18 118.9 . . ? C20 C19 C18 117.1(4) . . ? C20 C19 C25 121.7(5) . . ? C18 C19 C25 121.1(5) . . ? C19 C20 C21 122.9(4) . . ? C19 C20 H20 118.6 . . ? C21 C20 H20 118.6 . . ? C20 C21 C16 120.9(4) . . ? C20 C21 C28 118.1(4) . . ? C16 C21 C28 121.0(4) . . ? C23 C22 C24 111.0(5) . . ? C23 C22 C17 113.2(5) . . ? C24 C22 C17 112.3(5) . . ? C23 C22 H22 106.6 . . ? C24 C22 H22 106.6 . . ? C17 C22 H22 106.6 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C27 C25 C26 115.5(5) . . ? C27 C25 C19 113.5(5) . . ? C26 C25 C19 113.1(4) . . ? C27 C25 H25 104.4 . . ? C26 C25 H25 104.4 . . ? C19 C25 H25 104.4 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C21 C28 C30 114.4(4) . . ? C21 C28 C29 110.2(4) . . ? C30 C28 C29 109.6(4) . . ? C21 C28 H28 107.4 . . ? C30 C28 H28 107.4 . . ? C29 C28 H28 107.4 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O1 C31 C32 105.9(4) . . ? O1 C31 H31A 110.6 . . ? C32 C31 H31A 110.6 . . ? O1 C31 H31B 110.6 . . ? C32 C31 H31B 110.6 . . ? H31A C31 H31B 108.7 . . ? C33 C32 C31 105.4(4) . . ? C33 C32 H32A 110.7 . . ? C31 C32 H32A 110.7 . . ? C33 C32 H32B 110.7 . . ? C31 C32 H32B 110.7 . . ? H32A C32 H32B 108.8 . . ? C34 C33 C32 108.7(5) . . ? C34 C33 H33A 110.0 . . ? C32 C33 H33A 110.0 . . ? C34 C33 H33B 110.0 . . ? C32 C33 H33B 109.9 . . ? H33A C33 H33B 108.3 . . ? O1 C34 C33 107.1(4) . . ? O1 C34 H34A 110.3 . . ? C33 C34 H34A 110.3 . . ? O1 C34 H34B 110.3 . . ? C33 C34 H34B 110.3 . . ? H34A C34 H34B 108.5 . . ? O4 C43 C44 101.7(9) . . ? O4 C43 H43A 111.4 . . ? C44 C43 H43A 111.4 . . ? O4 C43 H43B 111.5 . . ? C44 C43 H43B 111.4 . . ? H43A C43 H43B 109.3 . . ? C45 C44 C43 105.8(7) . . ? C45 C44 H44A 110.6 . . ? C43 C44 H44A 110.6 . . ? C45 C44 H44B 110.6 . . ? C43 C44 H44B 110.6 . . ? H44A C44 H44B 108.7 . . ? C46 C45 C44 108.4(7) . . ? C46 C45 H45A 110.0 . . ? C44 C45 H45A 110.0 . . ? C46 C45 H45B 110.0 . . ? C44 C45 H45B 110.0 . . ? H45A C45 H45B 108.4 . . ? C45 C46 O4 105.1(8) . . ? C45 C46 H46A 110.7 . . ? O4 C46 H46A 110.7 . . ? C45 C46 H46B 110.7 . . ? O4 C46 H46B 110.7 . . ? H46A C46 H46B 108.8 . . ? O4 C43' C44' 104.8(11) . . ? O4 C43' K2 44.2(5) . . ? C44' C43' K2 148.4(8) . . ? O4 C43' H43C 110.8 . . ? C44' C43' H43C 110.8 . . ? K2 C43' H43C 90.3 . . ? O4 C43' H43D 110.8 . . ? C44' C43' H43D 110.8 . . ? K2 C43' H43D 82.3 . . ? H43C C43' H43D 108.9 . . ? C45' C44' C43' 105.6(9) . . ? C45' C44' H44C 110.6 . . ? C43' C44' H44C 110.6 . . ? C45' C44' H44D 110.6 . . ? C43' C44' H44D 110.6 . . ? H44C C44' H44D 108.8 . . ? C46' C45' C44' 107.6(9) . . ? C46' C45' H45C 110.2 . . ? C44' C45' H45C 110.2 . . ? C46' C45' H45D 110.2 . . ? C44' C45' H45D 110.2 . . ? H45C C45' H45D 108.5 . . ? C45' C46' O4 108.3(9) . . ? C45' C46' H46C 110.1 . . ? O4 C46' H46C 110.1 . . ? C45' C46' H46D 110.0 . . ? O4 C46' H46D 110.0 . . ? H46C C46' H46D 108.4 . . ? O3 C39 C40 104.4(7) . . ? O3 C39 H39A 110.9 . . ? C40 C39 H39A 110.9 . . ? O3 C39 H39B 110.8 . . ? C40 C39 H39B 110.9 . . ? H39A C39 H39B 108.9 . . ? C41 C40 C39 106.3(8) . . ? C41 C40 H40A 110.4 . . ? C39 C40 H40A 110.5 . . ? C41 C40 H40B 110.5 . . ? C39 C40 H40B 110.5 . . ? H40A C40 H40B 108.7 . . ? C42 C41 C40 106.9(9) . . ? C42 C41 H41A 110.3 . . ? C40 C41 H41A 110.4 . . ? C42 C41 H41B 110.4 . . ? C40 C41 H41B 110.3 . . ? H41A C41 H41B 108.6 . . ? O3 C42 C41 104.1(9) . . ? O3 C42 H42A 110.9 . . ? C41 C42 H42A 111.0 . . ? O3 C42 H42B 110.9 . . ? C41 C42 H42B 110.9 . . ? H42A C42 H42B 109.0 . . ? O3 C39' C40' 106.0(6) . . ? O3 C39' H39C 110.6 . . ? C40' C39' H39C 110.6 . . ? O3 C39' H39D 110.5 . . ? C40' C39' H39D 110.5 . . ? H39C C39' H39D 108.7 . . ? C41' C40' C39' 107.2(7) . . ? C41' C40' H40C 110.3 . . ? C39' C40' H40C 110.3 . . ? C41' C40' H40D 110.3 . . ? C39' C40' H40D 110.2 . . ? H40C C40' H40D 108.5 . . ? C40' C41' C42' 108.2(7) . . ? C40' C41' H41C 110.0 . . ? C42' C41' H41C 110.0 . . ? C40' C41' H41D 110.0 . . ? C42' C41' H41D 110.1 . . ? H41C C41' H41D 108.4 . . ? O3 C42' C41' 106.5(7) . . ? O3 C42' H42C 110.4 . . ? C41' C42' H42C 110.4 . . ? O3 C42' H42D 110.4 . . ? C41' C42' H42D 110.4 . . ? H42C C42' H42D 108.6 . . ? O2 C35 C36 93.9(11) . . ? O2 C35 H35A 112.9 . . ? C36 C35 H35A 112.9 . . ? O2 C35 H35B 113.0 . . ? C36 C35 H35B 113.0 . . ? H35A C35 H35B 110.4 . . ? C37 C36 C35 103.6(9) . . ? C37 C36 H36A 111.0 . . ? C35 C36 H36A 111.0 . . ? C37 C36 H36B 111.1 . . ? C35 C36 H36B 111.1 . . ? H36A C36 H36B 109.0 . . ? C38 C37 C36 105.2(9) . . ? C38 C37 H37A 110.7 . . ? C36 C37 H37A 110.7 . . ? C38 C37 H37B 110.7 . . ? C36 C37 H37B 110.7 . . ? H37A C37 H37B 108.8 . . ? C37 C38 O2 104.2(7) . . ? C37 C38 H38A 110.9 . . ? O2 C38 H38A 110.9 . . ? C37 C38 H38B 110.9 . . ? O2 C38 H38B 110.9 . . ? H38A C38 H38B 108.9 . . ? O2 C35' C36' 97.3(7) . . ? O2 C35' K1 42.0(3) . . ? C36' C35' K1 135.0(8) . . ? O2 C35' H35C 112.3 . . ? C36' C35' H35C 112.3 . . ? K1 C35' H35C 78.6 . . ? O2 C35' H35D 112.3 . . ? C36' C35' H35D 112.3 . . ? K1 C35' H35D 103.3 . . ? H35C C35' H35D 109.9 . . ? C37' C36' C35' 106.1(8) . . ? C37' C36' H36C 110.5 . . ? C35' C36' H36C 110.5 . . ? C37' C36' H36D 110.5 . . ? C35' C36' H36D 110.5 . . ? H36C C36' H36D 108.7 . . ? C38' C37' C36' 106.7(8) . . ? C38' C37' H37C 110.4 . . ? C36' C37' H37C 110.4 . . ? C38' C37' H37D 110.4 . . ? C36' C37' H37D 110.4 . . ? H37C C37' H37D 108.6 . . ? C37' C38' O2 104.3(7) . . ? C37' C38' H38C 110.9 . . ? O2 C38' H38C 110.9 . . ? C37' C38' H38D 110.8 . . ? O2 C38' H38D 110.9 . . ? H38C C38' H38D 108.9 . . ? _diffrn_measured_fraction_theta_max 0.896 _diffrn_reflns_theta_full 25.24 _diffrn_measured_fraction_theta_full 0.896 _refine_diff_density_max 0.473 _refine_diff_density_min -0.324 _refine_diff_density_rms 0.045 #------------------------------------------------------------------------------# # NEXT STRUCTURE # #------------------------------------------------------------------------------# data_c326 _database_code_CSD 165078 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H64 O2 P2 Rb2' _chemical_formula_weight 785.77 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' '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'p-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.165(3) _cell_length_b 13.643(3) _cell_length_c 13.807(3) _cell_angle_alpha 113.61(3) _cell_angle_beta 103.67(3) _cell_angle_gamma 91.66(3) _cell_volume 2186.6(8) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.61 _cell_measurement_theta_max 27.83 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.193 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 2.338 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.5406 _exptl_absorpt_correction_T_max 0.6521 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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-Diffractometer (AXS Bruker)' _diffrn_measurement_method 'omega-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19667 _diffrn_reflns_av_R_equivalents 0.0474 _diffrn_reflns_av_sigmaI/netI 0.0842 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 27.83 _reflns_number_total 9166 _reflns_number_gt 4945 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (AXS-Bruker)' _computing_cell_refinement 'SAINT (AXS-Bruker)' _computing_data_reduction 'SAINT (AXS-Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (AXS-Bruker)' _computing_publication_material ? _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^)+(0.1087P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9166 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1259 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1865 _refine_ls_wR_factor_gt 0.1389 _refine_ls_goodness_of_fit_ref 0.932 _refine_ls_restrained_S_all 0.932 _refine_ls_shift/su_max 0.153 _refine_ls_shift/su_mean 0.027 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 Rb1 Rb 1.53789(4) 0.93931(4) 0.65949(4) 0.06135(19) Uani 1 1 d . . . Rb2 Rb 1.33456(4) 0.59487(4) 0.43249(4) 0.06092(19) Uani 1 1 d . . . P1 P 1.57636(12) 0.64851(11) 0.61751(12) 0.0605(4) Uani 1 1 d . . . H1 H 1.5306 0.6380 0.6913 0.073 Uiso 1 1 calc R . . P2 P 1.37436(12) 0.85658(12) 0.39667(12) 0.0640(4) Uani 1 1 d . . . H2 H 1.2948 0.9068 0.4321 0.077 Uiso 1 1 calc R . . O1 O 1.2282(5) 0.5868(5) 0.5917(5) 0.1275(19) Uani 1 1 d . . . O2 O 1.3570(4) 1.0168(5) 0.7350(4) 0.1028(15) Uani 1 1 d . . . C1 C 1.2860(8) 0.5333(9) 0.6548(8) 0.137(3) Uani 1 1 d . . . H1A H 1.2948 0.4606 0.6060 0.164 Uiso 1 1 calc R . . H1B H 1.3559 0.5744 0.6978 0.164 Uiso 1 1 calc R . . C5 C 1.2665(8) 0.9592(9) 0.7315(9) 0.155(4) Uani 1 1 d . . . H5A H 1.2795 0.9372 0.7922 0.186 Uiso 1 1 calc R . . H5B H 1.2428 0.8946 0.6620 0.186 Uiso 1 1 calc R . . C6 C 1.1850(8) 1.0367(13) 0.7418(13) 0.232(8) Uani 1 1 d . . . H6A H 1.1156 0.9983 0.6932 0.278 Uiso 1 1 calc R . . H6B H 1.1795 1.0696 0.8174 0.278 Uiso 1 1 calc R . . C7 C 1.2176(9) 1.1139(12) 0.7128(13) 0.227(7) Uani 1 1 d . . . H7A H 1.2116 1.1858 0.7656 0.272 Uiso 1 1 calc R . . H7B H 1.1746 1.1025 0.6398 0.272 Uiso 1 1 calc R . . C3 C 1.1353(12) 0.5728(12) 0.7075(13) 0.226(7) Uani 1 1 d . . . H3A H 1.1288 0.6295 0.7762 0.271 Uiso 1 1 calc R . . H3B H 1.0729 0.5179 0.6761 0.271 Uiso 1 1 calc R . . C4 C 1.1461(10) 0.6177(13) 0.6307(14) 0.250(8) Uani 1 1 d . . . H4A H 1.0817 0.5940 0.5698 0.300 Uiso 1 1 calc R . . H4B H 1.1551 0.6968 0.6678 0.300 Uiso 1 1 calc R . . C2 C 1.2252(12) 0.5277(14) 0.7256(13) 0.251(9) Uani 1 1 d . . . H2A H 1.2069 0.4522 0.7115 0.301 Uiso 1 1 calc R . . H2B H 1.2666 0.5667 0.8023 0.301 Uiso 1 1 calc R . . C8 C 1.3265(8) 1.1041(8) 0.7124(11) 0.173(5) Uani 1 1 d . . . H8A H 1.3350 1.0937 0.6404 0.208 Uiso 1 1 calc R . . H8B H 1.3716 1.1707 0.7678 0.208 Uiso 1 1 calc R . . C9 C 1.6588(4) 0.7716(4) 0.7233(4) 0.0479(11) Uani 1 1 d . . . C10 C 1.6328(4) 0.8284(4) 0.8247(4) 0.0518(12) Uani 1 1 d . . . C11 C 1.6889(5) 0.9286(5) 0.8990(4) 0.0668(15) Uani 1 1 d . . . H11 H 1.6696 0.9642 0.9645 0.080 Uiso 1 1 calc R . . C12 C 1.7707(5) 0.9788(4) 0.8827(5) 0.0681(16) Uani 1 1 d . . . C13 C 1.7995(4) 0.9199(5) 0.7879(5) 0.0651(15) Uani 1 1 d . . . H13 H 1.8578 0.9501 0.7759 0.078 Uiso 1 1 calc R . . C14 C 1.7482(4) 0.8196(4) 0.7095(4) 0.0499(12) Uani 1 1 d . . . C15 C 1.8274(7) 1.0898(5) 0.9621(6) 0.113(3) Uani 1 1 d . . . H15 H 1.8884 1.0903 0.9318 0.135 Uiso 1 1 calc R . . C16 C 1.7797(8) 1.1749(5) 0.9421(6) 0.124(3) Uani 1 1 d . . . H16A H 1.7489 1.1510 0.8638 0.187 Uiso 1 1 calc R . . H16B H 1.8329 1.2373 0.9688 0.187 Uiso 1 1 calc R . . H16C H 1.7250 1.1944 0.9800 0.187 Uiso 1 1 calc R . . C17 C 1.8829(7) 1.0983(7) 1.0685(6) 0.142(4) Uani 1 1 d . . . H17A H 1.9091 1.0308 1.0615 0.213 Uiso 1 1 calc R . . H17B H 1.8353 1.1139 1.1152 0.213 Uiso 1 1 calc R . . H17C H 1.9417 1.1562 1.1009 0.213 Uiso 1 1 calc R . . C18 C 1.5425(5) 0.7778(5) 0.8489(5) 0.0742(16) Uani 1 1 d . . . H18 H 1.4956 0.7275 0.7768 0.089 Uiso 1 1 calc R . . C19 C 1.4775(9) 0.8529(9) 0.9040(14) 0.245(8) Uani 1 1 d . . . H19A H 1.4547 0.8969 0.8646 0.367 Uiso 1 1 calc R . . H19B H 1.5181 0.8990 0.9784 0.367 Uiso 1 1 calc R . . H19C H 1.4163 0.8131 0.9058 0.367 Uiso 1 1 calc R . . C20 C 1.5783(7) 0.7137(10) 0.9076(11) 0.212(6) Uani 1 1 d . . . H20A H 1.6184 0.6608 0.8680 0.318 Uiso 1 1 calc R . . H20B H 1.5180 0.6769 0.9143 0.318 Uiso 1 1 calc R . . H20C H 1.6228 0.7601 0.9802 0.318 Uiso 1 1 calc R . . C21 C 1.7876(4) 0.7642(5) 0.6081(4) 0.0654(14) Uani 1 1 d . . . H21 H 1.7624 0.6860 0.5774 0.078 Uiso 1 1 calc R . . C22 C 1.9101(5) 0.7783(8) 0.6361(6) 0.124(3) Uani 1 1 d . . . H22A H 1.9317 0.7407 0.5696 0.185 Uiso 1 1 calc R . . H22B H 1.9377 0.7485 0.6885 0.185 Uiso 1 1 calc R . . H22C H 1.9373 0.8545 0.6676 0.185 Uiso 1 1 calc R . . C23 C 1.7427(6) 0.8028(6) 0.5200(5) 0.094(2) Uani 1 1 d . . . H23A H 1.7680 0.7645 0.4561 0.141 Uiso 1 1 calc R . . H23B H 1.7653 0.8797 0.5479 0.141 Uiso 1 1 calc R . . H23C H 1.6663 0.7890 0.4995 0.141 Uiso 1 1 calc R . . C24 C 1.1820(4) 0.7106(4) 0.2993(4) 0.0568(13) Uani 1 1 d . . . C25 C 1.1228(4) 0.6100(5) 0.2310(5) 0.0726(16) Uani 1 1 d . . . H25 H 1.0536 0.5973 0.2348 0.087 Uiso 1 1 calc R . . C26 C 1.1614(5) 0.5285(5) 0.1585(5) 0.0784(18) Uani 1 1 d . . . C27 C 1.2605(5) 0.5509(5) 0.1507(5) 0.0734(16) Uani 1 1 d . . . H27 H 1.2869 0.4971 0.0988 0.088 Uiso 1 1 calc R . . C28 C 1.3242(4) 0.6509(4) 0.2168(4) 0.0583(13) Uani 1 1 d . . . C29 C 1.2870(4) 0.7334(4) 0.2970(4) 0.0509(12) Uani 1 1 d . . . C30 C 1.0945(6) 0.4162(6) 0.0950(8) 0.124(3) Uani 1 1 d . . . H30 H 1.0194 0.4258 0.0886 0.148 Uiso 1 1 calc R . . C31 C 1.1095(10) 0.3645(7) -0.0229(8) 0.194(6) Uani 1 1 d . . . H31A H 1.0900 0.4119 -0.0591 0.291 Uiso 1 1 calc R . . H31B H 1.0649 0.2952 -0.0646 0.291 Uiso 1 1 calc R . . H31C H 1.1827 0.3542 -0.0185 0.291 Uiso 1 1 calc R . . C32 C 1.1211(7) 0.3452(7) 0.1518(9) 0.164(5) Uani 1 1 d . . . H32A H 1.0764 0.2760 0.1099 0.246 Uiso 1 1 calc R . . H32B H 1.1099 0.3784 0.2243 0.246 Uiso 1 1 calc R . . H32C H 1.1945 0.3344 0.1585 0.246 Uiso 1 1 calc R . . C33 C 1.1313(4) 0.7959(5) 0.3757(5) 0.0703(15) Uani 1 1 d . . . H33 H 1.1870 0.8367 0.4449 0.084 Uiso 1 1 calc R . . C34 C 1.0942(5) 0.8761(5) 0.3279(5) 0.092(2) Uani 1 1 d . . . H34A H 1.0623 0.9303 0.3775 0.137 Uiso 1 1 calc R . . H34B H 1.0426 0.8381 0.2573 0.137 Uiso 1 1 calc R . . H34C H 1.1541 0.9108 0.3183 0.137 Uiso 1 1 calc R . . C35 C 1.0412(7) 0.7541(7) 0.4058(8) 0.132(3) Uani 1 1 d . . . H35A H 1.0144 0.8145 0.4545 0.198 Uiso 1 1 calc R . . H35B H 1.0662 0.7083 0.4425 0.198 Uiso 1 1 calc R . . H35C H 0.9852 0.7126 0.3397 0.198 Uiso 1 1 calc R . . C36 C 1.4315(5) 0.6689(5) 0.2011(5) 0.0827(18) Uani 1 1 d . . . H36 H 1.4544 0.7477 0.2319 0.099 Uiso 1 1 calc R . . C37 C 1.4295(8) 0.6184(8) 0.0782(7) 0.151(4) Uani 1 1 d . . . H37A H 1.3784 0.6486 0.0388 0.226 Uiso 1 1 calc R . . H37B H 1.4099 0.5408 0.0479 0.226 Uiso 1 1 calc R . . H37C H 1.4990 0.6341 0.0710 0.226 Uiso 1 1 calc R . . C38 C 1.5123(5) 0.6201(7) 0.2568(7) 0.117(3) Uani 1 1 d . . . H38A H 1.5800 0.6343 0.2453 0.175 Uiso 1 1 calc R . . H38B H 1.4912 0.5427 0.2265 0.175 Uiso 1 1 calc R . . H38C H 1.5180 0.6515 0.3349 0.175 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rb1 0.0625(3) 0.0603(3) 0.0703(4) 0.0381(3) 0.0143(3) 0.0146(3) Rb2 0.0626(3) 0.0615(3) 0.0674(4) 0.0382(3) 0.0128(3) 0.0131(3) P1 0.0634(9) 0.0491(8) 0.0613(9) 0.0203(7) 0.0081(7) 0.0060(7) P2 0.0654(9) 0.0572(9) 0.0680(9) 0.0292(8) 0.0108(7) 0.0032(7) O1 0.118(4) 0.178(5) 0.153(5) 0.108(4) 0.080(4) 0.061(4) O2 0.087(3) 0.130(4) 0.116(4) 0.067(3) 0.043(3) 0.026(3) C1 0.138(8) 0.175(9) 0.142(8) 0.099(7) 0.057(7) 0.040(7) C5 0.120(8) 0.187(10) 0.203(11) 0.138(9) 0.026(7) -0.003(7) C6 0.099(7) 0.39(2) 0.38(2) 0.315(19) 0.104(10) 0.095(11) C7 0.149(10) 0.341(18) 0.40(2) 0.298(17) 0.176(12) 0.148(11) C3 0.244(16) 0.283(17) 0.305(18) 0.195(15) 0.210(15) 0.126(14) C4 0.188(12) 0.39(2) 0.41(2) 0.33(2) 0.200(14) 0.186(14) C2 0.253(16) 0.41(2) 0.304(17) 0.268(18) 0.218(15) 0.206(16) C8 0.154(9) 0.150(9) 0.318(15) 0.157(10) 0.136(10) 0.064(7) C9 0.053(3) 0.046(3) 0.050(3) 0.027(2) 0.009(2) 0.014(2) C10 0.061(3) 0.051(3) 0.050(3) 0.027(3) 0.015(2) 0.012(3) C11 0.089(4) 0.063(4) 0.047(3) 0.025(3) 0.011(3) 0.018(3) C12 0.086(4) 0.053(3) 0.053(3) 0.022(3) -0.004(3) 0.003(3) C13 0.060(3) 0.067(4) 0.075(4) 0.044(3) 0.003(3) 0.001(3) C14 0.051(3) 0.051(3) 0.047(3) 0.025(3) 0.006(2) 0.004(2) C15 0.151(7) 0.066(5) 0.087(5) 0.030(4) -0.025(5) -0.011(5) C16 0.196(9) 0.056(4) 0.094(5) 0.018(4) 0.016(6) -0.002(5) C17 0.172(9) 0.116(7) 0.082(5) 0.029(5) -0.035(5) -0.055(6) C18 0.097(5) 0.072(4) 0.064(4) 0.027(3) 0.042(3) 0.011(3) C19 0.190(11) 0.207(12) 0.52(3) 0.239(15) 0.258(15) 0.123(10) C20 0.119(8) 0.336(16) 0.349(16) 0.303(15) 0.076(9) 0.036(9) C21 0.062(3) 0.074(4) 0.067(4) 0.033(3) 0.024(3) 0.011(3) C22 0.065(5) 0.202(9) 0.114(6) 0.069(6) 0.038(4) 0.023(5) C23 0.122(6) 0.109(5) 0.064(4) 0.044(4) 0.035(4) 0.022(4) C24 0.054(3) 0.064(4) 0.062(3) 0.040(3) 0.010(3) 0.013(3) C25 0.049(3) 0.079(4) 0.100(5) 0.054(4) 0.007(3) 0.012(3) C26 0.066(4) 0.064(4) 0.085(4) 0.029(4) -0.014(3) 0.008(3) C27 0.088(5) 0.062(4) 0.063(4) 0.025(3) 0.009(3) 0.025(3) C28 0.066(3) 0.061(4) 0.063(3) 0.037(3) 0.023(3) 0.022(3) C29 0.056(3) 0.053(3) 0.050(3) 0.029(3) 0.012(2) 0.010(2) C30 0.081(5) 0.076(5) 0.149(8) 0.018(5) -0.031(5) -0.003(4) C31 0.241(13) 0.097(7) 0.133(9) 0.006(6) -0.071(8) -0.001(7) C32 0.140(8) 0.093(6) 0.229(11) 0.091(7) -0.037(8) -0.040(6) C33 0.065(4) 0.085(4) 0.074(4) 0.040(3) 0.027(3) 0.019(3) C34 0.096(5) 0.088(5) 0.103(5) 0.048(4) 0.031(4) 0.041(4) C35 0.131(7) 0.158(8) 0.165(8) 0.093(7) 0.097(6) 0.044(6) C36 0.094(5) 0.082(4) 0.094(5) 0.046(4) 0.048(4) 0.026(4) C37 0.177(9) 0.204(10) 0.140(8) 0.104(8) 0.104(7) 0.071(8) C38 0.064(4) 0.150(7) 0.173(8) 0.102(6) 0.035(5) 0.019(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 Rb1 O2 2.883(5) . ? Rb1 C9 3.116(4) . ? Rb1 C10 3.253(5) . ? Rb1 C14 3.328(5) . ? Rb1 P2 3.4141(17) 2_876 ? Rb1 P2 3.459(2) . ? Rb1 C11 3.493(5) . ? Rb1 C13 3.551(5) . ? Rb1 C12 3.645(5) . ? Rb1 C8 3.653(9) . ? Rb1 P1 3.8401(17) . ? Rb1 Rb2 4.752(2) . ? Rb2 O1 2.906(5) . ? Rb2 C29 3.133(4) . ? Rb2 C24 3.266(5) . ? Rb2 C28 3.333(5) . ? Rb2 P1 3.4131(17) 2_866 ? Rb2 P1 3.423(2) . ? Rb2 C25 3.518(5) . ? Rb2 C27 3.571(6) . ? Rb2 C26 3.659(6) . ? Rb2 C1 3.675(9) . ? Rb2 P2 3.8336(17) . ? P1 C9 1.820(5) . ? P1 Rb2 3.4131(17) 2_866 ? P2 C29 1.824(5) . ? P2 Rb1 3.4141(17) 2_876 ? O1 C4 1.325(11) . ? O1 C1 1.449(9) . ? O2 C5 1.388(10) . ? O2 C8 1.394(9) . ? C1 C2 1.423(12) . ? C5 C6 1.519(14) . ? C6 C7 1.358(14) . ? C7 C8 1.445(12) . ? C3 C2 1.366(15) . ? C3 C4 1.451(15) . ? C9 C14 1.418(7) . ? C9 C10 1.432(7) . ? C10 C11 1.389(7) . ? C10 C18 1.525(7) . ? C11 C12 1.368(8) . ? C12 C13 1.383(8) . ? C12 C15 1.507(8) . ? C13 C14 1.384(7) . ? C14 C21 1.523(7) . ? C15 C16 1.428(9) . ? C15 C17 1.434(9) . ? C18 C20 1.433(9) . ? C18 C19 1.447(10) . ? C21 C23 1.515(7) . ? C21 C22 1.554(8) . ? C24 C25 1.391(8) . ? C24 C29 1.419(7) . ? C24 C33 1.519(7) . ? C25 C26 1.370(8) . ? C26 C27 1.369(9) . ? C26 C30 1.541(9) . ? C27 C28 1.404(8) . ? C28 C29 1.423(7) . ? C28 C36 1.506(8) . ? C30 C32 1.474(11) . ? C30 C31 1.557(14) . ? C33 C34 1.527(7) . ? C33 C35 1.513(9) . ? C36 C38 1.494(9) . ? C36 C37 1.548(10) . ? 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 O2 Rb1 C9 122.40(14) . . ? O2 Rb1 C10 100.43(14) . . ? C9 Rb1 C10 25.88(12) . . ? O2 Rb1 C14 143.41(13) . . ? C9 Rb1 C14 25.15(12) . . ? C10 Rb1 C14 43.13(12) . . ? O2 Rb1 P2 101.80(12) . 2_876 ? C9 Rb1 P2 130.50(10) . 2_876 ? C10 Rb1 P2 136.07(10) . 2_876 ? C14 Rb1 P2 105.37(9) . 2_876 ? O2 Rb1 P2 86.36(10) . . ? C9 Rb1 P2 119.13(10) . . ? C10 Rb1 P2 137.14(10) . . ? C14 Rb1 P2 121.25(9) . . ? P2 Rb1 P2 81.79(5) 2_876 . ? O2 Rb1 C11 98.46(14) . . ? C9 Rb1 C11 42.90(13) . . ? C10 Rb1 C11 23.41(12) . . ? C14 Rb1 C11 47.54(13) . . ? P2 Rb1 C11 115.31(11) 2_876 . ? P2 Rb1 C11 160.49(10) . . ? O2 Rb1 C13 135.04(14) . . ? C9 Rb1 C13 42.00(13) . . ? C10 Rb1 C13 47.25(13) . . ? C14 Rb1 C13 22.91(12) . . ? P2 Rb1 C13 91.48(9) 2_876 . ? P2 Rb1 C13 138.36(11) . . ? C11 Rb1 C13 38.52(14) . . ? O2 Rb1 C12 113.09(15) . . ? C9 Rb1 C12 49.50(13) . . ? C10 Rb1 C12 40.85(13) . . ? C14 Rb1 C12 40.78(13) . . ? P2 Rb1 C12 95.37(11) 2_876 . ? P2 Rb1 C12 160.46(11) . . ? C11 Rb1 C12 21.96(13) . . ? C13 Rb1 C12 22.10(13) . . ? O2 Rb1 C8 20.63(17) . . ? C9 Rb1 C8 142.58(19) . . ? C10 Rb1 C8 118.9(2) . . ? C14 Rb1 C8 159.1(2) . . ? P2 Rb1 C8 81.69(15) 2_876 . ? P2 Rb1 C8 78.9(2) . . ? C11 Rb1 C8 111.6(2) . . ? C13 Rb1 C8 141.0(2) . . ? C12 Rb1 C8 120.0(2) . . ? O2 Rb1 P1 115.95(12) . . ? C9 Rb1 P1 27.94(9) . . ? C10 Rb1 P1 46.16(10) . . ? C14 Rb1 P1 46.24(9) . . ? P2 Rb1 P1 141.47(4) 2_876 . ? P2 Rb1 P1 92.71(5) . . ? C11 Rb1 P1 68.14(10) . . ? C13 Rb1 P1 67.68(10) . . ? C12 Rb1 P1 77.44(10) . . ? C8 Rb1 P1 134.84(15) . . ? O2 Rb1 Rb2 89.67(12) . . ? C9 Rb1 Rb2 73.16(9) . . ? C10 Rb1 Rb2 84.68(10) . . ? C14 Rb1 Rb2 89.69(9) . . ? P2 Rb1 Rb2 132.56(3) 2_876 . ? P2 Rb1 Rb2 52.86(4) . . ? C11 Rb1 Rb2 108.03(11) . . ? C13 Rb1 Rb2 112.31(10) . . ? C12 Rb1 Rb2 122.23(9) . . ? C8 Rb1 Rb2 99.99(19) . . ? P1 Rb1 Rb2 45.44(3) . . ? O1 Rb2 C29 126.46(15) . . ? O1 Rb2 C24 104.53(15) . . ? C29 Rb2 C24 25.51(12) . . ? O1 Rb2 C28 147.06(15) . . ? C29 Rb2 C28 25.18(12) . . ? C24 Rb2 C28 42.87(13) . . ? O1 Rb2 P1 95.03(12) . 2_866 ? C29 Rb2 P1 133.74(10) . 2_866 ? C24 Rb2 P1 138.90(10) . 2_866 ? C28 Rb2 P1 108.58(10) . 2_866 ? O1 Rb2 P1 91.28(12) . . ? C29 Rb2 P1 118.70(10) . . ? C24 Rb2 P1 139.62(10) . . ? C28 Rb2 P1 116.75(10) . . ? P1 Rb2 P1 73.95(5) 2_866 . ? O1 Rb2 C25 101.34(16) . . ? C29 Rb2 C25 42.61(13) . . ? C24 Rb2 C25 23.29(13) . . ? C28 Rb2 C25 47.46(14) . . ? P1 Rb2 C25 117.97(11) 2_866 . ? P1 Rb2 C25 161.31(10) . . ? O1 Rb2 C27 136.86(17) . . ? C29 Rb2 C27 42.19(13) . . ? C24 Rb2 C27 47.21(13) . . ? C28 Rb2 C27 23.13(13) . . ? P1 Rb2 C27 94.52(10) 2_866 . ? P1 Rb2 C27 131.73(12) . . ? C25 Rb2 C27 38.56(14) . . ? O1 Rb2 C26 115.07(17) . . ? C29 Rb2 C26 49.00(14) . . ? C24 Rb2 C26 40.46(14) . . ? C28 Rb2 C26 40.42(15) . . ? P1 Rb2 C26 98.50(11) 2_866 . ? P1 Rb2 C26 153.33(13) . . ? C25 Rb2 C26 21.90(13) . . ? C27 Rb2 C26 21.79(14) . . ? O1 Rb2 C1 21.67(17) . . ? C29 Rb2 C1 147.37(18) . . ? C24 Rb2 C1 126.19(18) . . ? C28 Rb2 C1 168.00(18) . . ? P1 Rb2 C1 77.18(16) 2_866 . ? P1 Rb2 C1 74.70(16) . . ? C25 Rb2 C1 120.60(18) . . ? C27 Rb2 C1 149.5(2) . . ? C26 Rb2 C1 129.5(2) . . ? O1 Rb2 P2 120.59(12) . . ? C29 Rb2 P2 28.13(10) . . ? C24 Rb2 P2 46.55(10) . . ? C28 Rb2 P2 45.89(10) . . ? P1 Rb2 P2 142.77(4) 2_866 . ? P1 Rb2 P2 93.38(5) . . ? C25 Rb2 P2 68.37(11) . . ? C27 Rb2 P2 67.70(11) . . ? C26 Rb2 P2 77.13(11) . . ? C1 Rb2 P2 134.00(17) . . ? O1 Rb2 Rb1 96.36(13) . . ? C29 Rb2 Rb1 74.10(10) . . ? C24 Rb2 Rb1 87.93(10) . . ? C28 Rb2 Rb1 88.26(11) . . ? P1 Rb2 Rb1 125.83(3) 2_866 . ? P1 Rb2 Rb1 53.06(4) . . ? C25 Rb2 Rb1 111.21(11) . . ? C27 Rb2 Rb1 111.38(11) . . ? C26 Rb2 Rb1 123.10(10) . . ? C1 Rb2 Rb1 96.84(17) . . ? P2 Rb2 Rb1 45.99(3) . . ? C9 P1 Rb2 119.77(15) . 2_866 ? C9 P1 Rb2 134.14(15) . . ? Rb2 P1 Rb2 106.05(5) 2_866 . ? C9 P1 Rb1 53.32(14) . . ? Rb2 P1 Rb1 166.17(5) 2_866 . ? Rb2 P1 Rb1 81.51(5) . . ? C29 P2 Rb1 125.45(15) . 2_876 ? C29 P2 Rb1 135.17(15) . . ? Rb1 P2 Rb1 98.21(5) 2_876 . ? C29 P2 Rb2 54.06(14) . . ? Rb1 P2 Rb2 165.32(5) 2_876 . ? Rb1 P2 Rb2 81.16(5) . . ? C4 O1 C1 106.9(7) . . ? C4 O1 Rb2 142.5(6) . . ? C1 O1 Rb2 110.6(4) . . ? C5 O2 C8 107.4(7) . . ? C5 O2 Rb1 129.6(6) . . ? C8 O2 Rb1 112.6(5) . . ? C2 C1 O1 106.5(8) . . ? C2 C1 Rb2 154.1(8) . . ? O1 C1 Rb2 47.8(3) . . ? O2 C5 C6 105.0(8) . . ? C7 C6 C5 107.2(9) . . ? C6 C7 C8 106.3(9) . . ? C2 C3 C4 105.4(10) . . ? O1 C4 C3 111.0(9) . . ? C3 C2 C1 109.4(11) . . ? O2 C8 C7 110.1(8) . . ? O2 C8 Rb1 46.8(4) . . ? C7 C8 Rb1 150.8(8) . . ? C14 C9 C10 116.2(4) . . ? C14 C9 P1 123.1(4) . . ? C10 C9 P1 120.7(4) . . ? C14 C9 Rb1 85.8(3) . . ? C10 C9 Rb1 82.4(3) . . ? P1 C9 Rb1 98.74(17) . . ? C11 C10 C9 119.9(5) . . ? C11 C10 C18 120.9(5) . . ? C9 C10 C18 119.2(5) . . ? C11 C10 Rb1 88.1(3) . . ? C9 C10 Rb1 71.7(2) . . ? C18 C10 Rb1 109.7(3) . . ? C12 C11 C10 124.1(5) . . ? C12 C11 Rb1 85.3(3) . . ? C10 C11 Rb1 68.5(3) . . ? C13 C12 C11 115.3(5) . . ? C13 C12 C15 121.5(7) . . ? C11 C12 C15 123.2(6) . . ? C13 C12 Rb1 75.1(3) . . ? C11 C12 Rb1 72.8(3) . . ? C15 C12 Rb1 121.8(4) . . ? C12 C13 C14 124.5(5) . . ? C12 C13 Rb1 82.8(3) . . ? C14 C13 Rb1 69.4(3) . . ? C13 C14 C9 119.8(5) . . ? C13 C14 C21 119.0(5) . . ? C9 C14 C21 121.2(4) . . ? C13 C14 Rb1 87.7(3) . . ? C9 C14 Rb1 69.0(2) . . ? C21 C14 Rb1 112.1(3) . . ? C16 C15 C17 124.4(7) . . ? C16 C15 C12 113.5(6) . . ? C17 C15 C12 114.8(6) . . ? C20 C18 C19 109.9(8) . . ? C20 C18 C10 112.2(6) . . ? C19 C18 C10 115.1(6) . . ? C23 C21 C14 111.9(4) . . ? C23 C21 C22 110.2(5) . . ? C14 C21 C22 112.1(5) . . ? C25 C24 C29 120.8(5) . . ? C25 C24 C33 118.5(5) . . ? C29 C24 C33 120.7(5) . . ? C25 C24 Rb2 88.5(3) . . ? C29 C24 Rb2 72.0(3) . . ? C33 C24 Rb2 110.5(3) . . ? C26 C25 C24 122.6(6) . . ? C26 C25 Rb2 84.8(3) . . ? C24 C25 Rb2 68.2(3) . . ? C27 C26 C25 117.4(6) . . ? C27 C26 C30 123.6(7) . . ? C25 C26 C30 118.9(7) . . ? C27 C26 Rb2 75.5(3) . . ? C25 C26 Rb2 73.2(3) . . ? C30 C26 Rb2 118.5(5) . . ? C26 C27 C28 122.8(6) . . ? C26 C27 Rb2 82.7(4) . . ? C28 C27 Rb2 68.9(3) . . ? C27 C28 C29 119.9(5) . . ? C27 C28 C36 119.1(5) . . ? C29 C28 C36 121.0(5) . . ? C27 C28 Rb2 88.0(3) . . ? C29 C28 Rb2 69.5(3) . . ? C36 C28 Rb2 112.9(3) . . ? C24 C29 C28 116.2(5) . . ? C24 C29 P2 122.8(4) . . ? C28 C29 P2 120.9(4) . . ? C24 C29 Rb2 82.5(3) . . ? C28 C29 Rb2 85.3(3) . . ? P2 C29 Rb2 97.81(18) . . ? C32 C30 C31 111.0(8) . . ? C32 C30 C26 112.1(7) . . ? C31 C30 C26 109.0(8) . . ? C24 C33 C34 110.3(4) . . ? C24 C33 C35 115.9(6) . . ? C34 C33 C35 109.2(6) . . ? C38 C36 C28 112.3(5) . . ? C38 C36 C37 106.6(6) . . ? C28 C36 C37 111.7(6) . . ? _diffrn_measured_fraction_theta_max 0.883 _diffrn_reflns_theta_full 27.83 _diffrn_measured_fraction_theta_full 0.883 _refine_diff_density_max 0.552 _refine_diff_density_min -0.709 _refine_diff_density_rms 0.124 #------------------------------------------------------------------------------# # END OF DATA BLOCK # #------------------------------------------------------------------------------#