# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 # start Validation Reply Form _vrf_PLAT241_FO3583 ; PROBLEM: Check High Ueq as Compared to Neighbors for C31B RESPONSE: In this structure are two symmetry independent molecules in the asymmetric unit. The cation around LiB is very disorderd. The disorder could not solved with better results. The discussion of this structure will be concentrated at molecule A! ; _vrf_PLAT242_FO3583 ; PROBLEM: Check Low Ueq as Compared to Neighbors for Li1B RESPONSE: See above. ; _vrf_PLAT410_FO3583 ; PROBLEM: Short Intra H...H Contact H35C .. H36D .. 1.59 Ang. RESPONSE: See above. ; _vrf_PLAT773_FO3583 ; PROBLEM: Suspect C-C Bond in CIF: C34B -- C35B .. 1.92 Ang. RESPONSE: See above. ; # end Validation Reply Form #Added by publCIF (CCDC output) (Do 4. Dez 14:44:19 2008) _audit_update_record ; 2008-12-04 # Formatted by publCIF ; # 1. SUBMISSION DETAILS _publ_contact_author ; Matthias Westerhausen Institut f\"ur anorganische und analytische Chemie Friedrich-Schiller-Universit\"at Jena August-Bebel-Str. 2 07743 Jena Germany ; _publ_contact_author_phone '03641 948 110' _publ_contact_author_fax '03641 948 102' _publ_contact_author_email m.we@uni-jena.de # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis and Crystal Structures of Bis(diphenylphosphanyl)methanides of Lithium and Calcium as well as of their Borane Adducts ; loop_ _publ_author_name _publ_author_address 'Matthias Westerhausen' ; Institut f\"ur anorganische und analytische Chemie Friedrich-Schiller-Universit\"at Jena August-Bebel-Str. 2 D-07743 Jena Germany ; 'Katja Wimmer ' ; Institut f\"ur anorganische und analytische Chemie Friedrich-Schiller-Universit\"at Jena August-Bebel-Str. 2 D-07743 Jena Germany ; 'Jens Langer ' ; Institut f\"ur anorganische und analytische Chemie Friedrich-Schiller-Universit\"at Jena August-Bebel-Str. 2 D-07743 Jena Germany ; H.Gorls ; Institut f\"ur anorganische und analytische Chemie Friedrich-Schiller-Universit\"at Jena Lessing-Str. 8 D-07743 Jena Germany ; _publ_contact_author_name 'Matthias Westerhausen' # data_FO3481 _database_code_depnum_ccdc_archive 'CCDC 712109' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H45 Li N2 O P2, C4 H7 O' _chemical_formula_sum 'C39 H52 Li N2 O2 P2' _chemical_formula_weight 649.71 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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall -P2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.3975(6) _cell_length_b 9.8321(2) _cell_length_c 18.8821(6) _cell_angle_alpha 90.00 _cell_angle_beta 108.9380(10) _cell_angle_gamma 90.00 _cell_volume 3757.43(18) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 26018 _cell_measurement_theta_min 2.86 _cell_measurement_theta_max 27.49 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.149 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1396 _exptl_absorpt_coefficient_mu 0.150 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26018 _diffrn_reflns_av_R_equivalents 0.0582 _diffrn_reflns_av_sigmaI/netI 0.0595 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 27.49 _reflns_number_total 8610 _reflns_number_gt 6195 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0721P)^2^+2.8288P] 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 8610 _refine_ls_number_parameters 419 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0913 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1564 _refine_ls_wR_factor_gt 0.1390 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.21227(3) 0.08976(5) 0.85078(3) 0.01853(14) Uani 1 1 d . . . P2 P 0.33961(3) 0.20332(5) 0.85978(3) 0.02010(14) Uani 1 1 d . . . Li1 Li 0.2928(2) 0.1293(4) 0.9893(2) 0.0289(9) Uani 1 1 d . . . O1 O 0.28426(9) 0.32255(16) 1.00642(10) 0.0333(4) Uani 1 1 d . . . N1 N 0.24988(11) 0.0422(2) 1.06871(11) 0.0326(5) Uani 1 1 d . . . N2 N 0.37917(11) 0.0160(2) 1.04995(12) 0.0332(5) Uani 1 1 d . . . C1 C 0.25630(11) 0.1905(2) 0.80824(13) 0.0223(4) Uani 1 1 d . . . H1 H 0.2402(12) 0.216(2) 0.7555(15) 0.028(7) Uiso 1 1 d . . . C2 C 0.12883(11) 0.1644(2) 0.82645(12) 0.0224(5) Uani 1 1 d . . . C3 C 0.07758(12) 0.0977(2) 0.84359(14) 0.0295(5) Uani 1 1 d . . . H3A H 0.0844 0.0082 0.8637 0.035 Uiso 1 1 calc R . . C4 C 0.01722(12) 0.1608(3) 0.83156(16) 0.0376(6) Uani 1 1 d . . . H4A H -0.0168 0.1143 0.8438 0.045 Uiso 1 1 calc R . . C5 C 0.00573(13) 0.2909(3) 0.80198(18) 0.0420(7) Uani 1 1 d . . . H5A H -0.0357 0.3338 0.7941 0.050 Uiso 1 1 calc R . . C6 C 0.05538(13) 0.3570(3) 0.78411(18) 0.0427(7) Uani 1 1 d . . . H6A H 0.0479 0.4459 0.7633 0.051 Uiso 1 1 calc R . . C7 C 0.11639(12) 0.2947(2) 0.79620(15) 0.0317(5) Uani 1 1 d . . . H7A H 0.1501 0.3418 0.7836 0.038 Uiso 1 1 calc R . . C8 C 0.18949(10) -0.0733(2) 0.79911(12) 0.0206(4) Uani 1 1 d . . . C9 C 0.18501(13) -0.0850(2) 0.72404(14) 0.0318(5) Uani 1 1 d . . . H9A H 0.1917 -0.0066 0.6979 0.038 Uiso 1 1 calc R . . C10 C 0.17099(14) -0.2085(3) 0.68667(16) 0.0380(6) Uani 1 1 d . . . H10A H 0.1681 -0.2142 0.6355 0.046 Uiso 1 1 calc R . . C11 C 0.16125(12) -0.3234(2) 0.72406(16) 0.0334(6) Uani 1 1 d . . . H11A H 0.1519 -0.4082 0.6987 0.040 Uiso 1 1 calc R . . C12 C 0.16520(12) -0.3145(2) 0.79792(16) 0.0328(6) Uani 1 1 d . . . H12A H 0.1583 -0.3931 0.8237 0.039 Uiso 1 1 calc R . . C13 C 0.17926(12) -0.1904(2) 0.83503(14) 0.0285(5) Uani 1 1 d . . . H13A H 0.1819 -0.1856 0.8862 0.034 Uiso 1 1 calc R . . C14 C 0.38465(10) 0.1261(2) 0.80100(12) 0.0220(4) Uani 1 1 d . . . C15 C 0.43226(11) 0.1883(2) 0.77595(14) 0.0285(5) Uani 1 1 d . . . H15A H 0.4429 0.2813 0.7875 0.034 Uiso 1 1 calc R . . C16 C 0.46443(12) 0.1169(3) 0.73457(14) 0.0335(6) Uani 1 1 d . . . H16A H 0.4970 0.1612 0.7186 0.040 Uiso 1 1 calc R . . C17 C 0.44944(13) -0.0179(3) 0.71634(14) 0.0350(6) Uani 1 1 d . . . H17A H 0.4714 -0.0666 0.6878 0.042 Uiso 1 1 calc R . . C18 C 0.40214(14) -0.0811(2) 0.74006(15) 0.0357(6) Uani 1 1 d . . . H18A H 0.3915 -0.1739 0.7278 0.043 Uiso 1 1 calc R . . C19 C 0.37018(12) -0.0105(2) 0.78151(14) 0.0293(5) Uani 1 1 d . . . H19A H 0.3376 -0.0557 0.7971 0.035 Uiso 1 1 calc R . . C20 C 0.36591(11) 0.3821(2) 0.86054(12) 0.0212(4) Uani 1 1 d . . . C21 C 0.32185(12) 0.4866(2) 0.82838(13) 0.0257(5) Uani 1 1 d . . . H21A H 0.2771 0.4653 0.8018 0.031 Uiso 1 1 calc R . . C22 C 0.34227(13) 0.6213(2) 0.83449(15) 0.0311(5) Uani 1 1 d . . . H22A H 0.3114 0.6909 0.8120 0.037 Uiso 1 1 calc R . . C23 C 0.40680(13) 0.6548(2) 0.87290(14) 0.0302(5) Uani 1 1 d . . . H23A H 0.4208 0.7470 0.8763 0.036 Uiso 1 1 calc R . . C24 C 0.45140(12) 0.5527(2) 0.90665(14) 0.0288(5) Uani 1 1 d . . . H24A H 0.4960 0.5750 0.9338 0.035 Uiso 1 1 calc R . . C25 C 0.43090(11) 0.4181(2) 0.90076(13) 0.0256(5) Uani 1 1 d . . . H25A H 0.4616 0.3491 0.9245 0.031 Uiso 1 1 calc R . . C26 C 0.29392(15) -0.0725(3) 1.10030(16) 0.0414(7) Uani 1 1 d . . . H26A H 0.2828 -0.1493 1.0645 0.050 Uiso 1 1 calc R . . H26B H 0.2867 -0.1028 1.1471 0.050 Uiso 1 1 calc R . . C27 C 0.36582(15) -0.0356(3) 1.11700(16) 0.0455(7) Uani 1 1 d . . . H27A H 0.3782 0.0347 1.1566 0.055 Uiso 1 1 calc R . . H27B H 0.3935 -0.1169 1.1360 0.055 Uiso 1 1 calc R . . C28 C 0.44257(14) 0.0880(3) 1.07170(18) 0.0482(7) Uani 1 1 d . . . H28A H 0.4779 0.0263 1.0999 0.072 Uiso 1 1 calc R . . H28B H 0.4407 0.1664 1.1030 0.072 Uiso 1 1 calc R . . H28C H 0.4515 0.1194 1.0267 0.072 Uiso 1 1 calc R . . C29 C 0.38188(16) -0.0953(3) 0.99958(17) 0.0449(7) Uani 1 1 d . . . H29A H 0.4198 -0.1540 1.0242 0.067 Uiso 1 1 calc R . . H29B H 0.3866 -0.0578 0.9535 0.067 Uiso 1 1 calc R . . H29C H 0.3411 -0.1487 0.9873 0.067 Uiso 1 1 calc R . . C30 C 0.25143(18) 0.1427(3) 1.12704(16) 0.0488(8) Uani 1 1 d . . . H30A H 0.2325 0.1024 1.1630 0.073 Uiso 1 1 calc R . . H30B H 0.2256 0.2228 1.1039 0.073 Uiso 1 1 calc R . . H30C H 0.2972 0.1698 1.1531 0.073 Uiso 1 1 calc R . . C31 C 0.18210(14) -0.0054(3) 1.03536(17) 0.0457(7) Uani 1 1 d . . . H31A H 0.1664 -0.0435 1.0745 0.069 Uiso 1 1 calc R . . H31B H 0.1806 -0.0757 0.9980 0.069 Uiso 1 1 calc R . . H31C H 0.1538 0.0710 1.0112 0.069 Uiso 1 1 calc R . . C32 C 0.22654(15) 0.4026(3) 0.97152(18) 0.0474(7) Uani 1 1 d . . . H32A H 0.1868 0.3593 0.9776 0.057 Uiso 1 1 calc R . . H32B H 0.2196 0.4141 0.9174 0.057 Uiso 1 1 calc R . . C33 C 0.2401(2) 0.5371(4) 1.0112(3) 0.0922(16) Uani 1 1 d . . . H33A H 0.2180 0.6120 0.9773 0.111 Uiso 1 1 calc R . . H33B H 0.2248 0.5372 1.0554 0.111 Uiso 1 1 calc R . . C34 C 0.3116(2) 0.5505(3) 1.0337(2) 0.0862(15) Uani 1 1 d . . . H34A H 0.3284 0.6067 1.0794 0.103 Uiso 1 1 calc R . . H34B H 0.3251 0.5930 0.9933 0.103 Uiso 1 1 calc R . . C35 C 0.33694(15) 0.4104(3) 1.04796(19) 0.0487(7) Uani 1 1 d . . . H35A H 0.3759 0.3987 1.0312 0.058 Uiso 1 1 calc R . . H35B H 0.3501 0.3895 1.1021 0.058 Uiso 1 1 calc R . . O1T O -0.0241(3) -0.3815(6) 0.8965(3) 0.172(2) Uani 1 1 d . . . C1T C -0.0411(4) -0.2553(9) 0.9391(5) 0.158(3) Uani 1 1 d . . . H1TA H -0.0679 -0.1868 0.9038 0.190 Uiso 1 1 calc R . . H1TB H -0.0646 -0.2836 0.9740 0.190 Uiso 1 1 calc R . . C2T C 0.0256(4) -0.2042(7) 0.9794(4) 0.137(2) Uani 1 1 d . . . H2TA H 0.0285 -0.1079 0.9655 0.164 Uiso 1 1 calc R . . H2TB H 0.0327 -0.2073 1.0339 0.164 Uiso 1 1 calc R . . C3T C 0.0724(2) -0.2721(6) 0.9658(3) 0.107(2) Uani 1 1 d . . . H3TA H 0.1184 -0.2585 0.9899 0.128 Uiso 1 1 calc R . . C4T C 0.0469(3) -0.3599(7) 0.9150(4) 0.126(2) Uani 1 1 d . . . H4TA H 0.0696 -0.4479 0.9310 0.151 Uiso 1 1 calc R . . H4TB H 0.0559 -0.3316 0.8689 0.151 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 P1 0.0191(3) 0.0171(3) 0.0195(3) -0.0001(2) 0.0064(2) -0.0018(2) P2 0.0212(3) 0.0167(3) 0.0228(3) 0.0009(2) 0.0078(2) -0.0018(2) Li1 0.036(2) 0.0243(19) 0.023(2) -0.0003(16) 0.0045(17) 0.0023(16) O1 0.0365(10) 0.0237(8) 0.0337(10) -0.0052(7) 0.0033(8) 0.0000(7) N1 0.0449(13) 0.0306(11) 0.0229(10) 0.0002(8) 0.0118(9) 0.0004(9) N2 0.0386(12) 0.0288(11) 0.0289(11) 0.0026(9) 0.0066(9) 0.0016(9) C1 0.0231(11) 0.0224(11) 0.0213(11) 0.0034(9) 0.0072(9) -0.0039(8) C2 0.0201(11) 0.0228(11) 0.0226(11) -0.0064(9) 0.0048(9) -0.0013(8) C3 0.0275(12) 0.0285(12) 0.0332(13) -0.0026(10) 0.0107(10) -0.0020(9) C4 0.0242(13) 0.0423(15) 0.0483(17) -0.0090(12) 0.0148(12) -0.0040(11) C5 0.0233(13) 0.0380(15) 0.0597(19) -0.0112(13) 0.0066(12) 0.0060(11) C6 0.0325(14) 0.0294(13) 0.0584(19) 0.0009(13) 0.0038(13) 0.0077(11) C7 0.0254(12) 0.0237(11) 0.0426(15) 0.0015(10) 0.0063(11) -0.0003(9) C8 0.0166(10) 0.0184(10) 0.0263(12) -0.0008(9) 0.0061(9) 0.0009(8) C9 0.0409(14) 0.0285(12) 0.0294(13) -0.0036(10) 0.0160(11) -0.0071(10) C10 0.0454(16) 0.0371(14) 0.0347(15) -0.0129(12) 0.0173(12) -0.0060(12) C11 0.0264(12) 0.0251(12) 0.0487(16) -0.0129(11) 0.0123(12) -0.0019(9) C12 0.0338(13) 0.0189(11) 0.0469(16) -0.0016(10) 0.0145(12) -0.0016(9) C13 0.0355(13) 0.0223(11) 0.0290(13) 0.0002(10) 0.0123(11) 0.0001(9) C14 0.0191(11) 0.0220(10) 0.0234(11) 0.0024(9) 0.0050(9) 0.0025(8) C15 0.0241(12) 0.0295(12) 0.0311(13) 0.0004(10) 0.0080(10) -0.0029(9) C16 0.0260(12) 0.0452(15) 0.0311(14) 0.0058(11) 0.0117(11) 0.0038(11) C17 0.0349(14) 0.0416(15) 0.0300(13) 0.0051(11) 0.0128(11) 0.0181(11) C18 0.0493(16) 0.0239(12) 0.0353(14) 0.0005(10) 0.0159(12) 0.0096(11) C19 0.0338(13) 0.0217(11) 0.0352(14) 0.0029(10) 0.0152(11) 0.0017(9) C20 0.0263(11) 0.0185(10) 0.0209(11) -0.0017(8) 0.0105(9) -0.0029(8) C21 0.0244(12) 0.0244(11) 0.0278(12) 0.0000(9) 0.0077(10) -0.0031(9) C22 0.0350(14) 0.0215(11) 0.0363(14) 0.0023(10) 0.0108(11) 0.0019(10) C23 0.0397(14) 0.0197(11) 0.0333(14) -0.0050(10) 0.0146(11) -0.0095(10) C24 0.0266(12) 0.0307(12) 0.0276(13) -0.0054(10) 0.0070(10) -0.0103(10) C25 0.0240(11) 0.0235(11) 0.0276(12) 0.0005(9) 0.0058(10) -0.0016(9) C26 0.0551(18) 0.0331(14) 0.0366(15) 0.0125(12) 0.0156(13) 0.0011(12) C27 0.0509(18) 0.0469(16) 0.0324(15) 0.0143(13) 0.0045(13) 0.0077(13) C28 0.0373(16) 0.0531(18) 0.0475(18) 0.0039(14) 0.0046(13) -0.0024(13) C29 0.0604(19) 0.0298(14) 0.0440(17) 0.0019(12) 0.0161(14) 0.0117(12) C30 0.077(2) 0.0446(16) 0.0310(15) -0.0071(13) 0.0265(15) -0.0024(15) C31 0.0448(17) 0.0576(18) 0.0373(16) 0.0020(13) 0.0170(13) -0.0085(14) C32 0.0464(17) 0.0363(15) 0.0495(18) -0.0017(13) 0.0017(14) 0.0100(12) C33 0.104(4) 0.051(2) 0.089(3) -0.026(2) -0.013(3) 0.040(2) C34 0.123(4) 0.0297(17) 0.073(3) -0.0056(17) -0.013(3) -0.011(2) C35 0.0456(17) 0.0361(15) 0.0552(19) -0.0131(14) 0.0038(14) -0.0090(12) O1T 0.152(5) 0.173(5) 0.181(5) -0.030(4) 0.039(4) -0.003(4) C1T 0.116(5) 0.207(8) 0.164(7) -0.019(6) 0.064(5) 0.067(6) C2T 0.143(6) 0.119(5) 0.150(6) -0.064(4) 0.050(5) -0.037(4) C3T 0.061(3) 0.131(4) 0.126(4) -0.090(4) 0.027(3) -0.020(3) C4T 0.083(4) 0.166(6) 0.146(6) -0.039(5) 0.061(4) -0.013(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 P1 C1 1.733(2) . ? P1 C2 1.845(2) . ? P1 C8 1.858(2) . ? P1 Li1 2.653(4) . ? P2 C1 1.736(2) . ? P2 C20 1.844(2) . ? P2 C14 1.852(2) . ? P2 Li1 3.018(4) . ? Li1 O1 1.946(4) . ? Li1 N2 2.143(4) . ? Li1 N1 2.172(5) . ? O1 C32 1.432(3) . ? O1 C35 1.435(3) . ? N1 C31 1.458(4) . ? N1 C26 1.467(3) . ? N1 C30 1.472(3) . ? N2 C29 1.463(3) . ? N2 C28 1.466(3) . ? N2 C27 1.475(3) . ? C1 H1 0.97(3) . ? C2 C7 1.393(3) . ? C2 C3 1.403(3) . ? C3 C4 1.384(3) . ? C3 H3A 0.9500 . ? C4 C5 1.385(4) . ? C4 H4A 0.9500 . ? C5 C6 1.378(4) . ? C5 H5A 0.9500 . ? C6 C7 1.392(3) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 C13 1.389(3) . ? C8 C9 1.394(3) . ? C9 C10 1.388(3) . ? C9 H9A 0.9500 . ? C10 C11 1.383(4) . ? C10 H10A 0.9500 . ? C11 C12 1.372(4) . ? C11 H11A 0.9500 . ? C12 C13 1.390(3) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 C15 1.396(3) . ? C14 C19 1.401(3) . ? C15 C16 1.388(3) . ? C15 H15A 0.9500 . ? C16 C17 1.381(4) . ? C16 H16A 0.9500 . ? C17 C18 1.380(4) . ? C17 H17A 0.9500 . ? C18 C19 1.382(3) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 C25 1.396(3) . ? C20 C21 1.394(3) . ? C21 C22 1.387(3) . ? C21 H21A 0.9500 . ? C22 C23 1.375(4) . ? C22 H22A 0.9500 . ? C23 C24 1.389(4) . ? C23 H23A 0.9500 . ? C24 C25 1.387(3) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? C26 C27 1.511(4) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.501(5) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.456(6) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.473(5) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? O1T C4T 1.461(7) . ? O1T C1T 1.584(8) . ? C1T C2T 1.472(9) . ? C1T H1TA 0.9900 . ? C1T H1TB 0.9900 . ? C2T C3T 1.295(8) . ? C2T H2TA 0.9900 . ? C2T H2TB 0.9900 . ? C3T C4T 1.275(7) . ? C3T H3TA 0.9500 . ? C4T H4TA 0.9900 . ? C4T H4TB 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 P1 C2 106.56(11) . . ? C1 P1 C8 109.82(10) . . ? C2 P1 C8 98.31(9) . . ? C1 P1 Li1 95.53(12) . . ? C2 P1 Li1 116.98(11) . . ? C8 P1 Li1 128.32(11) . . ? C1 P2 C20 109.20(10) . . ? C1 P2 C14 105.88(10) . . ? C20 P2 C14 100.28(10) . . ? C1 P2 Li1 83.47(11) . . ? C20 P2 Li1 113.84(10) . . ? C14 P2 Li1 139.55(10) . . ? O1 Li1 N2 122.0(2) . . ? O1 Li1 N1 100.78(19) . . ? N2 Li1 N1 84.88(16) . . ? O1 Li1 P1 103.93(17) . . ? N2 Li1 P1 128.46(18) . . ? N1 Li1 P1 109.75(17) . . ? O1 Li1 P2 88.44(15) . . ? N2 Li1 P2 95.91(15) . . ? N1 Li1 P2 168.65(19) . . ? P1 Li1 P2 61.07(8) . . ? C32 O1 C35 109.1(2) . . ? C32 O1 Li1 125.0(2) . . ? C35 O1 Li1 125.4(2) . . ? C31 N1 C26 110.3(2) . . ? C31 N1 C30 108.4(2) . . ? C26 N1 C30 110.9(2) . . ? C31 N1 Li1 114.38(19) . . ? C26 N1 Li1 102.96(19) . . ? C30 N1 Li1 109.9(2) . . ? C29 N2 C28 108.4(2) . . ? C29 N2 C27 111.1(2) . . ? C28 N2 C27 110.2(2) . . ? C29 N2 Li1 104.5(2) . . ? C28 N2 Li1 117.2(2) . . ? C27 N2 Li1 105.28(19) . . ? P1 C1 P2 113.29(13) . . ? P1 C1 H1 123.6(15) . . ? P2 C1 H1 120.9(15) . . ? C7 C2 C3 117.7(2) . . ? C7 C2 P1 120.56(17) . . ? C3 C2 P1 121.50(17) . . ? C4 C3 C2 120.7(2) . . ? C4 C3 H3A 119.7 . . ? C2 C3 H3A 119.7 . . ? C3 C4 C5 121.0(2) . . ? C3 C4 H4A 119.5 . . ? C5 C4 H4A 119.5 . . ? C6 C5 C4 119.0(2) . . ? C6 C5 H5A 120.5 . . ? C4 C5 H5A 120.5 . . ? C5 C6 C7 120.6(3) . . ? C5 C6 H6A 119.7 . . ? C7 C6 H6A 119.7 . . ? C6 C7 C2 121.1(2) . . ? C6 C7 H7A 119.5 . . ? C2 C7 H7A 119.5 . . ? C13 C8 C9 117.3(2) . . ? C13 C8 P1 121.00(17) . . ? C9 C8 P1 121.64(17) . . ? C10 C9 C8 121.4(2) . . ? C10 C9 H9A 119.3 . . ? C8 C9 H9A 119.3 . . ? C11 C10 C9 119.9(2) . . ? C11 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C12 C11 C10 119.8(2) . . ? C12 C11 H11A 120.1 . . ? C10 C11 H11A 120.1 . . ? C11 C12 C13 120.0(2) . . ? C11 C12 H12A 120.0 . . ? C13 C12 H12A 120.0 . . ? C8 C13 C12 121.6(2) . . ? C8 C13 H13A 119.2 . . ? C12 C13 H13A 119.2 . . ? C15 C14 C19 117.0(2) . . ? C15 C14 P2 127.06(17) . . ? C19 C14 P2 115.89(16) . . ? C16 C15 C14 121.3(2) . . ? C16 C15 H15A 119.4 . . ? C14 C15 H15A 119.4 . . ? C17 C16 C15 120.5(2) . . ? C17 C16 H16A 119.7 . . ? C15 C16 H16A 119.7 . . ? C18 C17 C16 119.1(2) . . ? C18 C17 H17A 120.4 . . ? C16 C17 H17A 120.4 . . ? C17 C18 C19 120.5(2) . . ? C17 C18 H18A 119.8 . . ? C19 C18 H18A 119.8 . . ? C18 C19 C14 121.5(2) . . ? C18 C19 H19A 119.2 . . ? C14 C19 H19A 119.2 . . ? C25 C20 C21 117.6(2) . . ? C25 C20 P2 119.54(17) . . ? C21 C20 P2 122.55(17) . . ? C22 C21 C20 121.2(2) . . ? C22 C21 H21A 119.4 . . ? C20 C21 H21A 119.4 . . ? C23 C22 C21 120.5(2) . . ? C23 C22 H22A 119.8 . . ? C21 C22 H22A 119.8 . . ? C22 C23 C24 119.5(2) . . ? C22 C23 H23A 120.3 . . ? C24 C23 H23A 120.3 . . ? C25 C24 C23 120.0(2) . . ? C25 C24 H24A 120.0 . . ? C23 C24 H24A 120.0 . . ? C24 C25 C20 121.2(2) . . ? C24 C25 H25A 119.4 . . ? C20 C25 H25A 119.4 . . ? N1 C26 C27 112.1(2) . . ? N1 C26 H26A 109.2 . . ? C27 C26 H26A 109.2 . . ? N1 C26 H26B 109.2 . . ? C27 C26 H26B 109.2 . . ? H26A C26 H26B 107.9 . . ? N2 C27 C26 111.8(2) . . ? N2 C27 H27A 109.3 . . ? C26 C27 H27A 109.3 . . ? N2 C27 H27B 109.3 . . ? C26 C27 H27B 109.3 . . ? H27A C27 H27B 107.9 . . ? N2 C28 H28A 109.5 . . ? N2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N2 C29 H29A 109.5 . . ? N2 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N2 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N1 C30 H30A 109.5 . . ? N1 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N1 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N1 C31 H31A 109.5 . . ? N1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O1 C32 C33 104.9(3) . . ? O1 C32 H32A 110.8 . . ? C33 C32 H32A 110.8 . . ? O1 C32 H32B 110.8 . . ? C33 C32 H32B 110.8 . . ? H32A C32 H32B 108.9 . . ? C34 C33 C32 103.9(3) . . ? C34 C33 H33A 111.0 . . ? C32 C33 H33A 111.0 . . ? C34 C33 H33B 111.0 . . ? C32 C33 H33B 111.0 . . ? H33A C33 H33B 109.0 . . ? C33 C34 C35 105.0(3) . . ? C33 C34 H34A 110.8 . . ? C35 C34 H34A 110.8 . . ? C33 C34 H34B 110.8 . . ? C35 C34 H34B 110.8 . . ? H34A C34 H34B 108.8 . . ? O1 C35 C34 106.6(3) . . ? O1 C35 H35A 110.4 . . ? C34 C35 H35A 110.4 . . ? O1 C35 H35B 110.4 . . ? C34 C35 H35B 110.4 . . ? H35A C35 H35B 108.6 . . ? C4T O1T C1T 99.0(5) . . ? C2T C1T O1T 100.8(5) . . ? C2T C1T H1TA 111.6 . . ? O1T C1T H1TA 111.6 . . ? C2T C1T H1TB 111.6 . . ? O1T C1T H1TB 111.6 . . ? H1TA C1T H1TB 109.4 . . ? C3T C2T C1T 113.8(5) . . ? C3T C2T H2TA 108.8 . . ? C1T C2T H2TA 108.8 . . ? C3T C2T H2TB 108.8 . . ? C1T C2T H2TB 108.8 . . ? H2TA C2T H2TB 107.7 . . ? C4T C3T C2T 109.2(5) . . ? C4T C3T H3TA 125.4 . . ? C2T C3T H3TA 125.4 . . ? C3T C4T O1T 115.9(5) . . ? C3T C4T H4TA 108.3 . . ? O1T C4T H4TA 108.3 . . ? C3T C4T H4TB 108.3 . . ? O1T C4T H4TB 108.3 . . ? H4TA C4T H4TB 107.4 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.689 _refine_diff_density_min -0.485 _refine_diff_density_rms 0.059 #=== END data_FO3499 _database_code_depnum_ccdc_archive 'CCDC 712110' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H66 Ca O3 P4' _chemical_formula_sum 'C62 H66 Ca O3 P4' _chemical_formula_weight 1023.11 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' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall -P2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.2090(4) _cell_length_b 16.6792(5) _cell_length_c 27.0731(6) _cell_angle_alpha 90.00 _cell_angle_beta 95.218(2) _cell_angle_gamma 90.00 _cell_volume 5490.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 34850 _cell_measurement_theta_min 1.94 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.238 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2168 _exptl_absorpt_coefficient_mu 0.276 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34850 _diffrn_reflns_av_R_equivalents 0.0900 _diffrn_reflns_av_sigmaI/netI 0.1151 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 27.48 _reflns_number_total 12534 _reflns_number_gt 6779 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0644P)^2^+0.6259P] 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 12534 _refine_ls_number_parameters 639 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1397 _refine_ls_R_factor_gt 0.0588 _refine_ls_wR_factor_ref 0.1498 _refine_ls_wR_factor_gt 0.1223 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ca1 Ca 0.75686(5) 0.23891(3) 0.62717(2) 0.02963(16) Uani 1 1 d . . . P1 P 0.52158(7) 0.20759(5) 0.57323(3) 0.0340(2) Uani 1 1 d . . . P2 P 0.71207(7) 0.14144(5) 0.53147(3) 0.0344(2) Uani 1 1 d . . . P3 P 0.66099(7) 0.37252(5) 0.68755(3) 0.0337(2) Uani 1 1 d . . . P4 P 0.89734(7) 0.35289(5) 0.69816(3) 0.0328(2) Uani 1 1 d . . . O1 O 0.72716(18) 0.14332(12) 0.69056(7) 0.0419(5) Uani 1 1 d . . . O2 O 0.92998(17) 0.16669(13) 0.63001(8) 0.0439(5) Uani 1 1 d . . . O3 O 0.80146(18) 0.33777(13) 0.56937(7) 0.0444(6) Uani 1 1 d . . . C1 C 0.5718(3) 0.1579(2) 0.52393(11) 0.0370(7) Uani 1 1 d . . . H1 H 0.527(3) 0.1303(19) 0.4999(12) 0.047(9) Uiso 1 1 d . . . C2 C 0.4423(3) 0.13895(19) 0.60956(11) 0.0378(7) Uani 1 1 d . . . C3 C 0.4301(3) 0.1573(2) 0.65890(11) 0.0470(9) Uani 1 1 d . . . H3A H 0.4568 0.2071 0.6719 0.056 Uiso 1 1 calc R . . C4 C 0.3805(3) 0.1054(3) 0.68924(14) 0.0648(11) Uani 1 1 d . . . H4A H 0.3733 0.1191 0.7229 0.078 Uiso 1 1 calc R . . C5 C 0.3413(4) 0.0335(3) 0.67042(16) 0.0741(13) Uani 1 1 d . . . H5A H 0.3074 -0.0031 0.6912 0.089 Uiso 1 1 calc R . . C6 C 0.3508(3) 0.0136(2) 0.62106(15) 0.0608(10) Uani 1 1 d . . . H6A H 0.3227 -0.0359 0.6081 0.073 Uiso 1 1 calc R . . C7 C 0.4011(3) 0.06629(19) 0.59120(12) 0.0432(8) Uani 1 1 d . . . H7A H 0.4078 0.0527 0.5575 0.052 Uiso 1 1 calc R . . C8 C 0.4075(3) 0.27105(18) 0.54586(11) 0.0361(7) Uani 1 1 d . . . C9 C 0.3129(3) 0.28702(19) 0.56950(12) 0.0429(8) Uani 1 1 d . . . H9A H 0.3061 0.2651 0.6015 0.051 Uiso 1 1 calc R . . C10 C 0.2289(3) 0.3340(2) 0.54749(13) 0.0515(9) Uani 1 1 d . . . H10A H 0.1652 0.3438 0.5643 0.062 Uiso 1 1 calc R . . C11 C 0.2370(3) 0.3669(2) 0.50122(14) 0.0554(10) Uani 1 1 d . . . H11A H 0.1784 0.3980 0.4857 0.066 Uiso 1 1 calc R . . C12 C 0.3314(3) 0.3541(2) 0.47767(14) 0.0573(10) Uani 1 1 d . . . H12A H 0.3388 0.3778 0.4462 0.069 Uiso 1 1 calc R . . C13 C 0.4150(3) 0.3070(2) 0.49979(12) 0.0471(9) Uani 1 1 d . . . H13A H 0.4793 0.2988 0.4832 0.057 Uiso 1 1 calc R . . C14 C 0.7346(3) 0.03124(19) 0.52978(10) 0.0364(7) Uani 1 1 d . . . C15 C 0.6699(3) -0.0154(2) 0.55779(11) 0.0419(8) Uani 1 1 d . . . H15A H 0.6156 0.0097 0.5756 0.050 Uiso 1 1 calc R . . C16 C 0.6824(3) -0.0981(2) 0.56053(12) 0.0507(9) Uani 1 1 d . . . H16A H 0.6375 -0.1287 0.5803 0.061 Uiso 1 1 calc R . . C17 C 0.7593(3) -0.1359(2) 0.53484(14) 0.0544(9) Uani 1 1 d . . . H17A H 0.7678 -0.1924 0.5366 0.065 Uiso 1 1 calc R . . C18 C 0.8233(3) -0.0910(2) 0.50675(16) 0.0662(11) Uani 1 1 d . . . H18A H 0.8762 -0.1170 0.4886 0.079 Uiso 1 1 calc R . . C19 C 0.8127(3) -0.0075(2) 0.50403(13) 0.0535(9) Uani 1 1 d . . . H19A H 0.8589 0.0227 0.4846 0.064 Uiso 1 1 calc R . . C20 C 0.7730(3) 0.17381(18) 0.47444(10) 0.0343(7) Uani 1 1 d . . . C21 C 0.7077(3) 0.20509(19) 0.43481(11) 0.0400(8) Uani 1 1 d . . . H21A H 0.6302 0.2071 0.4360 0.048 Uiso 1 1 calc R . . C22 C 0.7537(3) 0.2337(2) 0.39318(12) 0.0460(8) Uani 1 1 d . . . H22A H 0.7075 0.2554 0.3663 0.055 Uiso 1 1 calc R . . C23 C 0.8653(3) 0.2311(2) 0.39051(13) 0.0512(9) Uani 1 1 d . . . H23A H 0.8964 0.2497 0.3617 0.061 Uiso 1 1 calc R . . C24 C 0.9324(3) 0.2008(2) 0.43034(13) 0.0582(10) Uani 1 1 d . . . H24A H 1.0099 0.1991 0.4291 0.070 Uiso 1 1 calc R . . C25 C 0.8857(3) 0.1732(2) 0.47184(12) 0.0465(8) Uani 1 1 d . . . H25A H 0.9321 0.1534 0.4992 0.056 Uiso 1 1 calc R . . C26 C 0.7839(3) 0.3994(2) 0.71972(11) 0.0368(7) Uani 1 1 d . . . H26 H 0.796(2) 0.445(2) 0.7394(11) 0.043(9) Uiso 1 1 d . . . C27 C 0.5583(2) 0.35502(17) 0.73289(11) 0.0335(7) Uani 1 1 d . . . C28 C 0.5916(3) 0.3463(2) 0.78292(12) 0.0441(8) Uani 1 1 d . . . H28A H 0.6676 0.3491 0.7939 0.053 Uiso 1 1 calc R . . C29 C 0.5153(3) 0.3335(2) 0.81737(13) 0.0544(10) Uani 1 1 d . . . H29A H 0.5394 0.3302 0.8517 0.065 Uiso 1 1 calc R . . C30 C 0.4057(3) 0.3257(2) 0.80197(14) 0.0531(9) Uani 1 1 d . . . H30A H 0.3541 0.3161 0.8255 0.064 Uiso 1 1 calc R . . C31 C 0.3708(3) 0.3318(2) 0.75265(14) 0.0513(9) Uani 1 1 d . . . H31A H 0.2952 0.3253 0.7418 0.062 Uiso 1 1 calc R . . C32 C 0.4471(3) 0.34783(19) 0.71823(12) 0.0437(8) Uani 1 1 d . . . H32A H 0.4220 0.3539 0.6842 0.052 Uiso 1 1 calc R . . C33 C 0.5936(3) 0.46138(19) 0.65770(11) 0.0395(8) Uani 1 1 d . . . C34 C 0.6184(3) 0.5382(2) 0.67402(13) 0.0538(10) Uani 1 1 d . . . H34A H 0.6739 0.5463 0.7005 0.065 Uiso 1 1 calc R . . C35 C 0.5630(4) 0.6043(2) 0.65202(18) 0.0769(14) Uani 1 1 d . . . H35A H 0.5808 0.6570 0.6635 0.092 Uiso 1 1 calc R . . C36 C 0.4824(4) 0.5925(3) 0.61359(19) 0.0832(16) Uani 1 1 d . . . H36A H 0.4427 0.6371 0.5993 0.100 Uiso 1 1 calc R . . C37 C 0.4595(4) 0.5168(3) 0.59605(17) 0.0770(13) Uani 1 1 d . . . H37A H 0.4061 0.5088 0.5687 0.092 Uiso 1 1 calc R . . C38 C 0.5143(3) 0.4521(2) 0.61827(13) 0.0556(10) Uani 1 1 d . . . H38A H 0.4972 0.3997 0.6062 0.067 Uiso 1 1 calc R . . C39 C 0.9922(2) 0.32081(19) 0.75172(11) 0.0364(7) Uani 1 1 d . . . C40 C 1.0284(3) 0.2428(2) 0.75556(12) 0.0466(8) Uani 1 1 d . . . H40A H 1.0054 0.2055 0.7302 0.056 Uiso 1 1 calc R . . C41 C 1.0990(3) 0.2177(3) 0.79638(14) 0.0586(11) Uani 1 1 d . . . H41A H 1.1230 0.1636 0.7987 0.070 Uiso 1 1 calc R . . C42 C 1.1332(3) 0.2715(3) 0.83291(13) 0.0566(10) Uani 1 1 d . . . H42A H 1.1808 0.2545 0.8607 0.068 Uiso 1 1 calc R . . C43 C 1.0990(3) 0.3489(3) 0.82943(12) 0.0563(10) Uani 1 1 d . . . H43A H 1.1233 0.3861 0.8547 0.068 Uiso 1 1 calc R . . C44 C 1.0288(3) 0.3741(2) 0.78927(11) 0.0472(9) Uani 1 1 d . . . H44A H 1.0054 0.4284 0.7873 0.057 Uiso 1 1 calc R . . C45 C 0.9871(3) 0.42930(18) 0.67347(10) 0.0351(7) Uani 1 1 d . . . C46 C 1.0993(3) 0.4175(2) 0.67048(11) 0.0422(8) Uani 1 1 d . . . H46A H 1.1328 0.3702 0.6843 0.051 Uiso 1 1 calc R . . C47 C 1.1634(3) 0.4724(2) 0.64811(12) 0.0496(9) Uani 1 1 d . . . H47A H 1.2397 0.4625 0.6467 0.059 Uiso 1 1 calc R . . C48 C 1.1169(3) 0.5413(2) 0.62776(13) 0.0578(10) Uani 1 1 d . . . H48A H 1.1610 0.5794 0.6126 0.069 Uiso 1 1 calc R . . C49 C 1.0059(4) 0.5551(2) 0.62950(13) 0.0574(10) Uani 1 1 d . . . H49A H 0.9735 0.6024 0.6152 0.069 Uiso 1 1 calc R . . C50 C 0.9406(3) 0.4994(2) 0.65237(11) 0.0459(9) Uani 1 1 d . . . H50A H 0.8643 0.5094 0.6535 0.055 Uiso 1 1 calc R . . C51 C 0.6789(3) 0.06368(19) 0.68870(11) 0.0445(8) Uani 1 1 d . . . H51A H 0.7322 0.0237 0.6784 0.053 Uiso 1 1 calc R . . H51B H 0.6125 0.0623 0.6648 0.053 Uiso 1 1 calc R . . C52 C 0.6490(4) 0.0458(2) 0.74077(13) 0.0614(11) Uani 1 1 d . . . H52A H 0.5724 0.0261 0.7401 0.074 Uiso 1 1 calc R . . H52B H 0.6991 0.0050 0.7570 0.074 Uiso 1 1 calc R . . C53 C 0.6618(4) 0.1252(2) 0.76756(13) 0.0628(11) Uani 1 1 d . . . H53A H 0.5929 0.1567 0.7636 0.075 Uiso 1 1 calc R . . H53B H 0.6841 0.1175 0.8033 0.075 Uiso 1 1 calc R . . C54 C 0.7494(3) 0.1640(2) 0.74241(12) 0.0547(10) Uani 1 1 d . . . H54A H 0.7476 0.2228 0.7470 0.066 Uiso 1 1 calc R . . H54B H 0.8225 0.1437 0.7556 0.066 Uiso 1 1 calc R . . C55 C 0.9364(3) 0.0805(2) 0.63647(14) 0.0500(9) Uani 1 1 d . . . H55A H 0.8754 0.0537 0.6162 0.060 Uiso 1 1 calc R . . H55B H 0.9318 0.0660 0.6717 0.060 Uiso 1 1 calc R . . C56 C 1.0446(4) 0.0555(3) 0.6200(2) 0.0849(15) Uani 1 1 d . . . H56A H 1.0389 0.0438 0.5840 0.102 Uiso 1 1 calc R . . H56B H 1.0743 0.0079 0.6385 0.102 Uiso 1 1 calc R . . C57 C 1.1152(3) 0.1303(3) 0.63252(19) 0.0776(13) Uani 1 1 d . . . H57A H 1.1422 0.1318 0.6681 0.093 Uiso 1 1 calc R . . H57B H 1.1787 0.1330 0.6123 0.093 Uiso 1 1 calc R . . C58 C 1.0364(3) 0.1952(2) 0.61971(14) 0.0544(9) Uani 1 1 d . . . H58A H 1.0564 0.2436 0.6398 0.065 Uiso 1 1 calc R . . H58B H 1.0363 0.2093 0.5842 0.065 Uiso 1 1 calc R . . C59 C 0.7229(3) 0.3866(3) 0.54045(15) 0.0709(12) Uani 1 1 d . . . H59A H 0.7058 0.4355 0.5590 0.085 Uiso 1 1 calc R . . H59B H 0.6538 0.3565 0.5320 0.085 Uiso 1 1 calc R . . C60 C 0.7759(3) 0.4082(2) 0.49439(14) 0.0631(11) Uani 1 1 d . . . H60A H 0.7652 0.3655 0.4690 0.076 Uiso 1 1 calc R . . H60B H 0.7468 0.4594 0.4801 0.076 Uiso 1 1 calc R . . C61 C 0.8938(3) 0.4157(2) 0.51362(14) 0.0631(11) Uani 1 1 d . . . H61A H 0.9092 0.4690 0.5288 0.076 Uiso 1 1 calc R . . H61B H 0.9428 0.4072 0.4869 0.076 Uiso 1 1 calc R . . C62 C 0.9081(3) 0.3506(2) 0.55177(11) 0.0437(8) Uani 1 1 d . . . H62A H 0.9347 0.3008 0.5369 0.052 Uiso 1 1 calc R . . H62B H 0.9621 0.3669 0.5794 0.052 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 Ca1 0.0294(3) 0.0304(3) 0.0296(3) 0.0003(2) 0.0054(2) 0.0010(3) P1 0.0316(5) 0.0356(5) 0.0354(4) -0.0034(4) 0.0056(3) 0.0014(4) P2 0.0321(5) 0.0393(5) 0.0319(4) -0.0048(3) 0.0035(3) 0.0035(4) P3 0.0321(5) 0.0327(4) 0.0368(4) -0.0044(3) 0.0052(3) 0.0020(4) P4 0.0312(5) 0.0342(4) 0.0333(4) -0.0020(3) 0.0037(3) -0.0020(4) O1 0.0530(15) 0.0390(13) 0.0350(11) 0.0047(10) 0.0102(10) -0.0043(11) O2 0.0335(13) 0.0383(13) 0.0599(14) -0.0029(11) 0.0040(10) 0.0079(10) O3 0.0418(14) 0.0492(14) 0.0427(12) 0.0153(10) 0.0058(10) -0.0009(11) C1 0.0334(19) 0.0413(19) 0.0361(17) -0.0034(15) 0.0019(14) 0.0031(15) C2 0.0324(18) 0.0425(19) 0.0384(17) -0.0006(14) 0.0031(13) 0.0054(15) C3 0.052(2) 0.052(2) 0.0375(18) -0.0002(16) 0.0061(15) 0.0068(18) C4 0.077(3) 0.074(3) 0.046(2) 0.017(2) 0.021(2) 0.017(2) C5 0.083(3) 0.064(3) 0.081(3) 0.035(2) 0.036(2) 0.015(2) C6 0.063(3) 0.039(2) 0.083(3) 0.005(2) 0.022(2) 0.0009(19) C7 0.042(2) 0.0390(19) 0.0494(19) 0.0048(16) 0.0090(15) 0.0037(16) C8 0.0352(19) 0.0309(17) 0.0429(17) -0.0042(14) 0.0066(14) 0.0007(14) C9 0.039(2) 0.041(2) 0.0495(19) -0.0034(16) 0.0105(15) 0.0024(16) C10 0.038(2) 0.049(2) 0.068(2) -0.0027(19) 0.0114(17) 0.0107(17) C11 0.046(2) 0.041(2) 0.078(3) 0.0070(19) 0.0020(19) 0.0138(17) C12 0.062(3) 0.051(2) 0.061(2) 0.0155(18) 0.0137(19) 0.013(2) C13 0.040(2) 0.049(2) 0.054(2) 0.0095(17) 0.0125(16) 0.0123(17) C14 0.0319(18) 0.0430(19) 0.0325(15) -0.0027(14) -0.0073(13) 0.0086(15) C15 0.044(2) 0.042(2) 0.0393(17) -0.0024(15) 0.0006(15) 0.0058(16) C16 0.055(2) 0.049(2) 0.0455(19) 0.0042(17) -0.0088(17) 0.0000(19) C17 0.053(2) 0.042(2) 0.065(2) -0.0048(19) -0.0121(19) 0.0130(19) C18 0.060(3) 0.056(3) 0.084(3) -0.007(2) 0.015(2) 0.028(2) C19 0.043(2) 0.052(2) 0.067(2) 0.0013(19) 0.0128(18) 0.0143(18) C20 0.037(2) 0.0342(17) 0.0320(16) -0.0071(13) 0.0034(13) -0.0013(14) C21 0.040(2) 0.0396(19) 0.0407(18) -0.0049(15) 0.0066(15) 0.0031(15) C22 0.051(2) 0.050(2) 0.0376(17) 0.0023(16) 0.0059(15) 0.0050(17) C23 0.058(3) 0.051(2) 0.047(2) -0.0015(17) 0.0200(18) -0.0043(19) C24 0.039(2) 0.077(3) 0.061(2) -0.002(2) 0.0199(18) -0.005(2) C25 0.036(2) 0.062(2) 0.0414(18) -0.0002(16) 0.0038(15) 0.0040(17) C26 0.0336(19) 0.0365(18) 0.0406(17) -0.0085(15) 0.0052(14) -0.0057(15) C27 0.0306(18) 0.0268(16) 0.0435(17) -0.0054(13) 0.0057(13) -0.0008(13) C28 0.035(2) 0.052(2) 0.0446(18) -0.0036(16) 0.0040(14) -0.0057(16) C29 0.048(2) 0.071(3) 0.0460(19) 0.0019(18) 0.0121(17) -0.0068(19) C30 0.044(2) 0.054(2) 0.063(2) 0.0052(18) 0.0193(18) -0.0017(18) C31 0.029(2) 0.049(2) 0.076(3) 0.0087(18) 0.0056(17) 0.0010(16) C32 0.035(2) 0.044(2) 0.0509(19) 0.0041(16) 0.0013(15) -0.0010(16) C33 0.039(2) 0.0402(19) 0.0415(17) 0.0028(15) 0.0136(15) 0.0076(15) C34 0.077(3) 0.037(2) 0.051(2) 0.0003(16) 0.0245(19) 0.0091(19) C35 0.114(4) 0.042(2) 0.083(3) 0.012(2) 0.058(3) 0.024(3) C36 0.082(4) 0.084(4) 0.090(3) 0.050(3) 0.044(3) 0.047(3) C37 0.057(3) 0.099(4) 0.076(3) 0.028(3) 0.010(2) 0.022(3) C38 0.046(2) 0.060(2) 0.060(2) 0.0151(19) 0.0011(18) 0.0088(19) C39 0.0300(18) 0.0398(19) 0.0403(17) 0.0035(14) 0.0084(13) -0.0063(14) C40 0.040(2) 0.050(2) 0.0501(19) 0.0074(16) 0.0053(15) 0.0022(17) C41 0.045(2) 0.065(3) 0.067(3) 0.030(2) 0.0107(19) 0.0098(19) C42 0.037(2) 0.088(3) 0.045(2) 0.022(2) -0.0002(16) -0.012(2) C43 0.049(2) 0.076(3) 0.0424(19) 0.0079(19) -0.0029(16) -0.016(2) C44 0.050(2) 0.051(2) 0.0397(18) 0.0001(16) 0.0000(15) -0.0083(17) C45 0.039(2) 0.0381(18) 0.0291(15) -0.0060(14) 0.0052(13) -0.0054(15) C46 0.040(2) 0.047(2) 0.0404(17) -0.0012(15) 0.0068(14) -0.0070(16) C47 0.044(2) 0.064(3) 0.0424(19) -0.0047(18) 0.0103(16) -0.0121(19) C48 0.067(3) 0.063(3) 0.047(2) -0.0038(19) 0.0236(19) -0.026(2) C49 0.078(3) 0.045(2) 0.051(2) 0.0074(17) 0.0141(19) -0.005(2) C50 0.055(2) 0.039(2) 0.0456(19) -0.0001(16) 0.0137(16) 0.0007(17) C51 0.053(2) 0.0346(18) 0.0461(19) 0.0014(15) 0.0036(16) -0.0002(16) C52 0.077(3) 0.050(2) 0.057(2) 0.0118(18) 0.002(2) -0.016(2) C53 0.082(3) 0.065(3) 0.043(2) 0.0046(19) 0.0135(19) -0.014(2) C54 0.067(3) 0.054(2) 0.0439(19) -0.0012(17) 0.0079(17) -0.0139(19) C55 0.046(2) 0.038(2) 0.066(2) -0.0064(17) 0.0029(17) 0.0073(16) C56 0.064(3) 0.051(3) 0.146(4) -0.001(3) 0.043(3) 0.010(2) C57 0.046(3) 0.080(3) 0.109(3) 0.009(3) 0.017(2) 0.014(2) C58 0.041(2) 0.049(2) 0.075(2) 0.0068(19) 0.0125(18) 0.0021(18) C59 0.045(2) 0.086(3) 0.082(3) 0.035(2) 0.006(2) 0.010(2) C60 0.077(3) 0.051(2) 0.058(2) 0.0154(19) -0.013(2) -0.005(2) C61 0.062(3) 0.069(3) 0.059(2) 0.022(2) 0.0095(19) -0.005(2) C62 0.044(2) 0.050(2) 0.0382(17) -0.0007(16) 0.0063(14) 0.0023(17) _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 Ca1 O3 2.370(2) . ? Ca1 O1 2.394(2) . ? Ca1 O2 2.428(2) . ? Ca1 P3 3.0589(9) . ? Ca1 P2 3.0654(9) . ? Ca1 P4 3.1066(10) . ? Ca1 P1 3.1455(10) . ? P1 C1 1.730(3) . ? P1 C2 1.841(3) . ? P1 C8 1.849(3) . ? P2 C1 1.728(3) . ? P2 C20 1.854(3) . ? P2 C14 1.860(3) . ? P3 C26 1.724(3) . ? P3 C33 1.846(3) . ? P3 C27 1.856(3) . ? P4 C26 1.734(3) . ? P4 C45 1.846(3) . ? P4 C39 1.851(3) . ? O1 C54 1.447(4) . ? O1 C51 1.452(4) . ? O2 C58 1.434(4) . ? O2 C55 1.450(4) . ? O3 C59 1.435(4) . ? O3 C62 1.443(4) . ? C1 H1 0.93(3) . ? C2 C7 1.387(4) . ? C2 C3 1.391(4) . ? C3 C4 1.371(5) . ? C3 H3A 0.9500 . ? C4 C5 1.372(6) . ? C4 H4A 0.9500 . ? C5 C6 1.392(5) . ? C5 H5A 0.9500 . ? C6 C7 1.376(5) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 C13 1.394(4) . ? C8 C9 1.396(4) . ? C9 C10 1.383(5) . ? C9 H9A 0.9500 . ? C10 C11 1.379(5) . ? C10 H10A 0.9500 . ? C11 C12 1.384(5) . ? C11 H11A 0.9500 . ? C12 C13 1.381(5) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 C15 1.383(4) . ? C14 C19 1.391(4) . ? C15 C16 1.389(5) . ? C15 H15A 0.9500 . ? C16 C17 1.371(5) . ? C16 H16A 0.9500 . ? C17 C18 1.362(5) . ? C17 H17A 0.9500 . ? C18 C19 1.401(5) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 C21 1.380(4) . ? C20 C25 1.383(4) . ? C21 C22 1.389(4) . ? C21 H21A 0.9500 . ? C22 C23 1.372(5) . ? C22 H22A 0.9500 . ? C23 C24 1.388(5) . ? C23 H23A 0.9500 . ? C24 C25 1.384(5) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? C26 H26 0.93(3) . ? C27 C28 1.386(4) . ? C27 C32 1.385(4) . ? C28 C29 1.393(4) . ? C28 H28A 0.9500 . ? C29 C30 1.371(5) . ? C29 H29A 0.9500 . ? C30 C31 1.368(5) . ? C30 H30A 0.9500 . ? C31 C32 1.401(4) . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? C33 C34 1.380(5) . ? C33 C38 1.383(5) . ? C34 C35 1.398(5) . ? C34 H34A 0.9500 . ? C35 C36 1.380(7) . ? C35 H35A 0.9500 . ? C36 C37 1.370(7) . ? C36 H36A 0.9500 . ? C37 C38 1.379(5) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? C39 C40 1.375(4) . ? C39 C44 1.393(4) . ? C40 C41 1.402(5) . ? C40 H40A 0.9500 . ? C41 C42 1.372(5) . ? C41 H41A 0.9500 . ? C42 C43 1.358(5) . ? C42 H42A 0.9500 . ? C43 C44 1.387(5) . ? C43 H43A 0.9500 . ? C44 H44A 0.9500 . ? C45 C46 1.394(4) . ? C45 C50 1.399(4) . ? C46 C47 1.379(5) . ? C46 H46A 0.9500 . ? C47 C48 1.376(5) . ? C47 H47A 0.9500 . ? C48 C49 1.380(5) . ? C48 H48A 0.9500 . ? C49 C50 1.403(5) . ? C49 H49A 0.9500 . ? C50 H50A 0.9500 . ? C51 C52 1.517(4) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.511(5) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.468(5) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.492(5) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.538(6) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.469(5) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.500(5) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.491(5) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.498(5) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? 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 O3 Ca1 O1 174.44(8) . . ? O3 Ca1 O2 96.57(8) . . ? O1 Ca1 O2 80.51(8) . . ? O3 Ca1 P3 88.17(6) . . ? O1 Ca1 P3 90.67(5) . . ? O2 Ca1 P3 135.96(6) . . ? O3 Ca1 P2 81.09(6) . . ? O1 Ca1 P2 103.04(6) . . ? O2 Ca1 P2 81.46(6) . . ? P3 Ca1 P2 142.24(3) . . ? O3 Ca1 P4 80.54(6) . . ? O1 Ca1 P4 94.31(6) . . ? O2 Ca1 P4 81.60(6) . . ? P3 Ca1 P4 55.95(2) . . ? P2 Ca1 P4 153.32(3) . . ? O3 Ca1 P1 93.67(6) . . ? O1 Ca1 P1 91.76(6) . . ? O2 Ca1 P1 133.47(6) . . ? P3 Ca1 P1 89.51(3) . . ? P2 Ca1 P1 55.55(2) . . ? P4 Ca1 P1 144.92(3) . . ? C1 P1 C2 110.80(15) . . ? C1 P1 C8 105.78(14) . . ? C2 P1 C8 99.01(14) . . ? C1 P1 Ca1 93.71(12) . . ? C2 P1 Ca1 110.96(10) . . ? C8 P1 Ca1 135.52(10) . . ? C1 P2 C20 108.89(14) . . ? C1 P2 C14 107.53(15) . . ? C20 P2 C14 101.30(13) . . ? C1 P2 Ca1 96.56(11) . . ? C20 P2 Ca1 119.67(10) . . ? C14 P2 Ca1 121.98(9) . . ? C26 P3 C33 110.21(16) . . ? C26 P3 C27 108.44(14) . . ? C33 P3 C27 96.60(13) . . ? C26 P3 Ca1 95.81(11) . . ? C33 P3 Ca1 121.87(10) . . ? C27 P3 Ca1 123.59(9) . . ? C26 P4 C45 109.40(15) . . ? C26 P4 C39 109.12(14) . . ? C45 P4 C39 97.67(14) . . ? C26 P4 Ca1 93.95(11) . . ? C45 P4 Ca1 120.75(9) . . ? C39 P4 Ca1 125.37(10) . . ? C54 O1 C51 106.9(2) . . ? C54 O1 Ca1 120.65(18) . . ? C51 O1 Ca1 132.20(17) . . ? C58 O2 C55 108.3(2) . . ? C58 O2 Ca1 129.06(19) . . ? C55 O2 Ca1 122.20(19) . . ? C59 O3 C62 108.3(2) . . ? C59 O3 Ca1 124.9(2) . . ? C62 O3 Ca1 126.11(18) . . ? P2 C1 P1 113.72(19) . . ? P2 C1 H1 121(2) . . ? P1 C1 H1 123(2) . . ? C7 C2 C3 118.0(3) . . ? C7 C2 P1 122.9(2) . . ? C3 C2 P1 118.9(3) . . ? C4 C3 C2 121.9(4) . . ? C4 C3 H3A 119.1 . . ? C2 C3 H3A 119.1 . . ? C3 C4 C5 119.2(4) . . ? C3 C4 H4A 120.4 . . ? C5 C4 H4A 120.4 . . ? C4 C5 C6 120.5(4) . . ? C4 C5 H5A 119.8 . . ? C6 C5 H5A 119.8 . . ? C7 C6 C5 119.6(4) . . ? C7 C6 H6A 120.2 . . ? C5 C6 H6A 120.2 . . ? C6 C7 C2 120.9(3) . . ? C6 C7 H7A 119.5 . . ? C2 C7 H7A 119.5 . . ? C13 C8 C9 116.9(3) . . ? C13 C8 P1 119.8(2) . . ? C9 C8 P1 123.3(2) . . ? C10 C9 C8 121.6(3) . . ? C10 C9 H9A 119.2 . . ? C8 C9 H9A 119.2 . . ? C9 C10 C11 120.3(3) . . ? C9 C10 H10A 119.8 . . ? C11 C10 H10A 119.8 . . ? C10 C11 C12 119.3(3) . . ? C10 C11 H11A 120.4 . . ? C12 C11 H11A 120.4 . . ? C13 C12 C11 120.1(3) . . ? C13 C12 H12A 119.9 . . ? C11 C12 H12A 119.9 . . ? C12 C13 C8 121.8(3) . . ? C12 C13 H13A 119.1 . . ? C8 C13 H13A 119.1 . . ? C15 C14 C19 117.7(3) . . ? C15 C14 P2 116.7(2) . . ? C19 C14 P2 125.5(3) . . ? C14 C15 C16 121.5(3) . . ? C14 C15 H15A 119.3 . . ? C16 C15 H15A 119.3 . . ? C17 C16 C15 120.4(3) . . ? C17 C16 H16A 119.8 . . ? C15 C16 H16A 119.8 . . ? C18 C17 C16 119.0(3) . . ? C18 C17 H17A 120.5 . . ? C16 C17 H17A 120.5 . . ? C17 C18 C19 121.4(3) . . ? C17 C18 H18A 119.3 . . ? C19 C18 H18A 119.3 . . ? C14 C19 C18 120.0(4) . . ? C14 C19 H19A 120.0 . . ? C18 C19 H19A 120.0 . . ? C21 C20 C25 118.0(3) . . ? C21 C20 P2 120.7(2) . . ? C25 C20 P2 121.1(2) . . ? C20 C21 C22 120.9(3) . . ? C20 C21 H21A 119.6 . . ? C22 C21 H21A 119.6 . . ? C23 C22 C21 120.6(3) . . ? C23 C22 H22A 119.7 . . ? C21 C22 H22A 119.7 . . ? C22 C23 C24 119.3(3) . . ? C22 C23 H23A 120.4 . . ? C24 C23 H23A 120.4 . . ? C25 C24 C23 119.6(3) . . ? C25 C24 H24A 120.2 . . ? C23 C24 H24A 120.2 . . ? C24 C25 C20 121.6(3) . . ? C24 C25 H25A 119.2 . . ? C20 C25 H25A 119.2 . . ? P3 C26 P4 113.53(18) . . ? P3 C26 H26 125.5(19) . . ? P4 C26 H26 118.2(19) . . ? C28 C27 C32 117.6(3) . . ? C28 C27 P3 120.5(2) . . ? C32 C27 P3 121.9(2) . . ? C27 C28 C29 121.1(3) . . ? C27 C28 H28A 119.5 . . ? C29 C28 H28A 119.5 . . ? C30 C29 C28 120.3(3) . . ? C30 C29 H29A 119.9 . . ? C28 C29 H29A 119.9 . . ? C31 C30 C29 119.9(3) . . ? C31 C30 H30A 120.1 . . ? C29 C30 H30A 120.1 . . ? C30 C31 C32 119.8(3) . . ? C30 C31 H31A 120.1 . . ? C32 C31 H31A 120.1 . . ? C27 C32 C31 121.3(3) . . ? C27 C32 H32A 119.4 . . ? C31 C32 H32A 119.4 . . ? C34 C33 C38 118.0(3) . . ? C34 C33 P3 122.0(3) . . ? C38 C33 P3 120.1(3) . . ? C33 C34 C35 120.8(4) . . ? C33 C34 H34A 119.6 . . ? C35 C34 H34A 119.6 . . ? C36 C35 C34 119.6(4) . . ? C36 C35 H35A 120.2 . . ? C34 C35 H35A 120.2 . . ? C37 C36 C35 120.1(4) . . ? C37 C36 H36A 119.9 . . ? C35 C36 H36A 119.9 . . ? C36 C37 C38 119.7(4) . . ? C36 C37 H37A 120.2 . . ? C38 C37 H37A 120.2 . . ? C37 C38 C33 121.8(4) . . ? C37 C38 H38A 119.1 . . ? C33 C38 H38A 119.1 . . ? C40 C39 C44 118.0(3) . . ? C40 C39 P4 120.5(3) . . ? C44 C39 P4 121.6(3) . . ? C39 C40 C41 120.8(3) . . ? C39 C40 H40A 119.6 . . ? C41 C40 H40A 119.6 . . ? C42 C41 C40 119.9(4) . . ? C42 C41 H41A 120.1 . . ? C40 C41 H41A 120.1 . . ? C43 C42 C41 120.0(3) . . ? C43 C42 H42A 120.0 . . ? C41 C42 H42A 120.0 . . ? C42 C43 C44 120.4(4) . . ? C42 C43 H43A 119.8 . . ? C44 C43 H43A 119.8 . . ? C43 C44 C39 120.9(4) . . ? C43 C44 H44A 119.5 . . ? C39 C44 H44A 119.5 . . ? C46 C45 C50 117.3(3) . . ? C46 C45 P4 122.9(2) . . ? C50 C45 P4 119.5(2) . . ? C47 C46 C45 122.1(3) . . ? C47 C46 H46A 118.9 . . ? C45 C46 H46A 118.9 . . ? C48 C47 C46 120.0(3) . . ? C48 C47 H47A 120.0 . . ? C46 C47 H47A 120.0 . . ? C47 C48 C49 119.8(3) . . ? C47 C48 H48A 120.1 . . ? C49 C48 H48A 120.1 . . ? C48 C49 C50 120.2(4) . . ? C48 C49 H49A 119.9 . . ? C50 C49 H49A 119.9 . . ? C45 C50 C49 120.5(3) . . ? C45 C50 H50A 119.7 . . ? C49 C50 H50A 119.7 . . ? O1 C51 C52 106.2(3) . . ? O1 C51 H51A 110.5 . . ? C52 C51 H51A 110.5 . . ? O1 C51 H51B 110.5 . . ? C52 C51 H51B 110.5 . . ? H51A C51 H51B 108.7 . . ? C53 C52 C51 104.5(3) . . ? C53 C52 H52A 110.9 . . ? C51 C52 H52A 110.9 . . ? C53 C52 H52B 110.9 . . ? C51 C52 H52B 110.9 . . ? H52A C52 H52B 108.9 . . ? C54 C53 C52 102.2(3) . . ? C54 C53 H53A 111.3 . . ? C52 C53 H53A 111.3 . . ? C54 C53 H53B 111.3 . . ? C52 C53 H53B 111.3 . . ? H53A C53 H53B 109.2 . . ? O1 C54 C53 105.4(3) . . ? O1 C54 H54A 110.7 . . ? C53 C54 H54A 110.7 . . ? O1 C54 H54B 110.7 . . ? C53 C54 H54B 110.7 . . ? H54A C54 H54B 108.8 . . ? O2 C55 C56 106.2(3) . . ? O2 C55 H55A 110.5 . . ? C56 C55 H55A 110.5 . . ? O2 C55 H55B 110.5 . . ? C56 C55 H55B 110.5 . . ? H55A C55 H55B 108.7 . . ? C55 C56 C57 101.6(3) . . ? C55 C56 H56A 111.4 . . ? C57 C56 H56A 111.4 . . ? C55 C56 H56B 111.4 . . ? C57 C56 H56B 111.4 . . ? H56A C56 H56B 109.3 . . ? C58 C57 C56 101.7(3) . . ? C58 C57 H57A 111.4 . . ? C56 C57 H57A 111.4 . . ? C58 C57 H57B 111.4 . . ? C56 C57 H57B 111.4 . . ? H57A C57 H57B 109.3 . . ? O2 C58 C57 107.2(3) . . ? O2 C58 H58A 110.3 . . ? C57 C58 H58A 110.3 . . ? O2 C58 H58B 110.3 . . ? C57 C58 H58B 110.3 . . ? H58A C58 H58B 108.5 . . ? O3 C59 C60 105.8(3) . . ? O3 C59 H59A 110.6 . . ? C60 C59 H59A 110.6 . . ? O3 C59 H59B 110.6 . . ? C60 C59 H59B 110.6 . . ? H59A C59 H59B 108.7 . . ? C61 C60 C59 101.9(3) . . ? C61 C60 H60A 111.4 . . ? C59 C60 H60A 111.4 . . ? C61 C60 H60B 111.4 . . ? C59 C60 H60B 111.4 . . ? H60A C60 H60B 109.3 . . ? C60 C61 C62 103.2(3) . . ? C60 C61 H61A 111.1 . . ? C62 C61 H61A 111.1 . . ? C60 C61 H61B 111.1 . . ? C62 C61 H61B 111.1 . . ? H61A C61 H61B 109.1 . . ? O3 C62 C61 106.4(3) . . ? O3 C62 H62A 110.4 . . ? C61 C62 H62A 110.4 . . ? O3 C62 H62B 110.4 . . ? C61 C62 H62B 110.4 . . ? H62A C62 H62B 108.6 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.581 _refine_diff_density_min -0.295 _refine_diff_density_rms 0.065 #=== END data_FO3518 _database_code_depnum_ccdc_archive 'CCDC 712111' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H47 B2 Li O2 P2' _chemical_formula_sum 'C33 H47 B2 Li O2 P2' _chemical_formula_weight 566.21 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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' 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 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0747(8) _cell_length_b 11.1578(7) _cell_length_c 16.7869(13) _cell_angle_alpha 97.819(4) _cell_angle_beta 104.841(3) _cell_angle_gamma 106.881(4) _cell_volume 1699.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 11602 _cell_measurement_theta_min 1.96 _cell_measurement_theta_max 27.47 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.106 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 608 _exptl_absorpt_coefficient_mu 0.154 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11602 _diffrn_reflns_av_R_equivalents 0.0555 _diffrn_reflns_av_sigmaI/netI 0.0858 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 27.47 _reflns_number_total 7587 _reflns_number_gt 5238 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.1137P)^2^+1.5978P] 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 7587 _refine_ls_number_parameters 392 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1241 _refine_ls_R_factor_gt 0.0834 _refine_ls_wR_factor_ref 0.2287 _refine_ls_wR_factor_gt 0.2010 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.16735(9) 0.57407(7) 0.21409(5) 0.0235(2) Uani 1 1 d . . . P2 P 0.13390(9) 0.84359(7) 0.21873(5) 0.0225(2) Uani 1 1 d . . . B1 B 0.1934(5) 0.5764(4) 0.3321(3) 0.0329(9) Uani 1 1 d . . . H1B1 H 0.097(4) 0.578(4) 0.349(2) 0.033(9) Uiso 1 1 d . . . H2B1 H 0.299(4) 0.666(4) 0.370(3) 0.043(11) Uiso 1 1 d . . . H3B1 H 0.205(5) 0.482(5) 0.339(3) 0.064(14) Uiso 1 1 d . . . B2 B 0.1480(5) 0.8800(4) 0.3364(2) 0.0308(9) Uani 1 1 d . . . H1B2 H 0.258(4) 0.882(4) 0.375(3) 0.044(11) Uiso 1 1 d . . . H2B2 H 0.056(4) 0.801(4) 0.349(2) 0.039(10) Uiso 1 1 d . . . H3B2 H 0.145(4) 0.981(4) 0.350(2) 0.039(10) Uiso 1 1 d . . . Li1 Li 0.1921(7) 0.7494(6) 0.4411(4) 0.0338(13) Uani 1 1 d . . . O1 O 0.3713(3) 0.7867(2) 0.53610(16) 0.0402(6) Uani 1 1 d . . . O2 O 0.0446(3) 0.7161(3) 0.50160(18) 0.0490(7) Uani 1 1 d . A . C1 C 0.1462(4) 0.7018(3) 0.1729(2) 0.0299(8) Uani 1 1 d . . . H1 H 0.142(4) 0.694(4) 0.115(3) 0.046(12) Uiso 1 1 d . . . C2 C 0.0148(4) 0.4287(3) 0.1520(2) 0.0267(7) Uani 1 1 d . . . C3 C 0.0200(4) 0.3077(3) 0.1629(2) 0.0310(7) Uani 1 1 d . . . H3A H 0.1031 0.3016 0.2022 0.037 Uiso 1 1 calc R . . C4 C -0.0952(4) 0.1967(3) 0.1169(2) 0.0367(8) Uani 1 1 d . . . H4A H -0.0909 0.1151 0.1248 0.044 Uiso 1 1 calc R . . C5 C -0.2157(4) 0.2047(3) 0.0597(2) 0.0364(8) Uani 1 1 d . . . H5A H -0.2946 0.1286 0.0284 0.044 Uiso 1 1 calc R . . C6 C -0.2222(4) 0.3240(4) 0.0478(2) 0.0382(8) Uani 1 1 d . . . H6A H -0.3051 0.3294 0.0080 0.046 Uiso 1 1 calc R . . C7 C -0.1068(4) 0.4357(3) 0.0945(2) 0.0322(8) Uani 1 1 d . . . H7A H -0.1118 0.5172 0.0867 0.039 Uiso 1 1 calc R . . C8 C 0.3215(4) 0.5417(3) 0.1883(2) 0.0267(7) Uani 1 1 d . . . C9 C 0.4584(4) 0.5899(4) 0.2480(3) 0.0466(10) Uani 1 1 d . . . H9A H 0.4697 0.6326 0.3035 0.056 Uiso 1 1 calc R . . C10 C 0.5805(5) 0.5768(5) 0.2278(4) 0.0626(13) Uani 1 1 d . . . H10A H 0.6741 0.6107 0.2693 0.075 Uiso 1 1 calc R . . C11 C 0.5641(5) 0.5144(4) 0.1476(3) 0.0548(12) Uani 1 1 d . . . H11A H 0.6468 0.5055 0.1334 0.066 Uiso 1 1 calc R . . C12 C 0.4298(5) 0.4656(4) 0.0885(3) 0.0477(11) Uani 1 1 d . . . H12A H 0.4195 0.4225 0.0332 0.057 Uiso 1 1 calc R . . C13 C 0.3070(4) 0.4777(3) 0.1077(2) 0.0343(8) Uani 1 1 d . . . H13A H 0.2138 0.4423 0.0659 0.041 Uiso 1 1 calc R . . C14 C 0.2717(4) 0.9774(3) 0.2007(2) 0.0254(7) Uani 1 1 d . . . C15 C 0.3845(4) 0.9582(3) 0.1748(2) 0.0302(7) Uani 1 1 d . . . H15A H 0.3891 0.8739 0.1639 0.036 Uiso 1 1 calc R . . C16 C 0.4914(4) 1.0601(3) 0.1644(2) 0.0355(8) Uani 1 1 d . . . H16A H 0.5680 1.0452 0.1460 0.043 Uiso 1 1 calc R . . C17 C 0.4864(4) 1.1832(4) 0.1808(2) 0.0373(8) Uani 1 1 d . . . H17A H 0.5593 1.2531 0.1735 0.045 Uiso 1 1 calc R . . C18 C 0.3748(4) 1.2042(3) 0.2079(2) 0.0340(8) Uani 1 1 d . . . H18A H 0.3720 1.2890 0.2200 0.041 Uiso 1 1 calc R . . C19 C 0.2672(4) 1.1023(3) 0.2174(2) 0.0280(7) Uani 1 1 d . . . H19A H 0.1901 1.1172 0.2353 0.034 Uiso 1 1 calc R . . C20 C -0.0361(4) 0.8573(3) 0.1550(2) 0.0265(7) Uani 1 1 d . . . C21 C -0.0572(4) 0.8637(3) 0.0706(2) 0.0337(8) Uani 1 1 d . . . H21A H 0.0203 0.8688 0.0473 0.040 Uiso 1 1 calc R . . C22 C -0.1904(5) 0.8627(4) 0.0203(3) 0.0438(10) Uani 1 1 d . . . H22A H -0.2030 0.8685 -0.0369 0.053 Uiso 1 1 calc R . . C23 C -0.3039(4) 0.8534(3) 0.0525(3) 0.0438(10) Uani 1 1 d . . . H23A H -0.3957 0.8508 0.0175 0.053 Uiso 1 1 calc R . . C24 C -0.2843(4) 0.8479(4) 0.1355(3) 0.0467(10) Uani 1 1 d . . . H24A H -0.3627 0.8423 0.1581 0.056 Uiso 1 1 calc R . . C25 C -0.1513(4) 0.8505(4) 0.1871(3) 0.0374(8) Uani 1 1 d . . . H25A H -0.1391 0.8475 0.2448 0.045 Uiso 1 1 calc R . . C26 C 0.5653(6) 0.6933(6) 0.5462(4) 0.0742(15) Uani 1 1 d . . . H26A H 0.5952 0.6217 0.5626 0.111 Uiso 1 1 calc R . . H26B H 0.6366 0.7748 0.5826 0.111 Uiso 1 1 calc R . . H26C H 0.5604 0.6927 0.4871 0.111 Uiso 1 1 calc R . . C27 C 0.4194(5) 0.6792(4) 0.5559(3) 0.0491(10) Uani 1 1 d . . . H27A H 0.3473 0.5979 0.5179 0.059 Uiso 1 1 calc R . . H27B H 0.4232 0.6740 0.6148 0.059 Uiso 1 1 calc R . . C28 C 0.4406(5) 0.8991(4) 0.6034(3) 0.0461(10) Uani 1 1 d . . . H28A H 0.5472 0.9296 0.6130 0.055 Uiso 1 1 calc R . . H28B H 0.4233 0.8786 0.6562 0.055 Uiso 1 1 calc R . . C29 C 0.3803(6) 1.0017(4) 0.5812(3) 0.0572(12) Uani 1 1 d . . . H29A H 0.4301 1.0798 0.6265 0.086 Uiso 1 1 calc R . . H29B H 0.2755 0.9725 0.5742 0.086 Uiso 1 1 calc R . . H29C H 0.3956 1.0203 0.5282 0.086 Uiso 1 1 calc R . . C30 C -0.1368(8) 0.8098(6) 0.4560(5) 0.098(2) Uani 1 1 d . . . H30A H -0.2375 0.7919 0.4209 0.147 Uiso 1 1 calc R . . H30B H -0.0694 0.8669 0.4333 0.147 Uiso 1 1 calc R . . H30C H -0.1237 0.8515 0.5141 0.147 Uiso 1 1 calc R . . C31 C -0.1072(6) 0.6913(6) 0.4556(4) 0.0794(17) Uani 1 1 d . . . H31A H -0.1294 0.6451 0.3965 0.095 Uiso 1 1 calc R . . H31B H -0.1708 0.6358 0.4820 0.095 Uiso 1 1 calc R . . C32 C 0.0668(7) 0.6794(7) 0.5801(4) 0.086(2) Uani 1 1 d . . . H32A H 0.1652 0.6725 0.5995 0.103 Uiso 0.66(2) 1 calc PR A 1 H32B H -0.0068 0.5951 0.5744 0.103 Uiso 0.66(2) 1 calc PR A 1 H32C H -0.0222 0.6049 0.5706 0.103 Uiso 0.34(2) 1 d PR A 2 H32D H 0.1460 0.6430 0.5826 0.103 Uiso 0.34(2) 1 d PR A 2 C33 C 0.0512(11) 0.7897(11) 0.6469(6) 0.079(4) Uiso 0.66(2) 1 d P A 1 H33A H 0.0660 0.7677 0.7023 0.119 Uiso 0.66(2) 1 calc PR A 1 H33B H -0.0466 0.7955 0.6270 0.119 Uiso 0.66(2) 1 calc PR A 1 H33C H 0.1246 0.8727 0.6519 0.119 Uiso 0.66(2) 1 calc PR A 1 C33A C 0.102(3) 0.728(2) 0.6562(14) 0.096(9) Uiso 0.34(2) 1 d P A 2 H33D H 0.1596 0.6839 0.6889 0.144 Uiso 0.34(2) 1 calc PR A 2 H33E H 0.0133 0.7192 0.6727 0.144 Uiso 0.34(2) 1 calc PR A 2 H33F H 0.1594 0.8193 0.6674 0.144 Uiso 0.34(2) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0325(5) 0.0130(4) 0.0261(4) 0.0036(3) 0.0097(4) 0.0091(3) P2 0.0326(5) 0.0127(4) 0.0229(4) 0.0034(3) 0.0093(3) 0.0083(3) B1 0.048(3) 0.0232(18) 0.030(2) 0.0079(15) 0.0134(19) 0.0144(18) B2 0.049(3) 0.0222(18) 0.0251(19) 0.0054(14) 0.0147(18) 0.0154(17) Li1 0.039(3) 0.030(3) 0.029(3) 0.007(2) 0.010(3) 0.008(3) O1 0.0446(16) 0.0377(14) 0.0304(14) 0.0037(11) 0.0023(12) 0.0127(12) O2 0.0421(16) 0.067(2) 0.0418(16) 0.0184(14) 0.0197(13) 0.0164(15) C1 0.053(2) 0.0154(14) 0.0270(18) 0.0060(12) 0.0157(16) 0.0157(15) C2 0.0347(18) 0.0197(15) 0.0294(17) 0.0062(12) 0.0145(15) 0.0104(13) C3 0.039(2) 0.0175(15) 0.0343(19) 0.0056(13) 0.0087(16) 0.0093(14) C4 0.048(2) 0.0151(15) 0.044(2) 0.0054(14) 0.0152(18) 0.0067(15) C5 0.040(2) 0.0239(17) 0.036(2) -0.0003(14) 0.0141(17) -0.0014(15) C6 0.034(2) 0.0338(19) 0.040(2) 0.0041(16) 0.0050(17) 0.0091(16) C7 0.0348(19) 0.0242(16) 0.0369(19) 0.0052(14) 0.0099(16) 0.0107(15) C8 0.0345(18) 0.0125(13) 0.0368(18) 0.0059(12) 0.0161(15) 0.0090(13) C9 0.038(2) 0.040(2) 0.057(3) 0.0015(19) 0.015(2) 0.0106(18) C10 0.039(2) 0.057(3) 0.089(4) 0.007(3) 0.022(2) 0.014(2) C11 0.051(3) 0.032(2) 0.098(4) 0.017(2) 0.045(3) 0.018(2) C12 0.071(3) 0.0237(18) 0.065(3) 0.0118(18) 0.047(3) 0.0175(19) C13 0.045(2) 0.0216(16) 0.041(2) 0.0089(14) 0.0232(17) 0.0098(15) C14 0.0337(18) 0.0161(14) 0.0227(16) 0.0027(12) 0.0041(14) 0.0076(13) C15 0.0383(19) 0.0226(16) 0.0319(18) 0.0053(13) 0.0141(15) 0.0111(14) C16 0.039(2) 0.0324(18) 0.039(2) 0.0095(15) 0.0191(17) 0.0111(16) C17 0.037(2) 0.0317(18) 0.037(2) 0.0142(15) 0.0075(17) 0.0042(16) C18 0.045(2) 0.0166(15) 0.0357(19) 0.0079(13) 0.0048(16) 0.0093(15) C19 0.0334(18) 0.0164(14) 0.0328(18) 0.0072(13) 0.0076(15) 0.0082(13) C20 0.0309(17) 0.0121(13) 0.0338(18) 0.0028(12) 0.0078(14) 0.0063(12) C21 0.0361(19) 0.0274(17) 0.0305(18) -0.0008(14) 0.0063(15) 0.0074(15) C22 0.050(2) 0.0316(19) 0.036(2) 0.0012(16) -0.0051(18) 0.0131(18) C23 0.033(2) 0.0225(17) 0.063(3) 0.0053(17) -0.0037(19) 0.0077(15) C24 0.034(2) 0.039(2) 0.072(3) 0.018(2) 0.019(2) 0.0152(17) C25 0.040(2) 0.0341(19) 0.045(2) 0.0168(16) 0.0169(18) 0.0155(16) C26 0.066(3) 0.074(4) 0.075(4) 0.001(3) 0.009(3) 0.031(3) C27 0.057(3) 0.038(2) 0.042(2) 0.0042(18) 0.005(2) 0.013(2) C28 0.051(2) 0.036(2) 0.036(2) 0.0021(16) 0.0008(19) 0.0059(18) C29 0.076(3) 0.037(2) 0.047(3) 0.0010(19) 0.007(2) 0.015(2) C30 0.120(6) 0.078(4) 0.128(6) 0.021(4) 0.083(5) 0.042(4) C31 0.072(4) 0.069(4) 0.105(5) 0.021(3) 0.043(4) 0.021(3) C32 0.069(4) 0.132(6) 0.062(4) 0.053(4) 0.033(3) 0.020(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 P1 C1 1.710(3) . ? P1 C2 1.830(3) . ? P1 C8 1.833(3) . ? P1 B1 1.926(4) . ? P2 C1 1.716(3) . ? P2 C20 1.832(3) . ? P2 C14 1.839(3) . ? P2 B2 1.922(4) . ? B1 Li1 2.478(7) . ? B1 H1B1 1.08(4) . ? B1 H2B1 1.18(4) . ? B1 H3B1 1.11(5) . ? B2 Li1 2.467(7) . ? B2 H1B2 1.12(4) . ? B2 H2B2 1.17(4) . ? B2 H3B2 1.13(4) . ? Li1 O1 1.971(7) . ? Li1 O2 1.983(7) . ? Li1 H1B1 2.08(4) . ? Li1 H2B1 2.10(4) . ? Li1 H1B2 2.02(4) . ? Li1 H2B2 2.05(4) . ? O1 C28 1.428(5) . ? O1 C27 1.465(5) . ? O2 C32 1.414(6) . ? O2 C31 1.450(6) . ? C1 H1 0.96(4) . ? C2 C7 1.382(5) . ? C2 C3 1.400(4) . ? C3 C4 1.387(5) . ? C3 H3A 0.9500 . ? C4 C5 1.375(5) . ? C4 H4A 0.9500 . ? C5 C6 1.390(5) . ? C5 H5A 0.9500 . ? C6 C7 1.395(5) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 C9 1.382(5) . ? C8 C13 1.392(5) . ? C9 C10 1.397(6) . ? C9 H9A 0.9500 . ? C10 C11 1.375(7) . ? C10 H10A 0.9500 . ? C11 C12 1.360(7) . ? C11 H11A 0.9500 . ? C12 C13 1.393(5) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 C15 1.376(5) . ? C14 C19 1.401(4) . ? C15 C16 1.387(5) . ? C15 H15A 0.9500 . ? C16 C17 1.382(5) . ? C16 H16A 0.9500 . ? C17 C18 1.382(5) . ? C17 H17A 0.9500 . ? C18 C19 1.384(5) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 C25 1.387(5) . ? C20 C21 1.394(5) . ? C21 C22 1.386(5) . ? C21 H21A 0.9500 . ? C22 C23 1.369(6) . ? C22 H22A 0.9500 . ? C23 C24 1.369(6) . ? C23 H23A 0.9500 . ? C24 C25 1.387(5) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? C26 C27 1.485(7) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.491(6) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.438(8) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33A 1.23(2) . ? C32 C33 1.621(13) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C32 H32C 0.9900 . ? C32 H32D 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C33A H33D 0.9800 . ? C33A H33E 0.9800 . ? C33A H33F 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 C1 P1 C2 108.79(16) . . ? C1 P1 C8 106.89(16) . . ? C2 P1 C8 101.72(14) . . ? C1 P1 B1 121.57(16) . . ? C2 P1 B1 107.89(17) . . ? C8 P1 B1 108.21(17) . . ? C1 P2 C20 107.41(16) . . ? C1 P2 C14 108.45(16) . . ? C20 P2 C14 101.55(14) . . ? C1 P2 B2 120.29(16) . . ? C20 P2 B2 109.47(17) . . ? C14 P2 B2 108.07(16) . . ? P1 B1 Li1 127.1(2) . . ? P1 B1 H1B1 112(2) . . ? Li1 B1 H1B1 56(2) . . ? P1 B1 H2B1 106.0(19) . . ? Li1 B1 H2B1 57.5(19) . . ? H1B1 B1 H2B1 114(3) . . ? P1 B1 H3B1 104(2) . . ? Li1 B1 H3B1 128(2) . . ? H1B1 B1 H3B1 106(3) . . ? H2B1 B1 H3B1 114(3) . . ? P2 B2 Li1 128.6(2) . . ? P2 B2 H1B2 109(2) . . ? Li1 B2 H1B2 54(2) . . ? P2 B2 H2B2 110.1(19) . . ? Li1 B2 H2B2 55.6(19) . . ? H1B2 B2 H2B2 110(3) . . ? P2 B2 H3B2 105(2) . . ? Li1 B2 H3B2 126(2) . . ? H1B2 B2 H3B2 108(3) . . ? H2B2 B2 H3B2 116(3) . . ? O1 Li1 O2 100.1(3) . . ? O1 Li1 B2 127.1(3) . . ? O2 Li1 B2 113.2(3) . . ? O1 Li1 B1 105.7(3) . . ? O2 Li1 B1 120.8(3) . . ? B2 Li1 B1 91.5(2) . . ? O1 Li1 H1B1 123.5(10) . . ? O2 Li1 H1B1 97.3(11) . . ? B2 Li1 H1B1 92.6(10) . . ? B1 Li1 H1B1 25.6(10) . . ? O1 Li1 H2B1 84.5(11) . . ? O2 Li1 H2B1 145.4(12) . . ? B2 Li1 H2B1 89.5(11) . . ? B1 Li1 H2B1 28.4(11) . . ? H1B1 Li1 H2B1 54.0(15) . . ? O1 Li1 H1B2 101.9(12) . . ? O2 Li1 H1B2 134.3(12) . . ? B2 Li1 H1B2 26.8(11) . . ? B1 Li1 H1B2 90.7(12) . . ? H1B1 Li1 H1B2 103.0(16) . . ? H2B1 Li1 H1B2 76.5(16) . . ? O1 Li1 H2B2 152.9(12) . . ? O2 Li1 H2B2 90.3(11) . . ? B2 Li1 H2B2 28.2(11) . . ? B1 Li1 H2B2 89.7(11) . . ? H1B1 Li1 H2B2 79.2(15) . . ? H2B1 Li1 H2B2 101.0(15) . . ? H1B2 Li1 H2B2 54.9(16) . . ? C28 O1 C27 112.4(3) . . ? C28 O1 Li1 127.1(3) . . ? C27 O1 Li1 118.2(3) . . ? C32 O2 C31 114.3(4) . . ? C32 O2 Li1 124.0(4) . . ? C31 O2 Li1 119.4(3) . . ? P1 C1 P2 130.8(2) . . ? P1 C1 H1 115(2) . . ? P2 C1 H1 114(2) . . ? C7 C2 C3 118.9(3) . . ? C7 C2 P1 121.2(2) . . ? C3 C2 P1 119.9(3) . . ? C4 C3 C2 120.6(3) . . ? C4 C3 H3A 119.7 . . ? C2 C3 H3A 119.7 . . ? C5 C4 C3 120.1(3) . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C4 C5 C6 120.1(3) . . ? C4 C5 H5A 119.9 . . ? C6 C5 H5A 119.9 . . ? C5 C6 C7 119.8(3) . . ? C5 C6 H6A 120.1 . . ? C7 C6 H6A 120.1 . . ? C2 C7 C6 120.5(3) . . ? C2 C7 H7A 119.7 . . ? C6 C7 H7A 119.7 . . ? C9 C8 C13 118.6(3) . . ? C9 C8 P1 119.6(3) . . ? C13 C8 P1 121.6(3) . . ? C8 C9 C10 120.9(4) . . ? C8 C9 H9A 119.5 . . ? C10 C9 H9A 119.5 . . ? C11 C10 C9 119.6(5) . . ? C11 C10 H10A 120.2 . . ? C9 C10 H10A 120.2 . . ? C12 C11 C10 120.0(4) . . ? C12 C11 H11A 120.0 . . ? C10 C11 H11A 120.0 . . ? C11 C12 C13 121.0(4) . . ? C11 C12 H12A 119.5 . . ? C13 C12 H12A 119.5 . . ? C8 C13 C12 119.8(4) . . ? C8 C13 H13A 120.1 . . ? C12 C13 H13A 120.1 . . ? C15 C14 C19 118.9(3) . . ? C15 C14 P2 121.0(2) . . ? C19 C14 P2 120.0(3) . . ? C14 C15 C16 120.9(3) . . ? C14 C15 H15A 119.5 . . ? C16 C15 H15A 119.5 . . ? C17 C16 C15 120.0(3) . . ? C17 C16 H16A 120.0 . . ? C15 C16 H16A 120.0 . . ? C16 C17 C18 119.7(3) . . ? C16 C17 H17A 120.1 . . ? C18 C17 H17A 120.1 . . ? C17 C18 C19 120.3(3) . . ? C17 C18 H18A 119.9 . . ? C19 C18 H18A 119.9 . . ? C18 C19 C14 120.2(3) . . ? C18 C19 H19A 119.9 . . ? C14 C19 H19A 119.9 . . ? C25 C20 C21 118.3(3) . . ? C25 C20 P2 121.0(3) . . ? C21 C20 P2 120.5(3) . . ? C22 C21 C20 120.5(4) . . ? C22 C21 H21A 119.8 . . ? C20 C21 H21A 119.8 . . ? C23 C22 C21 120.6(4) . . ? C23 C22 H22A 119.7 . . ? C21 C22 H22A 119.7 . . ? C22 C23 C24 119.5(4) . . ? C22 C23 H23A 120.2 . . ? C24 C23 H23A 120.2 . . ? C23 C24 C25 120.8(4) . . ? C23 C24 H24A 119.6 . . ? C25 C24 H24A 119.6 . . ? C24 C25 C20 120.4(4) . . ? C24 C25 H25A 119.8 . . ? C20 C25 H25A 119.8 . . ? C27 C26 H26A 109.5 . . ? C27 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C27 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O1 C27 C26 112.2(4) . . ? O1 C27 H27A 109.2 . . ? C26 C27 H27A 109.2 . . ? O1 C27 H27B 109.2 . . ? C26 C27 H27B 109.2 . . ? H27A C27 H27B 107.9 . . ? O1 C28 C29 109.5(3) . . ? O1 C28 H28A 109.8 . . ? C29 C28 H28A 109.8 . . ? O1 C28 H28B 109.8 . . ? C29 C28 H28B 109.8 . . ? H28A C28 H28B 108.2 . . ? 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 . . ? C31 C30 H30A 109.5 . . ? C31 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C31 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C30 C31 O2 110.5(5) . . ? C30 C31 H31A 109.5 . . ? O2 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? O2 C31 H31B 109.5 . . ? H31A C31 H31B 108.1 . . ? C33A C32 O2 139.6(15) . . ? C33A C32 C33 36.8(13) . . ? O2 C32 C33 107.0(6) . . ? C33A C32 H32A 80.1 . . ? O2 C32 H32A 110.3 . . ? C33 C32 H32A 110.3 . . ? C33A C32 H32B 102.1 . . ? O2 C32 H32B 110.3 . . ? C33 C32 H32B 110.3 . . ? H32A C32 H32B 108.6 . . ? C33A C32 H32C 103.2 . . ? O2 C32 H32C 103.6 . . ? C33 C32 H32C 103.5 . . ? H32A C32 H32C 121.1 . . ? H32B C32 H32C 12.6 . . ? C33A C32 H32D 97.9 . . ? O2 C32 H32D 103.5 . . ? C33 C32 H32D 131.1 . . ? H32A C32 H32D 21.5 . . ? H32B C32 H32D 93.2 . . ? H32C C32 H32D 105.3 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C33A H33D 109.5 . . ? C32 C33A H33E 109.5 . . ? H33D C33A H33E 109.5 . . ? C32 C33A H33F 109.5 . . ? H33D C33A H33F 109.5 . . ? H33E C33A H33F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.665 _refine_diff_density_min -0.515 _refine_diff_density_rms 0.091 #=== END data_FO3583 _database_code_depnum_ccdc_archive 'CCDC 712112' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H27 B2 P2, C12 H30 Li O6' _chemical_formula_sum 'C37 H57 B2 Li O6 P2' _chemical_formula_weight 688.33 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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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 triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2500(2) _cell_length_b 12.3814(2) _cell_length_c 29.6450(5) _cell_angle_alpha 86.239(1) _cell_angle_beta 81.939(1) _cell_angle_gamma 82.513(1) _cell_volume 4048.91(12) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 28533 _cell_measurement_theta_min 1.83 _cell_measurement_theta_max 27.53 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.129 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 0.147 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28533 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0769 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 27.53 _reflns_number_total 17957 _reflns_number_gt 11470 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.1343P)^2^+8.5876P] 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 17957 _refine_ls_number_parameters 829 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1443 _refine_ls_R_factor_gt 0.0934 _refine_ls_wR_factor_ref 0.2805 _refine_ls_wR_factor_gt 0.2404 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1A P 1.00686(8) -0.20156(7) 0.87030(3) 0.0225(2) Uani 1 1 d . . . P2A P 0.77481(8) -0.32211(8) 0.87591(3) 0.0243(2) Uani 1 1 d . . . B1A B 1.1095(4) -0.1482(4) 0.81793(15) 0.0318(9) Uani 1 1 d . . . H1B1 H 1.0602 -0.0988 0.7988 0.048 Uiso 1 1 calc R . . H2B1 H 1.1501 -0.2099 0.8003 0.048 Uiso 1 1 calc R . . H3B1 H 1.1703 -0.1090 0.8282 0.048 Uiso 1 1 calc R . . B2A B 0.7109(4) -0.2969(4) 0.93900(15) 0.0368(10) Uani 1 1 d . . . H1B2 H 0.7693 -0.3312 0.9588 0.055 Uiso 1 1 calc R . . H2B2 H 0.6346 -0.3284 0.9467 0.055 Uiso 1 1 calc R . . H3B2 H 0.6964 -0.2182 0.9434 0.055 Uiso 1 1 calc R . . C1A C 0.9113(3) -0.2805(3) 0.85215(12) 0.0261(7) Uani 1 1 d . . . H1A H 0.937(3) -0.303(3) 0.8259(14) 0.026(10) Uiso 1 1 d . . . C2A C 1.1028(3) -0.2703(3) 0.91156(12) 0.0261(7) Uani 1 1 d . . . C3A C 1.2098(3) -0.2293(3) 0.91674(13) 0.0341(9) Uani 1 1 d . . . H3AA H 1.2328 -0.1680 0.8982 0.041 Uiso 1 1 calc R . . C4A C 1.2833(4) -0.2769(4) 0.94859(14) 0.0420(10) Uani 1 1 d . . . H4AA H 1.3557 -0.2480 0.9518 0.050 Uiso 1 1 calc R . . C5A C 1.2503(4) -0.3657(4) 0.97540(14) 0.0419(10) Uani 1 1 d . . . H5AA H 1.2999 -0.3983 0.9972 0.050 Uiso 1 1 calc R . . C6A C 1.1446(4) -0.4076(4) 0.97055(14) 0.0409(10) Uani 1 1 d . . . H6AA H 1.1217 -0.4687 0.9892 0.049 Uiso 1 1 calc R . . C7A C 1.0720(4) -0.3604(3) 0.93839(13) 0.0325(8) Uani 1 1 d . . . H7AA H 1.0005 -0.3906 0.9349 0.039 Uiso 1 1 calc R . . C8A C 0.9186(3) -0.0925(3) 0.90403(12) 0.0240(7) Uani 1 1 d . . . C9A C 0.9318(3) -0.0776(3) 0.94884(12) 0.0281(8) Uani 1 1 d . . . H9AA H 0.9915 -0.1238 0.9631 0.034 Uiso 1 1 calc R . . C10A C 0.8588(3) 0.0043(3) 0.97331(13) 0.0318(8) Uani 1 1 d . . . H10A H 0.8690 0.0139 1.0040 0.038 Uiso 1 1 calc R . . C11A C 0.7716(3) 0.0716(3) 0.95286(14) 0.0337(9) Uani 1 1 d . . . H11A H 0.7213 0.1271 0.9696 0.040 Uiso 1 1 calc R . . C12A C 0.7576(4) 0.0579(3) 0.90818(14) 0.0366(9) Uani 1 1 d . . . H12A H 0.6973 0.1040 0.8942 0.044 Uiso 1 1 calc R . . C13A C 0.8311(4) -0.0227(3) 0.88345(14) 0.0331(8) Uani 1 1 d . . . H13A H 0.8220 -0.0307 0.8525 0.040 Uiso 1 1 calc R . . C14A C 0.7892(3) -0.4678(3) 0.86533(12) 0.0264(7) Uani 1 1 d . . . C15A C 0.7928(4) -0.5445(3) 0.90119(14) 0.0351(9) Uani 1 1 d . . . H15A H 0.7798 -0.5213 0.9316 0.042 Uiso 1 1 calc R . . C16A C 0.8151(4) -0.6545(3) 0.89344(16) 0.0406(10) Uani 1 1 d . . . H16A H 0.8166 -0.7064 0.9185 0.049 Uiso 1 1 calc R . . C17A C 0.8353(4) -0.6897(3) 0.84922(17) 0.0410(10) Uani 1 1 d . . . H17A H 0.8508 -0.7654 0.8439 0.049 Uiso 1 1 calc R . . C18A C 0.8326(4) -0.6139(4) 0.81301(16) 0.0440(10) Uani 1 1 d . . . H18A H 0.8472 -0.6371 0.7826 0.053 Uiso 1 1 calc R . . C19A C 0.8084(4) -0.5029(3) 0.82116(14) 0.0366(9) Uani 1 1 d . . . H19A H 0.8051 -0.4509 0.7962 0.044 Uiso 1 1 calc R . . C20A C 0.6564(3) -0.2667(3) 0.84081(12) 0.0281(8) Uani 1 1 d . . . C21A C 0.5434(3) -0.3052(4) 0.84818(14) 0.0370(9) Uani 1 1 d . . . H21A H 0.5293 -0.3623 0.8705 0.044 Uiso 1 1 calc R . . C22A C 0.4520(4) -0.2609(4) 0.82335(16) 0.0455(11) Uani 1 1 d . . . H22B H 0.3760 -0.2885 0.8284 0.055 Uiso 1 1 calc R . . C23A C 0.4706(4) -0.1767(4) 0.79124(16) 0.0471(12) Uani 1 1 d . . . H23A H 0.4073 -0.1455 0.7746 0.056 Uiso 1 1 calc R . . C24A C 0.5820(4) -0.1379(4) 0.78347(15) 0.0457(11) Uani 1 1 d . . . H24A H 0.5954 -0.0804 0.7612 0.055 Uiso 1 1 calc R . . C25A C 0.6743(4) -0.1830(3) 0.80816(13) 0.0363(9) Uani 1 1 d . . . H25A H 0.7506 -0.1561 0.8026 0.044 Uiso 1 1 calc R . . Li1A Li 1.3297(6) 0.2488(6) 0.8685(2) 0.0367(15) Uani 1 1 d . . . O1A O 1.2711(3) 0.4063(3) 0.83355(11) 0.0503(8) Uani 1 1 d . . . O2A O 1.4635(3) 0.2631(3) 0.81489(10) 0.0446(7) Uani 1 1 d . . . O3A O 1.4008(2) 0.3251(2) 0.91949(10) 0.0382(7) Uani 1 1 d . . . O4A O 1.4325(3) 0.1105(2) 0.90507(10) 0.0391(7) Uani 1 1 d . . . O5A O 1.1613(2) 0.2464(2) 0.90659(9) 0.0357(6) Uani 1 1 d . . . O6A O 1.2541(2) 0.1341(2) 0.83309(9) 0.0321(6) Uani 1 1 d . . . C26A C 1.1509(5) 0.4610(5) 0.8356(2) 0.0695(16) Uani 1 1 d . . . H26A H 1.1538 0.5392 0.8286 0.104 Uiso 1 1 calc R . . H26B H 1.1076 0.4500 0.8663 0.104 Uiso 1 1 calc R . . H26F H 1.1087 0.4315 0.8133 0.104 Uiso 1 1 calc R . . C27A C 1.3395(5) 0.4159(4) 0.78981(18) 0.0591(14) Uani 1 1 d . . . H27A H 1.3374 0.4937 0.7794 0.071 Uiso 1 1 calc R . . H27B H 1.3046 0.3774 0.7676 0.071 Uiso 1 1 calc R . . C28A C 1.4669(5) 0.3673(5) 0.79257(18) 0.0605(14) Uani 1 1 d . . . H28A H 1.5124 0.3609 0.7616 0.073 Uiso 1 1 calc R . . H28D H 1.5073 0.4141 0.8099 0.073 Uiso 1 1 calc R . . C29A C 1.5777(4) 0.1965(5) 0.80957(18) 0.0612(15) Uani 1 1 d . . . H29A H 1.6027 0.1830 0.7772 0.092 Uiso 1 1 calc R . . H29E H 1.5707 0.1269 0.8269 0.092 Uiso 1 1 calc R . . H29F H 1.6383 0.2340 0.8210 0.092 Uiso 1 1 calc R . . C30A C 1.4386(5) 0.4308(4) 0.9135(2) 0.0611(15) Uani 1 1 d . . . H30A H 1.4399 0.4597 0.9434 0.092 Uiso 1 1 calc R . . H30E H 1.3820 0.4792 0.8968 0.092 Uiso 1 1 calc R . . H30F H 1.5198 0.4264 0.8962 0.092 Uiso 1 1 calc R . . C31A C 1.4760(4) 0.2540(4) 0.94619(15) 0.0405(10) Uani 1 1 d . . . H31A H 1.4710 0.2820 0.9770 0.049 Uiso 1 1 calc R . . H31D H 1.5612 0.2496 0.9317 0.049 Uiso 1 1 calc R . . C32A C 1.4344(4) 0.1435(4) 0.94968(14) 0.0410(10) Uani 1 1 d . . . H32A H 1.4902 0.0908 0.9657 0.049 Uiso 1 1 calc R . . H32D H 1.3525 0.1462 0.9672 0.049 Uiso 1 1 calc R . . C33A C 1.4223(5) -0.0033(4) 0.90409(19) 0.0534(12) Uani 1 1 d . . . H33D H 1.4971 -0.0459 0.9118 0.080 Uiso 1 1 calc R . . H33E H 1.4089 -0.0201 0.8735 0.080 Uiso 1 1 calc R . . H33F H 1.3541 -0.0218 0.9263 0.080 Uiso 1 1 calc R . . C34A C 1.1211(4) 0.2844(4) 0.95088(15) 0.0493(12) Uani 1 1 d . . . H34A H 1.0335 0.3062 0.9541 0.074 Uiso 1 1 calc R . . H34B H 1.1621 0.3473 0.9554 0.074 Uiso 1 1 calc R . . H34C H 1.1398 0.2261 0.9737 0.074 Uiso 1 1 calc R . . C35A C 1.1055(4) 0.1550(3) 0.89691(14) 0.0355(9) Uani 1 1 d . . . H35A H 1.0175 0.1665 0.9075 0.043 Uiso 1 1 calc R . . H35B H 1.1409 0.0879 0.9126 0.043 Uiso 1 1 calc R . . C36A C 1.1275(3) 0.1443(4) 0.84661(14) 0.0358(9) Uani 1 1 d . . . H36A H 1.0942 0.0791 0.8384 0.043 Uiso 1 1 calc R . . H36B H 1.0876 0.2094 0.8310 0.043 Uiso 1 1 calc R . . C37A C 1.2847(4) 0.1169(4) 0.78541(13) 0.0398(10) Uani 1 1 d . . . H37A H 1.2389 0.0610 0.7769 0.060 Uiso 1 1 calc R . . H37B H 1.3715 0.0928 0.7787 0.060 Uiso 1 1 calc R . . H37C H 1.2645 0.1852 0.7679 0.060 Uiso 1 1 calc R . . P1B P 0.53324(9) -0.79038(9) 0.61976(3) 0.0310(2) Uani 1 1 d . . . P2B P 0.76381(9) -0.67332(8) 0.62621(3) 0.0291(2) Uani 1 1 d . . . B1B B 0.4515(5) -0.7691(6) 0.68123(18) 0.0593(17) Uani 1 1 d . . . H1B3 H 0.5037 -0.8035 0.7033 0.089 Uiso 1 1 calc R . . H2B3 H 0.3759 -0.8021 0.6853 0.089 Uiso 1 1 calc R . . H3B3 H 0.4334 -0.6908 0.6862 0.089 Uiso 1 1 calc R . . B2B B 0.8804(5) -0.6199(5) 0.57877(19) 0.0498(13) Uani 1 1 d . . . H1B4 H 0.8381 -0.5709 0.5572 0.075 Uiso 1 1 calc R . . H2B4 H 0.9271 -0.6815 0.5626 0.075 Uiso 1 1 calc R . . H3B4 H 0.9352 -0.5800 0.5924 0.075 Uiso 1 1 calc R . . C1B C 0.6740(3) -0.7505(4) 0.60303(13) 0.0323(8) Uani 1 1 d . . . H1B H 0.704(5) -0.772(4) 0.5737(18) 0.060(15) Uiso 1 1 d . . . C2B C 0.4293(3) -0.7290(3) 0.57991(13) 0.0318(8) Uani 1 1 d . . . C3B C 0.4671(4) -0.6572(3) 0.54441(14) 0.0367(9) Uani 1 1 d . . . H3BA H 0.5481 -0.6404 0.5403 0.044 Uiso 1 1 calc R . . C4B C 0.3876(5) -0.6098(4) 0.51491(16) 0.0488(11) Uani 1 1 d . . . H4BA H 0.4143 -0.5608 0.4907 0.059 Uiso 1 1 calc R . . C5B C 0.2701(5) -0.6335(4) 0.52067(19) 0.0548(13) Uani 1 1 d . . . H5BA H 0.2157 -0.6007 0.5005 0.066 Uiso 1 1 calc R . . C6B C 0.2315(4) -0.7044(5) 0.5554(2) 0.0586(14) Uani 1 1 d . . . H6BA H 0.1505 -0.7212 0.5592 0.070 Uiso 1 1 calc R . . C7B C 0.3106(4) -0.7517(4) 0.58500(16) 0.0465(11) Uani 1 1 d . . . H7BA H 0.2830 -0.8003 0.6092 0.056 Uiso 1 1 calc R . . C8B C 0.5471(4) -0.9339(4) 0.60625(19) 0.0481(12) Uani 1 1 d . B . C9B C 0.5515(5) -1.0142(4) 0.6410(3) 0.0749(19) Uani 1 1 d . . . H9BA H 0.5417 -0.9846 0.6703 0.090 Uiso 0.50 1 calc PR A 1 H9C H 0.5412 -1.0004 0.6726 0.090 Uiso 0.50 1 d PR A 2 C10B C 0.5653(10) -1.1159(10) 0.6431(5) 0.058(3) Uiso 0.50 1 d P B 1 H10B H 0.5682 -1.1609 0.6703 0.070 Uiso 0.50 1 calc PR B 1 C11B C 0.5758(9) -1.1535(9) 0.5983(5) 0.047(2) Uiso 0.50 1 d P B 1 H11B H 0.5863 -1.2300 0.5945 0.056 Uiso 0.50 1 calc PR B 1 C12B C 0.5716(10) -1.0837(10) 0.5595(4) 0.052(3) Uiso 0.50 1 d P B 1 H12B H 0.5753 -1.1136 0.5305 0.062 Uiso 0.50 1 calc PR B 1 C10C C 0.5765(10) -1.1308(10) 0.6223(5) 0.052(3) Uiso 0.50 1 d P B 2 H10C H 0.5790 -1.1919 0.6434 0.062 Uiso 0.50 1 calc PR B 2 C11C C 0.5952(10) -1.1494(10) 0.5758(5) 0.054(3) Uiso 0.50 1 d P B 2 H11C H 0.6073 -1.2226 0.5668 0.065 Uiso 0.50 1 calc PR B 2 C12C C 0.5972(13) -1.0657(11) 0.5419(5) 0.068(4) Uiso 0.50 1 d P B 2 H12C H 0.6190 -1.0750 0.5101 0.082 Uiso 0.50 1 calc PR B 2 C13B C 0.5616(6) -0.9654(5) 0.5625(2) 0.0734(18) Uani 1 1 d . . . H13B H 0.5648 -0.9157 0.5367 0.088 Uiso 0.50 1 calc PR B 1 H13C H 0.5419 -0.9061 0.5418 0.088 Uiso 0.50 1 d PR B 2 C14B C 0.6724(4) -0.5605(3) 0.65680(13) 0.0317(8) Uani 1 1 d . . . C15B C 0.5792(5) -0.5016(4) 0.6369(2) 0.0651(17) Uani 1 1 d . . . H15B H 0.5624 -0.5213 0.6082 0.078 Uiso 1 1 calc R . . C16B C 0.5096(6) -0.4139(5) 0.6582(2) 0.0733(19) Uani 1 1 d . . . H16B H 0.4461 -0.3738 0.6438 0.088 Uiso 1 1 calc R . . C17B C 0.5316(5) -0.3845(4) 0.69984(18) 0.0515(12) Uani 1 1 d . . . H17B H 0.4816 -0.3262 0.7149 0.062 Uiso 1 1 calc R . . C18B C 0.6258(4) -0.4398(4) 0.71936(16) 0.0471(11) Uani 1 1 d . . . H18B H 0.6439 -0.4181 0.7475 0.057 Uiso 1 1 calc R . . C19B C 0.6954(4) -0.5277(4) 0.69802(15) 0.0422(10) Uani 1 1 d . . . H19B H 0.7603 -0.5661 0.7121 0.051 Uiso 1 1 calc R . . C20B C 0.8440(4) -0.7466(3) 0.67108(14) 0.0359(9) Uani 1 1 d . . . C21B C 0.7950(4) -0.8266(4) 0.69942(15) 0.0458(11) Uani 1 1 d . . . H21B H 0.7174 -0.8447 0.6959 0.055 Uiso 1 1 calc R . . C22B C 0.8575(5) -0.8814(4) 0.73312(16) 0.0562(14) Uani 1 1 d . . . H22A H 0.8219 -0.9357 0.7527 0.067 Uiso 1 1 calc R . . C23B C 0.9705(5) -0.8572(4) 0.73808(17) 0.0570(14) Uani 1 1 d . . . H23B H 1.0130 -0.8950 0.7610 0.068 Uiso 1 1 calc R . . C24B C 1.0218(6) -0.7793(5) 0.7102(2) 0.0664(16) Uani 1 1 d . . . H24B H 1.1002 -0.7632 0.7136 0.080 Uiso 1 1 calc R . . C25B C 0.9591(5) -0.7233(4) 0.67682(19) 0.0546(13) Uani 1 1 d . . . H25B H 0.9951 -0.6686 0.6577 0.066 Uiso 1 1 calc R . . Li1B Li 1.0826(7) -1.2257(7) 0.6233(3) 0.0457(18) Uani 1 1 d . . . O1B O 1.1854(4) -1.1354(3) 0.65604(15) 0.0770(12) Uani 1 1 d . . . O2B O 1.0190(5) -1.0587(4) 0.5996(3) 0.118(2) Uani 1 1 d . . . O3B O 1.2044(4) -1.2510(5) 0.56650(14) 0.104(2) Uani 1 1 d . . . O4B O 0.9799(3) -1.3027(4) 0.58654(13) 0.0771(13) Uani 1 1 d . . . O5B O 0.9520(5) -1.2414(4) 0.67736(18) 0.108(2) Uani 1 1 d . . . O6B O 1.1632(7) -1.3904(6) 0.6577(3) 0.141(2) Uiso 1 1 d . . . C26B C 1.2539(6) -1.1740(7) 0.6900(2) 0.087(2) Uani 1 1 d . . . H26C H 1.2926 -1.1145 0.6996 0.130 Uiso 1 1 calc R . . H26D H 1.3161 -1.2323 0.6785 0.130 Uiso 1 1 calc R . . H26E H 1.2016 -1.2028 0.7161 0.130 Uiso 1 1 calc R . . C27B C 1.1756(9) -1.0259(8) 0.6484(3) 0.123(3) Uiso 1 1 d . . . H27C H 1.2557 -1.0042 0.6357 0.148 Uiso 1 1 calc R . . H27D H 1.1494 -0.9901 0.6777 0.148 Uiso 1 1 calc R . . C28B C 1.0860(11) -0.9880(10) 0.6158(4) 0.146(4) Uiso 1 1 d . . . H28B H 1.0278 -0.9298 0.6307 0.175 Uiso 1 1 calc R . . H28C H 1.1310 -0.9530 0.5889 0.175 Uiso 1 1 calc R . . C29B C 0.9203(9) -1.0137(8) 0.5817(3) 0.127(3) Uiso 1 1 d . . . H29B H 0.9252 -0.9357 0.5748 0.191 Uiso 1 1 calc R . . H29C H 0.8481 -1.0230 0.6035 0.191 Uiso 1 1 calc R . . H29D H 0.9155 -1.0493 0.5535 0.191 Uiso 1 1 calc R . . C30B C 1.3201(11) -1.2471(10) 0.5570(4) 0.166(5) Uiso 1 1 d . . . H30B H 1.3456 -1.2599 0.5246 0.249 Uiso 1 1 calc R . . H30C H 1.3633 -1.3034 0.5755 0.249 Uiso 1 1 calc R . . H30D H 1.3388 -1.1751 0.5637 0.249 Uiso 1 1 calc R . . C31B C 1.1599(13) -1.3103(12) 0.5343(5) 0.187(5) Uiso 1 1 d . . . H31B H 1.2097 -1.3823 0.5322 0.224 Uiso 1 1 calc R . . H31C H 1.1742 -1.2715 0.5041 0.224 Uiso 1 1 calc R . . C32B C 1.0262(8) -1.3304(7) 0.5425(2) 0.102(3) Uani 1 1 d . . . H32B H 0.9805 -1.2853 0.5203 0.123 Uiso 1 1 calc R . . H32C H 1.0195 -1.4081 0.5385 0.123 Uiso 1 1 calc R . . C33B C 0.8603(6) -1.3154(7) 0.6002(3) 0.107(3) Uani 1 1 d . . . H33A H 0.8303 -1.3545 0.5773 0.161 Uiso 1 1 calc R . . H33B H 0.8127 -1.2436 0.6036 0.161 Uiso 1 1 calc R . . H33C H 0.8527 -1.3572 0.6295 0.161 Uiso 1 1 calc R . . C34B C 0.8926(12) -1.1683(11) 0.7062(4) 0.171(5) Uiso 1 1 d . . . H34D H 0.8356 -1.2038 0.7286 0.256 Uiso 1 1 calc R . . H34E H 0.8481 -1.1097 0.6891 0.256 Uiso 1 1 calc R . . H34F H 0.9504 -1.1376 0.7220 0.256 Uiso 1 1 calc R . . C35B C 0.9740(17) -1.3123(15) 0.7166(6) 0.232(7) Uiso 1 1 d . . . H35C H 1.0550 -1.3205 0.7268 0.279 Uiso 1 1 calc R . . H35D H 0.9255 -1.3736 0.7247 0.279 Uiso 1 1 calc R . . C36B C 1.0685(15) -1.4343(12) 0.6868(6) 0.212(6) Uiso 1 1 d . . . H36C H 0.9855 -1.4223 0.6784 0.254 Uiso 1 1 calc R . . H36D H 1.0757 -1.4481 0.7197 0.254 Uiso 1 1 calc R . . C37B C 1.2028(12) -1.4885(11) 0.6417(5) 0.176(5) Uiso 1 1 d . . . H37D H 1.2312 -1.5377 0.6662 0.264 Uiso 1 1 calc R . . H37E H 1.2696 -1.4823 0.6170 0.264 Uiso 1 1 calc R . . H37F H 1.1368 -1.5177 0.6300 0.264 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 P1A 0.0222(4) 0.0221(5) 0.0241(4) 0.0004(3) -0.0048(3) -0.0047(3) P2A 0.0249(5) 0.0283(5) 0.0210(4) -0.0020(4) -0.0043(3) -0.0067(4) B1A 0.030(2) 0.032(2) 0.033(2) 0.0035(18) -0.0017(17) -0.0077(17) B2A 0.038(2) 0.047(3) 0.027(2) -0.007(2) 0.0002(18) -0.011(2) C1A 0.0266(18) 0.030(2) 0.0229(17) -0.0079(15) -0.0007(14) -0.0066(14) C2A 0.0294(18) 0.0216(18) 0.0265(17) 0.0000(14) -0.0053(14) 0.0006(14) C3A 0.031(2) 0.040(2) 0.032(2) 0.0005(17) -0.0087(16) -0.0046(16) C4A 0.032(2) 0.057(3) 0.038(2) -0.007(2) -0.0126(17) 0.0026(19) C5A 0.039(2) 0.053(3) 0.030(2) -0.0017(19) -0.0128(17) 0.014(2) C6A 0.050(3) 0.036(2) 0.033(2) 0.0091(18) -0.0063(18) 0.0045(19) C7A 0.032(2) 0.030(2) 0.035(2) -0.0008(16) -0.0055(16) 0.0005(15) C8A 0.0251(17) 0.0214(17) 0.0275(17) 0.0015(14) -0.0076(14) -0.0070(13) C9A 0.0289(19) 0.029(2) 0.0275(18) -0.0016(15) -0.0080(14) -0.0032(15) C10A 0.034(2) 0.035(2) 0.0268(18) -0.0058(16) -0.0039(15) -0.0053(16) C11A 0.033(2) 0.028(2) 0.040(2) -0.0044(17) -0.0025(17) -0.0012(15) C12A 0.038(2) 0.031(2) 0.041(2) -0.0020(17) -0.0113(17) 0.0032(16) C13A 0.039(2) 0.029(2) 0.032(2) -0.0014(16) -0.0118(16) 0.0008(16) C14A 0.0240(17) 0.0270(19) 0.0305(18) -0.0026(15) -0.0079(14) -0.0068(14) C15A 0.037(2) 0.034(2) 0.035(2) 0.0020(17) -0.0066(17) -0.0089(17) C16A 0.038(2) 0.033(2) 0.051(3) 0.0103(19) -0.0107(19) -0.0074(17) C17A 0.038(2) 0.023(2) 0.066(3) -0.0035(19) -0.016(2) -0.0052(16) C18A 0.055(3) 0.035(2) 0.046(2) -0.013(2) -0.017(2) -0.0028(19) C19A 0.049(2) 0.031(2) 0.033(2) -0.0013(17) -0.0134(18) -0.0087(18) C20A 0.0287(18) 0.0293(19) 0.0269(18) -0.0093(15) -0.0039(14) -0.0017(15) C21A 0.028(2) 0.044(2) 0.039(2) -0.0045(18) -0.0060(16) -0.0045(17) C22A 0.026(2) 0.059(3) 0.053(3) -0.012(2) -0.0103(19) 0.0012(19) C23A 0.039(2) 0.055(3) 0.048(3) -0.018(2) -0.022(2) 0.015(2) C24A 0.055(3) 0.048(3) 0.033(2) -0.0019(19) -0.012(2) 0.006(2) C25A 0.036(2) 0.043(2) 0.030(2) -0.0024(17) -0.0054(16) -0.0026(17) Li1A 0.035(4) 0.046(4) 0.031(3) -0.008(3) 0.003(3) -0.017(3) O1A 0.054(2) 0.051(2) 0.0421(17) 0.0059(15) -0.0002(15) -0.0035(15) O2A 0.0354(16) 0.057(2) 0.0401(16) -0.0033(14) 0.0076(13) -0.0148(14) O3A 0.0324(15) 0.0403(16) 0.0436(16) -0.0110(13) -0.0063(12) -0.0048(12) O4A 0.0492(17) 0.0349(16) 0.0349(15) -0.0014(12) -0.0081(13) -0.0091(13) O5A 0.0360(15) 0.0444(17) 0.0273(13) -0.0090(12) 0.0048(11) -0.0128(12) O6A 0.0260(13) 0.0433(16) 0.0278(13) -0.0044(12) -0.0015(10) -0.0082(11) C26A 0.072(4) 0.052(3) 0.078(4) 0.007(3) -0.013(3) 0.013(3) C27A 0.081(4) 0.047(3) 0.047(3) 0.009(2) 0.001(3) -0.013(3) C28A 0.066(3) 0.068(4) 0.047(3) 0.001(3) 0.015(2) -0.033(3) C29A 0.031(2) 0.104(5) 0.046(3) 0.001(3) 0.002(2) -0.011(3) C30A 0.060(3) 0.039(3) 0.090(4) -0.022(3) -0.024(3) -0.006(2) C31A 0.034(2) 0.051(3) 0.037(2) -0.0105(19) -0.0075(17) -0.0013(18) C32A 0.040(2) 0.052(3) 0.031(2) -0.0009(19) -0.0034(17) -0.0065(19) C33A 0.061(3) 0.037(3) 0.062(3) -0.002(2) -0.011(2) -0.007(2) C34A 0.043(3) 0.068(3) 0.037(2) -0.018(2) 0.0054(19) -0.009(2) C35A 0.030(2) 0.038(2) 0.039(2) -0.0036(18) 0.0007(16) -0.0108(16) C36A 0.030(2) 0.040(2) 0.040(2) -0.0055(18) -0.0082(17) -0.0065(16) C37A 0.041(2) 0.056(3) 0.0241(19) -0.0064(18) -0.0030(16) -0.0105(19) P1B 0.0282(5) 0.0373(6) 0.0286(5) 0.0037(4) -0.0063(4) -0.0075(4) P2B 0.0293(5) 0.0342(5) 0.0257(5) 0.0017(4) -0.0095(4) -0.0063(4) B1B 0.044(3) 0.099(5) 0.031(3) 0.006(3) 0.006(2) -0.010(3) B2B 0.038(3) 0.069(4) 0.046(3) 0.011(3) -0.007(2) -0.024(3) C1B 0.0280(19) 0.047(2) 0.0220(18) -0.0060(16) -0.0021(15) -0.0063(16) C2B 0.032(2) 0.035(2) 0.0298(19) -0.0044(16) -0.0049(15) -0.0039(16) C3B 0.039(2) 0.040(2) 0.033(2) 0.0008(17) -0.0089(17) -0.0088(18) C4B 0.063(3) 0.044(3) 0.041(2) 0.008(2) -0.020(2) -0.007(2) C5B 0.055(3) 0.051(3) 0.062(3) -0.001(2) -0.031(2) 0.005(2) C6B 0.034(2) 0.073(4) 0.072(4) 0.002(3) -0.019(2) -0.005(2) C7B 0.031(2) 0.060(3) 0.050(3) 0.005(2) -0.0087(19) -0.010(2) C8B 0.034(2) 0.037(2) 0.079(4) 0.003(2) -0.027(2) -0.0069(18) C9B 0.058(3) 0.042(3) 0.124(6) 0.031(3) -0.022(3) -0.012(2) C13B 0.083(4) 0.046(3) 0.099(5) -0.026(3) -0.044(4) 0.006(3) C14B 0.038(2) 0.027(2) 0.033(2) 0.0042(16) -0.0119(16) -0.0088(16) C15B 0.086(4) 0.046(3) 0.071(4) -0.020(3) -0.054(3) 0.021(3) C16B 0.089(4) 0.050(3) 0.087(4) -0.028(3) -0.057(4) 0.029(3) C17B 0.066(3) 0.030(2) 0.060(3) -0.010(2) -0.021(2) 0.007(2) C18B 0.060(3) 0.043(3) 0.040(2) -0.008(2) -0.014(2) -0.001(2) C19B 0.043(2) 0.048(3) 0.037(2) -0.0032(19) -0.0158(19) -0.0001(19) C20B 0.041(2) 0.034(2) 0.033(2) -0.0067(17) -0.0143(17) 0.0044(17) C21B 0.042(2) 0.055(3) 0.036(2) 0.006(2) -0.0057(19) 0.007(2) C22B 0.066(3) 0.058(3) 0.036(2) 0.008(2) -0.006(2) 0.018(3) C23B 0.070(3) 0.057(3) 0.044(3) -0.013(2) -0.032(2) 0.024(3) C24B 0.075(4) 0.061(4) 0.074(4) -0.009(3) -0.054(3) 0.003(3) C25B 0.058(3) 0.048(3) 0.066(3) -0.003(2) -0.038(3) -0.006(2) Li1B 0.038(4) 0.060(5) 0.038(4) -0.018(4) 0.001(3) -0.005(3) O1B 0.100(3) 0.055(2) 0.089(3) -0.001(2) -0.047(3) -0.024(2) O2B 0.086(3) 0.055(3) 0.227(7) -0.005(3) -0.075(4) 0.001(2) O3B 0.046(2) 0.221(6) 0.051(2) -0.056(3) 0.0083(18) -0.026(3) O4B 0.061(2) 0.134(4) 0.048(2) -0.023(2) -0.0089(18) -0.045(2) O5B 0.127(4) 0.100(4) 0.089(3) -0.041(3) 0.062(3) -0.046(3) C26B 0.077(4) 0.131(6) 0.056(4) -0.017(4) -0.023(3) -0.007(4) C32B 0.125(7) 0.134(7) 0.056(4) -0.024(4) 0.003(4) -0.055(5) C33B 0.046(4) 0.098(6) 0.178(9) -0.026(6) -0.001(4) -0.016(3) _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 P1A C1A 1.704(4) . ? P1A C8A 1.833(4) . ? P1A C2A 1.839(4) . ? P1A B1A 1.934(4) . ? P2A C1A 1.725(4) . ? P2A C14A 1.834(4) . ? P2A C20A 1.840(4) . ? P2A B2A 1.937(4) . ? B1A H1B1 0.9800 . ? B1A H2B1 0.9800 . ? B1A H3B1 0.9800 . ? B2A H1B2 0.9800 . ? B2A H2B2 0.9800 . ? B2A H3B2 0.9800 . ? C1A H1A 0.84(4) . ? C2A C7A 1.381(5) . ? C2A C3A 1.396(5) . ? C3A C4A 1.393(5) . ? C3A H3AA 0.9500 . ? C4A C5A 1.374(7) . ? C4A H4AA 0.9500 . ? C5A C6A 1.387(7) . ? C5A H5AA 0.9500 . ? C6A C7A 1.392(5) . ? C6A H6AA 0.9500 . ? C7A H7AA 0.9500 . ? C8A C9A 1.384(5) . ? C8A C13A 1.402(5) . ? C9A C10A 1.393(5) . ? C9A H9AA 0.9500 . ? C10A C11A 1.383(5) . ? C10A H10A 0.9500 . ? C11A C12A 1.379(6) . ? C11A H11A 0.9500 . ? C12A C13A 1.389(5) . ? C12A H12A 0.9500 . ? C13A H13A 0.9500 . ? C14A C15A 1.379(5) . ? C14A C19A 1.386(5) . ? C15A C16A 1.381(6) . ? C15A H15A 0.9500 . ? C16A C17A 1.388(6) . ? C16A H16A 0.9500 . ? C17A C18A 1.380(6) . ? C17A H17A 0.9500 . ? C18A C19A 1.396(6) . ? C18A H18A 0.9500 . ? C19A H19A 0.9500 . ? C20A C25A 1.385(6) . ? C20A C21A 1.399(5) . ? C21A C22A 1.383(6) . ? C21A H21A 0.9500 . ? C22A C23A 1.382(7) . ? C22A H22B 0.9500 . ? C23A C24A 1.384(7) . ? C23A H23A 0.9500 . ? C24A C25A 1.391(6) . ? C24A H24A 0.9500 . ? C25A H25A 0.9500 . ? Li1A O2A 2.045(7) . ? Li1A O5A 2.068(7) . ? Li1A O3A 2.131(7) . ? Li1A O6A 2.145(7) . ? Li1A O1A 2.214(8) . ? Li1A O4A 2.244(8) . ? O1A C27A 1.418(6) . ? O1A C26A 1.427(6) . ? O2A C28A 1.413(6) . ? O2A C29A 1.428(6) . ? O3A C30A 1.420(6) . ? O3A C31A 1.422(5) . ? O4A C32A 1.414(5) . ? O4A C33A 1.430(5) . ? O5A C34A 1.418(5) . ? O5A C35A 1.428(5) . ? O6A C36A 1.416(5) . ? O6A C37A 1.430(4) . ? C26A H26A 0.9800 . ? C26A H26B 0.9800 . ? C26A H26F 0.9800 . ? C27A C28A 1.491(8) . ? C27A H27A 0.9900 . ? C27A H27B 0.9900 . ? C28A H28A 0.9900 . ? C28A H28D 0.9900 . ? C29A H29A 0.9800 . ? C29A H29E 0.9800 . ? C29A H29F 0.9800 . ? C30A H30A 0.9800 . ? C30A H30E 0.9800 . ? C30A H30F 0.9800 . ? C31A C32A 1.496(6) . ? C31A H31A 0.9900 . ? C31A H31D 0.9900 . ? C32A H32A 0.9900 . ? C32A H32D 0.9900 . ? C33A H33D 0.9800 . ? C33A H33E 0.9800 . ? C33A H33F 0.9800 . ? C34A H34A 0.9800 . ? C34A H34B 0.9800 . ? C34A H34C 0.9800 . ? C35A C36A 1.489(6) . ? C35A H35A 0.9900 . ? C35A H35B 0.9900 . ? C36A H36A 0.9900 . ? C36A H36B 0.9900 . ? C37A H37A 0.9800 . ? C37A H37B 0.9800 . ? C37A H37C 0.9800 . ? P1B C1B 1.717(4) . ? P1B C8B 1.830(5) . ? P1B C2B 1.838(4) . ? P1B B1B 1.941(5) . ? P2B C1B 1.714(4) . ? P2B C14B 1.834(4) . ? P2B C20B 1.836(4) . ? P2B B2B 1.929(5) . ? B1B H1B3 0.9800 . ? B1B H2B3 0.9800 . ? B1B H3B3 0.9800 . ? B2B H1B4 0.9800 . ? B2B H2B4 0.9800 . ? B2B H3B4 0.9800 . ? C1B H1B 0.93(5) . ? C2B C7B 1.386(6) . ? C2B C3B 1.389(6) . ? C3B C4B 1.387(6) . ? C3B H3BA 0.9500 . ? C4B C5B 1.377(7) . ? C4B H4BA 0.9500 . ? C5B C6B 1.368(8) . ? C5B H5BA 0.9500 . ? C6B C7B 1.386(6) . ? C6B H6BA 0.9500 . ? C7B H7BA 0.9500 . ? C8B C13B 1.360(8) . ? C8B C9B 1.385(7) . ? C9B C10B 1.247(13) . ? C9B C10C 1.559(14) . ? C9B H9BA 0.9500 . ? C9B H9C 0.9501 . ? C10B C11B 1.422(16) . ? C10B H10B 0.9500 . ? C11B C12B 1.396(17) . ? C11B H11B 0.9500 . ? C12B C13B 1.463(13) . ? C12B H12B 0.9500 . ? C10C C11C 1.393(17) . ? C10C H10C 0.9500 . ? C11C C12C 1.396(19) . ? C11C H11C 0.9500 . ? C12C C13B 1.408(14) . ? C12C H12C 0.9500 . ? C13B H13B 0.9500 . ? C13B H13C 0.9500 . ? C14B C15B 1.377(6) . ? C14B C19B 1.381(6) . ? C15B C16B 1.385(7) . ? C15B H15B 0.9500 . ? C16B C17B 1.374(7) . ? C16B H16B 0.9500 . ? C17B C18B 1.363(6) . ? C17B H17B 0.9500 . ? C18B C19B 1.388(6) . ? C18B H18B 0.9500 . ? C19B H19B 0.9500 . ? C20B C21B 1.376(6) . ? C20B C25B 1.399(6) . ? C21B C22B 1.392(6) . ? C21B H21B 0.9500 . ? C22B C23B 1.373(8) . ? C22B H22A 0.9500 . ? C23B C24B 1.361(8) . ? C23B H23B 0.9500 . ? C24B C25B 1.391(7) . ? C24B H24B 0.9500 . ? C25B H25B 0.9500 . ? Li1B O3B 2.031(8) . ? Li1B O5B 2.034(8) . ? Li1B O4B 2.052(8) . ? Li1B O1B 2.079(8) . ? Li1B O2B 2.202(10) . ? Li1B O6B 2.350(11) . ? O1B C27B 1.353(10) . ? O1B C26B 1.376(7) . ? O2B C29B 1.339(10) . ? O2B C28B 1.377(12) . ? O3B C30B 1.299(12) . ? O3B C31B 1.423(14) . ? O4B C33B 1.376(7) . ? O4B C32B 1.385(7) . ? O5B C34B 1.334(12) . ? O5B C35B 1.440(17) . ? O6B C37B 1.332(13) . ? O6B C36B 1.417(16) . ? C26B H26C 0.9800 . ? C26B H26D 0.9800 . ? C26B H26E 0.9800 . ? C27B C28B 1.503(13) . ? C27B H27C 0.9900 . ? C27B H27D 0.9900 . ? C28B H28B 0.9900 . ? C28B H28C 0.9900 . ? C29B H29B 0.9800 . ? C29B H29C 0.9800 . ? C29B H29D 0.9800 . ? C30B H30B 0.9800 . ? C30B H30C 0.9800 . ? C30B H30D 0.9800 . ? C31B C32B 1.539(15) . ? C31B H31B 0.9900 . ? C31B H31C 0.9900 . ? C32B H32B 0.9900 . ? C32B H32C 0.9900 . ? C33B H33A 0.9800 . ? C33B H33B 0.9800 . ? C33B H33C 0.9800 . ? C34B C35B 1.92(2) . ? C34B H34D 0.9800 . ? C34B H34E 0.9800 . ? C34B H34F 0.9800 . ? C35B H35C 0.9900 . ? C35B H35D 0.9900 . ? C36B C37B 1.95(2) . ? C36B H36C 0.9900 . ? C36B H36D 0.9900 . ? C37B H37D 0.9800 . ? C37B H37E 0.9800 . ? C37B H37F 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 C1A P1A C8A 109.47(17) . . ? C1A P1A C2A 114.89(18) . . ? C8A P1A C2A 101.38(16) . . ? C1A P1A B1A 108.91(19) . . ? C8A P1A B1A 113.37(18) . . ? C2A P1A B1A 108.79(18) . . ? C1A P2A C14A 105.04(17) . . ? C1A P2A C20A 109.72(18) . . ? C14A P2A C20A 101.18(16) . . ? C1A P2A B2A 121.06(19) . . ? C14A P2A B2A 110.5(2) . . ? C20A P2A B2A 107.54(19) . . ? P1A B1A H1B1 109.5 . . ? P1A B1A H2B1 109.5 . . ? H1B1 B1A H2B1 109.5 . . ? P1A B1A H3B1 109.5 . . ? H1B1 B1A H3B1 109.5 . . ? H2B1 B1A H3B1 109.5 . . ? P2A B2A H1B2 109.5 . . ? P2A B2A H2B2 109.5 . . ? H1B2 B2A H2B2 109.5 . . ? P2A B2A H3B2 109.5 . . ? H1B2 B2A H3B2 109.5 . . ? H2B2 B2A H3B2 109.5 . . ? P1A C1A P2A 133.5(2) . . ? P1A C1A H1A 112(3) . . ? P2A C1A H1A 114(3) . . ? C7A C2A C3A 118.4(3) . . ? C7A C2A P1A 122.3(3) . . ? C3A C2A P1A 119.3(3) . . ? C4A C3A C2A 121.1(4) . . ? C4A C3A H3AA 119.4 . . ? C2A C3A H3AA 119.4 . . ? C5A C4A C3A 119.6(4) . . ? C5A C4A H4AA 120.2 . . ? C3A C4A H4AA 120.2 . . ? C4A C5A C6A 119.9(4) . . ? C4A C5A H5AA 120.0 . . ? C6A C5A H5AA 120.0 . . ? C5A C6A C7A 120.3(4) . . ? C5A C6A H6AA 119.9 . . ? C7A C6A H6AA 119.9 . . ? C2A C7A C6A 120.6(4) . . ? C2A C7A H7AA 119.7 . . ? C6A C7A H7AA 119.7 . . ? C9A C8A C13A 118.8(3) . . ? C9A C8A P1A 123.4(3) . . ? C13A C8A P1A 117.8(3) . . ? C8A C9A C10A 120.8(3) . . ? C8A C9A H9AA 119.6 . . ? C10A C9A H9AA 119.6 . . ? C11A C10A C9A 120.0(4) . . ? C11A C10A H10A 120.0 . . ? C9A C10A H10A 120.0 . . ? C12A C11A C10A 119.9(4) . . ? C12A C11A H11A 120.0 . . ? C10A C11A H11A 120.0 . . ? C11A C12A C13A 120.4(4) . . ? C11A C12A H12A 119.8 . . ? C13A C12A H12A 119.8 . . ? C12A C13A C8A 120.2(4) . . ? C12A C13A H13A 119.9 . . ? C8A C13A H13A 119.9 . . ? C15A C14A C19A 118.9(4) . . ? C15A C14A P2A 120.2(3) . . ? C19A C14A P2A 120.6(3) . . ? C14A C15A C16A 120.8(4) . . ? C14A C15A H15A 119.6 . . ? C16A C15A H15A 119.6 . . ? C15A C16A C17A 120.3(4) . . ? C15A C16A H16A 119.9 . . ? C17A C16A H16A 119.9 . . ? C18A C17A C16A 119.5(4) . . ? C18A C17A H17A 120.2 . . ? C16A C17A H17A 120.2 . . ? C17A C18A C19A 119.8(4) . . ? C17A C18A H18A 120.1 . . ? C19A C18A H18A 120.1 . . ? C14A C19A C18A 120.6(4) . . ? C14A C19A H19A 119.7 . . ? C18A C19A H19A 119.7 . . ? C25A C20A C21A 118.4(4) . . ? C25A C20A P2A 121.3(3) . . ? C21A C20A P2A 120.2(3) . . ? C22A C21A C20A 120.8(4) . . ? C22A C21A H21A 119.6 . . ? C20A C21A H21A 119.6 . . ? C23A C22A C21A 120.3(4) . . ? C23A C22A H22B 119.9 . . ? C21A C22A H22B 119.9 . . ? C22A C23A C24A 119.6(4) . . ? C22A C23A H23A 120.2 . . ? C24A C23A H23A 120.2 . . ? C23A C24A C25A 120.1(4) . . ? C23A C24A H24A 119.9 . . ? C25A C24A H24A 119.9 . . ? C20A C25A C24A 120.8(4) . . ? C20A C25A H25A 119.6 . . ? C24A C25A H25A 119.6 . . ? O2A Li1A O5A 162.1(4) . . ? O2A Li1A O3A 100.1(3) . . ? O5A Li1A O3A 93.6(3) . . ? O2A Li1A O6A 90.8(3) . . ? O5A Li1A O6A 78.8(2) . . ? O3A Li1A O6A 162.7(4) . . ? O2A Li1A O1A 76.2(3) . . ? O5A Li1A O1A 91.7(3) . . ? O3A Li1A O1A 93.1(3) . . ? O6A Li1A O1A 102.5(3) . . ? O2A Li1A O4A 95.4(3) . . ? O5A Li1A O4A 99.1(3) . . ? O3A Li1A O4A 75.8(3) . . ? O6A Li1A O4A 90.0(3) . . ? O1A Li1A O4A 164.9(4) . . ? C27A O1A C26A 113.2(4) . . ? C27A O1A Li1A 110.3(3) . . ? C26A O1A Li1A 127.0(4) . . ? C28A O2A C29A 113.2(4) . . ? C28A O2A Li1A 116.7(3) . . ? C29A O2A Li1A 124.9(4) . . ? C30A O3A C31A 111.3(3) . . ? C30A O3A Li1A 123.8(4) . . ? C31A O3A Li1A 115.0(3) . . ? C32A O4A C33A 112.4(3) . . ? C32A O4A Li1A 106.8(3) . . ? C33A O4A Li1A 127.3(3) . . ? C34A O5A C35A 113.3(3) . . ? C34A O5A Li1A 128.5(3) . . ? C35A O5A Li1A 111.3(3) . . ? C36A O6A C37A 111.8(3) . . ? C36A O6A Li1A 108.8(3) . . ? C37A O6A Li1A 124.0(3) . . ? O1A C26A H26A 109.5 . . ? O1A C26A H26B 109.5 . . ? H26A C26A H26B 109.5 . . ? O1A C26A H26F 109.5 . . ? H26A C26A H26F 109.5 . . ? H26B C26A H26F 109.5 . . ? O1A C27A C28A 109.0(4) . . ? O1A C27A H27A 109.9 . . ? C28A C27A H27A 109.9 . . ? O1A C27A H27B 109.9 . . ? C28A C27A H27B 109.9 . . ? H27A C27A H27B 108.3 . . ? O2A C28A C27A 107.6(4) . . ? O2A C28A H28A 110.2 . . ? C27A C28A H28A 110.2 . . ? O2A C28A H28D 110.2 . . ? C27A C28A H28D 110.2 . . ? H28A C28A H28D 108.5 . . ? O2A C29A H29A 109.5 . . ? O2A C29A H29E 109.5 . . ? H29A C29A H29E 109.5 . . ? O2A C29A H29F 109.5 . . ? H29A C29A H29F 109.5 . . ? H29E C29A H29F 109.5 . . ? O3A C30A H30A 109.5 . . ? O3A C30A H30E 109.5 . . ? H30A C30A H30E 109.5 . . ? O3A C30A H30F 109.5 . . ? H30A C30A H30F 109.5 . . ? H30E C30A H30F 109.5 . . ? O3A C31A C32A 108.6(3) . . ? O3A C31A H31A 110.0 . . ? C32A C31A H31A 110.0 . . ? O3A C31A H31D 110.0 . . ? C32A C31A H31D 110.0 . . ? H31A C31A H31D 108.4 . . ? O4A C32A C31A 108.3(3) . . ? O4A C32A H32A 110.0 . . ? C31A C32A H32A 110.0 . . ? O4A C32A H32D 110.0 . . ? C31A C32A H32D 110.0 . . ? H32A C32A H32D 108.4 . . ? O4A C33A H33D 109.5 . . ? O4A C33A H33E 109.5 . . ? H33D C33A H33E 109.5 . . ? O4A C33A H33F 109.5 . . ? H33D C33A H33F 109.5 . . ? H33E C33A H33F 109.5 . . ? O5A C34A H34A 109.5 . . ? O5A C34A H34B 109.5 . . ? H34A C34A H34B 109.5 . . ? O5A C34A H34C 109.5 . . ? H34A C34A H34C 109.5 . . ? H34B C34A H34C 109.5 . . ? O5A C35A C36A 107.3(3) . . ? O5A C35A H35A 110.3 . . ? C36A C35A H35A 110.3 . . ? O5A C35A H35B 110.3 . . ? C36A C35A H35B 110.3 . . ? H35A C35A H35B 108.5 . . ? O6A C36A C35A 107.8(3) . . ? O6A C36A H36A 110.2 . . ? C35A C36A H36A 110.2 . . ? O6A C36A H36B 110.2 . . ? C35A C36A H36B 110.2 . . ? H36A C36A H36B 108.5 . . ? O6A C37A H37A 109.5 . . ? O6A C37A H37B 109.5 . . ? H37A C37A H37B 109.5 . . ? O6A C37A H37C 109.5 . . ? H37A C37A H37C 109.5 . . ? H37B C37A H37C 109.5 . . ? C1B P1B C8B 105.6(2) . . ? C1B P1B C2B 109.49(19) . . ? C8B P1B C2B 100.53(19) . . ? C1B P1B B1B 121.0(2) . . ? C8B P1B B1B 110.6(3) . . ? C2B P1B B1B 107.7(2) . . ? C1B P2B C14B 110.94(18) . . ? C1B P2B C20B 113.8(2) . . ? C14B P2B C20B 102.21(17) . . ? C1B P2B B2B 109.6(2) . . ? C14B P2B B2B 111.0(2) . . ? C20B P2B B2B 109.1(2) . . ? P1B B1B H1B3 109.5 . . ? P1B B1B H2B3 109.5 . . ? H1B3 B1B H2B3 109.5 . . ? P1B B1B H3B3 109.5 . . ? H1B3 B1B H3B3 109.5 . . ? H2B3 B1B H3B3 109.5 . . ? P2B B2B H1B4 109.5 . . ? P2B B2B H2B4 109.5 . . ? H1B4 B2B H2B4 109.5 . . ? P2B B2B H3B4 109.5 . . ? H1B4 B2B H3B4 109.5 . . ? H2B4 B2B H3B4 109.5 . . ? P2B C1B P1B 134.6(2) . . ? P2B C1B H1B 115(3) . . ? P1B C1B H1B 110(3) . . ? C7B C2B C3B 118.3(4) . . ? C7B C2B P1B 120.9(3) . . ? C3B C2B P1B 120.8(3) . . ? C4B C3B C2B 120.5(4) . . ? C4B C3B H3BA 119.7 . . ? C2B C3B H3BA 119.7 . . ? C5B C4B C3B 120.1(4) . . ? C5B C4B H4BA 120.0 . . ? C3B C4B H4BA 120.0 . . ? C6B C5B C4B 120.1(4) . . ? C6B C5B H5BA 119.9 . . ? C4B C5B H5BA 119.9 . . ? C5B C6B C7B 119.9(5) . . ? C5B C6B H6BA 120.0 . . ? C7B C6B H6BA 120.0 . . ? C2B C7B C6B 121.0(4) . . ? C2B C7B H7BA 119.5 . . ? C6B C7B H7BA 119.5 . . ? C13B C8B C9B 118.3(5) . . ? C13B C8B P1B 121.9(4) . . ? C9B C8B P1B 119.7(5) . . ? C10B C9B C8B 135.3(10) . . ? C10B C9B C10C 23.5(7) . . ? C8B C9B C10C 111.9(8) . . ? C10B C9B H9BA 112.3 . . ? C8B C9B H9BA 112.3 . . ? C10C C9B H9BA 135.7 . . ? C10B C9B H9C 100.2 . . ? C8B C9B H9C 124.5 . . ? C10C C9B H9C 123.6 . . ? H9BA C9B H9C 12.3 . . ? C9B C10B C11B 108.9(11) . . ? C9B C10B H10B 125.6 . . ? C11B C10B H10B 125.6 . . ? C12B C11B C10B 123.2(11) . . ? C12B C11B H11B 118.4 . . ? C10B C11B H11B 118.4 . . ? C11B C12B C13B 121.2(10) . . ? C11B C12B H12B 119.4 . . ? C13B C12B H12B 119.4 . . ? C11C C10C C9B 122.8(10) . . ? C11C C10C H10C 118.6 . . ? C9B C10C H10C 118.6 . . ? C10C C11C C12C 123.3(12) . . ? C10C C11C H11C 118.3 . . ? C12C C11C H11C 118.3 . . ? C11C C12C C13B 108.6(12) . . ? C11C C12C H12C 125.7 . . ? C13B C12C H12C 125.7 . . ? C8B C13B C12C 134.1(8) . . ? C8B C13B C12B 112.9(7) . . ? C12C C13B C12B 24.2(6) . . ? C8B C13B H13B 123.5 . . ? C12C C13B H13B 101.3 . . ? C12B C13B H13B 123.5 . . ? C8B C13B H13C 111.8 . . ? C12C C13B H13C 114.1 . . ? C12B C13B H13C 132.8 . . ? H13B C13B H13C 17.9 . . ? C15B C14B C19B 117.7(4) . . ? C15B C14B P2B 118.8(3) . . ? C19B C14B P2B 123.4(3) . . ? C14B C15B C16B 120.9(4) . . ? C14B C15B H15B 119.6 . . ? C16B C15B H15B 119.6 . . ? C17B C16B C15B 120.5(5) . . ? C17B C16B H16B 119.7 . . ? C15B C16B H16B 119.7 . . ? C18B C17B C16B 119.4(4) . . ? C18B C17B H17B 120.3 . . ? C16B C17B H17B 120.3 . . ? C17B C18B C19B 120.0(4) . . ? C17B C18B H18B 120.0 . . ? C19B C18B H18B 120.0 . . ? C14B C19B C18B 121.4(4) . . ? C14B C19B H19B 119.3 . . ? C18B C19B H19B 119.3 . . ? C21B C20B C25B 117.9(4) . . ? C21B C20B P2B 121.9(3) . . ? C25B C20B P2B 120.2(4) . . ? C20B C21B C22B 121.0(5) . . ? C20B C21B H21B 119.5 . . ? C22B C21B H21B 119.5 . . ? C23B C22B C21B 120.1(5) . . ? C23B C22B H22A 120.0 . . ? C21B C22B H22A 120.0 . . ? C24B C23B C22B 120.3(4) . . ? C24B C23B H23B 119.9 . . ? C22B C23B H23B 119.9 . . ? C23B C24B C25B 119.9(5) . . ? C23B C24B H24B 120.0 . . ? C25B C24B H24B 120.0 . . ? C24B C25B C20B 120.9(5) . . ? C24B C25B H25B 119.6 . . ? C20B C25B H25B 119.6 . . ? O3B Li1B O5B 164.6(5) . . ? O3B Li1B O4B 81.5(3) . . ? O5B Li1B O4B 86.9(4) . . ? O3B Li1B O1B 96.5(4) . . ? O5B Li1B O1B 96.0(4) . . ? O4B Li1B O1B 174.5(5) . . ? O3B Li1B O2B 92.9(4) . . ? O5B Li1B O2B 98.3(4) . . ? O4B Li1B O2B 96.1(4) . . ? O1B Li1B O2B 78.9(3) . . ? O3B Li1B O6B 90.6(4) . . ? O5B Li1B O6B 80.0(4) . . ? O4B Li1B O6B 92.9(4) . . ? O1B Li1B O6B 92.2(4) . . ? O2B Li1B O6B 170.7(4) . . ? C27B O1B C26B 114.2(6) . . ? C27B O1B Li1B 119.3(6) . . ? C26B O1B Li1B 126.0(5) . . ? C29B O2B C28B 116.4(7) . . ? C29B O2B Li1B 133.7(6) . . ? C28B O2B Li1B 108.4(6) . . ? C30B O3B C31B 111.9(9) . . ? C30B O3B Li1B 134.2(7) . . ? C31B O3B Li1B 111.8(7) . . ? C33B O4B C32B 116.4(6) . . ? C33B O4B Li1B 124.0(5) . . ? C32B O4B Li1B 118.9(4) . . ? C34B O5B C35B 87.6(9) . . ? C34B O5B Li1B 130.9(7) . . ? C35B O5B Li1B 121.7(9) . . ? C37B O6B C36B 90.5(10) . . ? C37B O6B Li1B 132.6(8) . . ? C36B O6B Li1B 108.3(8) . . ? O1B C26B H26C 109.5 . . ? O1B C26B H26D 109.5 . . ? H26C C26B H26D 109.5 . . ? O1B C26B H26E 109.5 . . ? H26C C26B H26E 109.5 . . ? H26D C26B H26E 109.5 . . ? O1B C27B C28B 111.2(8) . . ? O1B C27B H27C 109.4 . . ? C28B C27B H27C 109.4 . . ? O1B C27B H27D 109.4 . . ? C28B C27B H27D 109.4 . . ? H27C C27B H27D 108.0 . . ? O2B C28B C27B 121.9(9) . . ? O2B C28B H28B 106.9 . . ? C27B C28B H28B 106.9 . . ? O2B C28B H28C 106.9 . . ? C27B C28B H28C 106.9 . . ? H28B C28B H28C 106.7 . . ? O2B C29B H29B 109.5 . . ? O2B C29B H29C 109.5 . . ? H29B C29B H29C 109.5 . . ? O2B C29B H29D 109.5 . . ? H29B C29B H29D 109.5 . . ? H29C C29B H29D 109.5 . . ? O3B C30B H30B 109.5 . . ? O3B C30B H30C 109.5 . . ? H30B C30B H30C 109.5 . . ? O3B C30B H30D 109.5 . . ? H30B C30B H30D 109.5 . . ? H30C C30B H30D 109.5 . . ? O3B C31B C32B 118.8(10) . . ? O3B C31B H31B 107.6 . . ? C32B C31B H31B 107.6 . . ? O3B C31B H31C 107.6 . . ? C32B C31B H31C 107.6 . . ? H31B C31B H31C 107.1 . . ? O4B C32B C31B 107.9(7) . . ? O4B C32B H32B 110.1 . . ? C31B C32B H32B 110.1 . . ? O4B C32B H32C 110.1 . . ? C31B C32B H32C 110.1 . . ? H32B C32B H32C 108.4 . . ? O4B C33B H33A 109.5 . . ? O4B C33B H33B 109.5 . . ? H33A C33B H33B 109.5 . . ? O4B C33B H33C 109.5 . . ? H33A C33B H33C 109.5 . . ? H33B C33B H33C 109.5 . . ? O5B C34B C35B 48.5(7) . . ? O5B C34B H34D 109.5 . . ? C35B C34B H34D 75.6 . . ? O5B C34B H34E 109.5 . . ? C35B C34B H34E 155.8 . . ? H34D C34B H34E 109.5 . . ? O5B C34B H34F 109.5 . . ? C35B C34B H34F 90.0 . . ? H34D C34B H34F 109.5 . . ? H34E C34B H34F 109.5 . . ? O5B C35B C34B 43.9(6) . . ? O5B C35B H35C 119.1 . . ? C34B C35B H35C 119.1 . . ? O5B C35B H35D 119.1 . . ? C34B C35B H35D 119.1 . . ? H35C C35B H35D 116.7 . . ? O6B C36B C37B 43.0(6) . . ? O6B C36B H36C 119.2 . . ? C37B C36B H36C 119.2 . . ? O6B C36B H36D 119.2 . . ? C37B C36B H36D 119.2 . . ? H36C C36B H36D 116.8 . . ? O6B C37B C36B 46.5(7) . . ? O6B C37B H37D 109.5 . . ? C36B C37B H37D 86.5 . . ? O6B C37B H37E 109.5 . . ? C36B C37B H37E 155.6 . . ? H37D C37B H37E 109.5 . . ? O6B C37B H37F 109.5 . . ? C36B C37B H37F 80.7 . . ? H37D C37B H37F 109.5 . . ? H37E C37B H37F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C8A P1A C1A P2A -34.9(4) . . . . ? C2A P1A C1A P2A 78.3(3) . . . . ? B1A P1A C1A P2A -159.4(3) . . . . ? C14A P2A C1A P1A -135.2(3) . . . . ? C20A P2A C1A P1A 116.8(3) . . . . ? B2A P2A C1A P1A -9.3(4) . . . . ? C1A P1A C2A C7A -23.0(4) . . . . ? C8A P1A C2A C7A 94.9(3) . . . . ? B1A P1A C2A C7A -145.4(3) . . . . ? C1A P1A C2A C3A 158.1(3) . . . . ? C8A P1A C2A C3A -83.9(3) . . . . ? B1A P1A C2A C3A 35.8(4) . . . . ? C7A C2A C3A C4A -0.9(6) . . . . ? P1A C2A C3A C4A 178.0(3) . . . . ? C2A C3A C4A C5A 0.1(6) . . . . ? C3A C4A C5A C6A 0.2(6) . . . . ? C4A C5A C6A C7A 0.4(6) . . . . ? C3A C2A C7A C6A 1.5(6) . . . . ? P1A C2A C7A C6A -177.4(3) . . . . ? C5A C6A C7A C2A -1.3(6) . . . . ? C1A P1A C8A C9A 121.5(3) . . . . ? C2A P1A C8A C9A -0.3(3) . . . . ? B1A P1A C8A C9A -116.7(3) . . . . ? C1A P1A C8A C13A -56.7(3) . . . . ? C2A P1A C8A C13A -178.5(3) . . . . ? B1A P1A C8A C13A 65.1(3) . . . . ? C13A C8A C9A C10A 0.7(5) . . . . ? P1A C8A C9A C10A -177.5(3) . . . . ? C8A C9A C10A C11A 0.2(6) . . . . ? C9A C10A C11A C12A -0.4(6) . . . . ? C10A C11A C12A C13A -0.3(6) . . . . ? C11A C12A C13A C8A 1.3(6) . . . . ? C9A C8A C13A C12A -1.5(6) . . . . ? P1A C8A C13A C12A 176.9(3) . . . . ? C1A P2A C14A C15A 112.1(3) . . . . ? C20A P2A C14A C15A -133.8(3) . . . . ? B2A P2A C14A C15A -20.0(4) . . . . ? C1A P2A C14A C19A -61.5(3) . . . . ? C20A P2A C14A C19A 52.6(3) . . . . ? B2A P2A C14A C19A 166.3(3) . . . . ? C19A C14A C15A C16A -0.1(6) . . . . ? P2A C14A C15A C16A -173.8(3) . . . . ? C14A C15A C16A C17A 0.5(6) . . . . ? C15A C16A C17A C18A -0.2(6) . . . . ? C16A C17A C18A C19A -0.7(7) . . . . ? C15A C14A C19A C18A -0.8(6) . . . . ? P2A C14A C19A C18A 172.9(3) . . . . ? C17A C18A C19A C14A 1.2(7) . . . . ? C1A P2A C20A C25A -15.0(4) . . . . ? C14A P2A C20A C25A -125.6(3) . . . . ? B2A P2A C20A C25A 118.4(3) . . . . ? C1A P2A C20A C21A 168.1(3) . . . . ? C14A P2A C20A C21A 57.5(3) . . . . ? B2A P2A C20A C21A -58.4(4) . . . . ? C25A C20A C21A C22A 0.2(6) . . . . ? P2A C20A C21A C22A 177.2(3) . . . . ? C20A C21A C22A C23A -0.9(6) . . . . ? C21A C22A C23A C24A 1.0(7) . . . . ? C22A C23A C24A C25A -0.5(7) . . . . ? C21A C20A C25A C24A 0.3(6) . . . . ? P2A C20A C25A C24A -176.6(3) . . . . ? C23A C24A C25A C20A -0.2(6) . . . . ? O2A Li1A O1A C27A 13.6(4) . . . . ? O5A Li1A O1A C27A -153.0(4) . . . . ? O3A Li1A O1A C27A 113.3(4) . . . . ? O6A Li1A O1A C27A -74.1(4) . . . . ? O4A Li1A O1A C27A 71.2(14) . . . . ? O2A Li1A O1A C26A 157.1(4) . . . . ? O5A Li1A O1A C26A -9.5(5) . . . . ? O3A Li1A O1A C26A -103.2(5) . . . . ? O6A Li1A O1A C26A 69.4(5) . . . . ? O4A Li1A O1A C26A -145.3(12) . . . . ? O5A Li1A O2A C28A 63.8(14) . . . . ? O3A Li1A O2A C28A -75.8(4) . . . . ? O6A Li1A O2A C28A 117.6(4) . . . . ? O1A Li1A O2A C28A 14.9(4) . . . . ? O4A Li1A O2A C28A -152.4(4) . . . . ? O5A Li1A O2A C29A -143.4(12) . . . . ? O3A Li1A O2A C29A 77.0(5) . . . . ? O6A Li1A O2A C29A -89.5(4) . . . . ? O1A Li1A O2A C29A 167.8(4) . . . . ? O4A Li1A O2A C29A 0.5(5) . . . . ? O2A Li1A O3A C30A 52.8(5) . . . . ? O5A Li1A O3A C30A -115.6(4) . . . . ? O6A Li1A O3A C30A -178.7(11) . . . . ? O1A Li1A O3A C30A -23.7(4) . . . . ? O4A Li1A O3A C30A 145.9(4) . . . . ? O2A Li1A O3A C31A -89.9(4) . . . . ? O5A Li1A O3A C31A 101.6(3) . . . . ? O6A Li1A O3A C31A 38.5(13) . . . . ? O1A Li1A O3A C31A -166.5(3) . . . . ? O4A Li1A O3A C31A 3.2(3) . . . . ? O2A Li1A O4A C32A 125.2(3) . . . . ? O5A Li1A O4A C32A -65.4(3) . . . . ? O3A Li1A O4A C32A 26.1(3) . . . . ? O6A Li1A O4A C32A -144.0(3) . . . . ? O1A Li1A O4A C32A 69.8(14) . . . . ? O2A Li1A O4A C33A -98.0(4) . . . . ? O5A Li1A O4A C33A 71.4(4) . . . . ? O3A Li1A O4A C33A 162.9(4) . . . . ? O6A Li1A O4A C33A -7.2(5) . . . . ? O1A Li1A O4A C33A -153.4(12) . . . . ? O2A Li1A O5A C34A -140.8(12) . . . . ? O3A Li1A O5A C34A -0.5(5) . . . . ? O6A Li1A O5A C34A 163.8(4) . . . . ? O1A Li1A O5A C34A -93.7(4) . . . . ? O4A Li1A O5A C34A 75.7(5) . . . . ? O2A Li1A O5A C35A 70.6(14) . . . . ? O3A Li1A O5A C35A -149.1(3) . . . . ? O6A Li1A O5A C35A 15.2(3) . . . . ? O1A Li1A O5A C35A 117.7(3) . . . . ? O4A Li1A O5A C35A -72.9(3) . . . . ? O2A Li1A O6A C36A -149.4(3) . . . . ? O5A Li1A O6A C36A 15.9(3) . . . . ? O3A Li1A O6A C36A 81.0(13) . . . . ? O1A Li1A O6A C36A -73.4(3) . . . . ? O4A Li1A O6A C36A 115.1(3) . . . . ? O2A Li1A O6A C37A -14.7(5) . . . . ? O5A Li1A O6A C37A 150.7(3) . . . . ? O3A Li1A O6A C37A -144.2(12) . . . . ? O1A Li1A O6A C37A 61.4(4) . . . . ? O4A Li1A O6A C37A -110.1(3) . . . . ? C26A O1A C27A C28A 173.6(5) . . . . ? Li1A O1A C27A C28A -37.5(5) . . . . ? C29A O2A C28A C27A 164.8(4) . . . . ? Li1A O2A C28A C27A -39.2(5) . . . . ? O1A C27A C28A O2A 49.4(6) . . . . ? C30A O3A C31A C32A -177.9(4) . . . . ? Li1A O3A C31A C32A -30.5(4) . . . . ? C33A O4A C32A C31A 165.9(4) . . . . ? Li1A O4A C32A C31A -50.2(4) . . . . ? O3A C31A C32A O4A 54.4(4) . . . . ? C34A O5A C35A C36A 164.0(4) . . . . ? Li1A O5A C35A C36A -42.4(4) . . . . ? C37A O6A C36A C35A 176.6(3) . . . . ? Li1A O6A C36A C35A -42.8(4) . . . . ? O5A C35A C36A O6A 56.7(4) . . . . ? C14B P2B C1B P1B -35.7(4) . . . . ? C20B P2B C1B P1B 78.8(4) . . . . ? B2B P2B C1B P1B -158.7(4) . . . . ? C8B P1B C1B P2B -137.5(4) . . . . ? C2B P1B C1B P2B 115.0(3) . . . . ? B1B P1B C1B P2B -11.0(5) . . . . ? C1B P1B C2B C7B 177.8(4) . . . . ? C8B P1B C2B C7B 66.9(4) . . . . ? B1B P1B C2B C7B -48.9(4) . . . . ? C1B P1B C2B C3B -3.4(4) . . . . ? C8B P1B C2B C3B -114.3(4) . . . . ? B1B P1B C2B C3B 129.9(4) . . . . ? C7B C2B C3B C4B -0.1(6) . . . . ? P1B C2B C3B C4B -178.9(3) . . . . ? C2B C3B C4B C5B 0.1(7) . . . . ? C3B C4B C5B C6B -0.3(8) . . . . ? C4B C5B C6B C7B 0.5(8) . . . . ? C3B C2B C7B C6B 0.3(7) . . . . ? P1B C2B C7B C6B 179.1(4) . . . . ? C5B C6B C7B C2B -0.5(8) . . . . ? C1B P1B C8B C13B -70.3(5) . . . . ? C2B P1B C8B C13B 43.5(5) . . . . ? B1B P1B C8B C13B 157.1(4) . . . . ? C1B P1B C8B C9B 105.1(4) . . . . ? C2B P1B C8B C9B -141.1(4) . . . . ? B1B P1B C8B C9B -27.5(5) . . . . ? C13B C8B C9B C10B -0.9(12) . . . . ? P1B C8B C9B C10B -176.5(9) . . . . ? C13B C8B C9B C10C 1.4(8) . . . . ? P1B C8B C9B C10C -174.2(5) . . . . ? C8B C9B C10B C11B -1.6(15) . . . . ? C10C C9B C10B C11B -6.9(15) . . . . ? C9B C10B C11B C12B 0.4(15) . . . . ? C10B C11B C12B C13B 3.0(16) . . . . ? C10B C9B C10C C11C 178(3) . . . . ? C8B C9B C10C C11C 1.8(12) . . . . ? C9B C10C C11C C12C 2.1(17) . . . . ? C10C C11C C12C C13B -7.8(16) . . . . ? C9B C8B C13B C12C -10.1(12) . . . . ? P1B C8B C13B C12C 165.3(9) . . . . ? C9B C8B C13B C12B 4.1(8) . . . . ? P1B C8B C13B C12B 179.6(6) . . . . ? C11C C12C C13B C8B 13.0(16) . . . . ? C11C C12C C13B C12B -20.5(15) . . . . ? C11B C12B C13B C8B -5.1(13) . . . . ? C11B C12B C13B C12C 149(3) . . . . ? C1B P2B C14B C15B -43.7(5) . . . . ? C20B P2B C14B C15B -165.3(4) . . . . ? B2B P2B C14B C15B 78.5(4) . . . . ? C1B P2B C14B C19B 139.5(4) . . . . ? C20B P2B C14B C19B 17.8(4) . . . . ? B2B P2B C14B C19B -98.4(4) . . . . ? C19B C14B C15B C16B -1.3(9) . . . . ? P2B C14B C15B C16B -178.4(5) . . . . ? C14B C15B C16B C17B -0.6(11) . . . . ? C15B C16B C17B C18B 2.6(10) . . . . ? C16B C17B C18B C19B -2.6(8) . . . . ? C15B C14B C19B C18B 1.3(7) . . . . ? P2B C14B C19B C18B 178.1(4) . . . . ? C17B C18B C19B C14B 0.7(8) . . . . ? C1B P2B C20B C21B -32.0(4) . . . . ? C14B P2B C20B C21B 87.7(4) . . . . ? B2B P2B C20B C21B -154.7(4) . . . . ? C1B P2B C20B C25B 146.8(4) . . . . ? C14B P2B C20B C25B -93.5(4) . . . . ? B2B P2B C20B C25B 24.1(4) . . . . ? C25B C20B C21B C22B 0.9(7) . . . . ? P2B C20B C21B C22B 179.8(3) . . . . ? C20B C21B C22B C23B -1.0(7) . . . . ? C21B C22B C23B C24B 0.2(8) . . . . ? C22B C23B C24B C25B 0.5(8) . . . . ? C23B C24B C25B C20B -0.6(8) . . . . ? C21B C20B C25B C24B -0.2(7) . . . . ? P2B C20B C25B C24B -179.0(4) . . . . ? O3B Li1B O1B C27B 89.0(7) . . . . ? O5B Li1B O1B C27B -100.0(7) . . . . ? O4B Li1B O1B C27B 22(5) . . . . ? O2B Li1B O1B C27B -2.7(7) . . . . ? O6B Li1B O1B C27B 179.9(6) . . . . ? O3B Li1B O1B C26B -99.7(6) . . . . ? O5B Li1B O1B C26B 71.3(6) . . . . ? O4B Li1B O1B C26B -167(4) . . . . ? O2B Li1B O1B C26B 168.6(5) . . . . ? O6B Li1B O1B C26B -8.9(6) . . . . ? O3B Li1B O2B C29B 103.2(9) . . . . ? O5B Li1B O2B C29B -66.2(10) . . . . ? O4B Li1B O2B C29B 21.5(10) . . . . ? O1B Li1B O2B C29B -160.7(9) . . . . ? O6B Li1B O2B C29B -145(3) . . . . ? O3B Li1B O2B C28B -91.5(7) . . . . ? O5B Li1B O2B C28B 99.0(7) . . . . ? O4B Li1B O2B C28B -173.2(7) . . . . ? O1B Li1B O2B C28B 4.5(7) . . . . ? O6B Li1B O2B C28B 21(3) . . . . ? O5B Li1B O3B C30B -124.1(19) . . . . ? O4B Li1B O3B C30B -165.0(10) . . . . ? O1B Li1B O3B C30B 20.0(12) . . . . ? O2B Li1B O3B C30B 99.2(11) . . . . ? O6B Li1B O3B C30B -72.2(11) . . . . ? O5B Li1B O3B C31B 38(2) . . . . ? O4B Li1B O3B C31B -3.2(8) . . . . ? O1B Li1B O3B C31B -178.1(8) . . . . ? O2B Li1B O3B C31B -98.9(8) . . . . ? O6B Li1B O3B C31B 89.7(8) . . . . ? O3B Li1B O4B C33B -174.2(6) . . . . ? O5B Li1B O4B C33B 15.8(7) . . . . ? O1B Li1B O4B C33B -106(5) . . . . ? O2B Li1B O4B C33B -82.2(7) . . . . ? O6B Li1B O4B C33B 95.6(6) . . . . ? O3B Li1B O4B C32B -3.8(7) . . . . ? O5B Li1B O4B C32B -173.8(6) . . . . ? O1B Li1B O4B C32B 64(5) . . . . ? O2B Li1B O4B C32B 88.2(6) . . . . ? O6B Li1B O4B C32B -94.0(6) . . . . ? O3B Li1B O5B C34B -170.4(18) . . . . ? O4B Li1B O5B C34B -129.9(10) . . . . ? O1B Li1B O5B C34B 45.4(10) . . . . ? O2B Li1B O5B C34B -34.2(10) . . . . ? O6B Li1B O5B C34B 136.6(10) . . . . ? O3B Li1B O5B C35B 71(2) . . . . ? O4B Li1B O5B C35B 112.0(10) . . . . ? O1B Li1B O5B C35B -72.7(10) . . . . ? O2B Li1B O5B C35B -152.3(10) . . . . ? O6B Li1B O5B C35B 18.5(10) . . . . ? O3B Li1B O6B C37B -40.1(11) . . . . ? O5B Li1B O6B C37B 127.7(11) . . . . ? O4B Li1B O6B C37B 41.4(11) . . . . ? O1B Li1B O6B C37B -136.6(11) . . . . ? O2B Li1B O6B C37B -152(3) . . . . ? O3B Li1B O6B C36B -148.5(9) . . . . ? O5B Li1B O6B C36B 19.3(9) . . . . ? O4B Li1B O6B C36B -67.0(9) . . . . ? O1B Li1B O6B C36B 115.0(9) . . . . ? O2B Li1B O6B C36B 99(3) . . . . ? C26B O1B C27B C28B -172.0(7) . . . . ? Li1B O1B C27B C28B 0.3(11) . . . . ? C29B O2B C28B C27B 161.9(10) . . . . ? Li1B O2B C28B C27B -6.2(13) . . . . ? O1B C27B C28B O2B 4.3(15) . . . . ? C30B O3B C31B C32B 175.4(11) . . . . ? Li1B O3B C31B C32B 9.3(14) . . . . ? C33B O4B C32B C31B -179.9(8) . . . . ? Li1B O4B C32B C31B 8.9(11) . . . . ? O3B C31B C32B O4B -11.9(15) . . . . ? Li1B O5B C34B C35B -131.3(12) . . . . ? Li1B O5B C35B C34B 138.1(9) . . . . ? Li1B O6B C36B C37B 135.7(9) . . . . ? Li1B O6B C37B C36B -115.8(12) . . . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 1.642 _refine_diff_density_min -0.807 _refine_diff_density_rms 0.084 #=== END data_FO3550 _database_code_depnum_ccdc_archive 'CCDC 712113' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H62 B4 Ca O P4' _chemical_formula_sum 'C54 H62 B4 Ca O P4' _chemical_formula_weight 934.24 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' B B 0.0013 0.0007 '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' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall -P2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.4163(4) _cell_length_b 13.8646(4) _cell_length_c 28.3332(6) _cell_angle_alpha 90.00 _cell_angle_beta 101.003(2) _cell_angle_gamma 90.00 _cell_volume 5173.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 31260 _cell_measurement_theta_min 1.92 _cell_measurement_theta_max 27.44 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.199 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1976 _exptl_absorpt_coefficient_mu 0.282 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31260 _diffrn_reflns_av_R_equivalents 0.0644 _diffrn_reflns_av_sigmaI/netI 0.0664 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 27.44 _reflns_number_total 11746 _reflns_number_gt 7944 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0520P)^2^+5.6576P] 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 11746 _refine_ls_number_parameters 633 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0983 _refine_ls_R_factor_gt 0.0562 _refine_ls_wR_factor_ref 0.1457 _refine_ls_wR_factor_gt 0.1253 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ca1 Ca 0.25455(4) 0.22295(4) 0.794426(19) 0.02947(14) Uani 1 1 d . . . P1 P 0.02062(5) 0.28918(5) 0.74656(2) 0.02814(16) Uani 1 1 d . . . P2 P 0.19889(5) 0.38880(5) 0.70861(2) 0.02826(16) Uani 1 1 d . . . P3 P 0.30112(5) 0.26787(5) 0.94978(2) 0.02737(16) Uani 1 1 d . . . P4 P 0.47127(5) 0.36735(5) 0.90729(2) 0.02646(16) Uani 1 1 d . . . O1 O 0.32272(16) 0.06753(15) 0.78865(7) 0.0399(5) Uani 1 1 d . . . B1 B 0.0576(3) 0.1550(2) 0.75709(13) 0.0345(7) Uani 1 1 d . . . H1B1 H 0.094(2) 0.153(2) 0.7962(11) 0.038(8) Uiso 1 1 d . . . H2B1 H -0.010(3) 0.112(2) 0.7496(12) 0.053(10) Uiso 1 1 d . . . H3B1 H 0.112(2) 0.137(2) 0.7331(11) 0.039(8) Uiso 1 1 d . . . B2 B 0.2882(3) 0.2845(3) 0.70061(13) 0.0361(8) Uani 1 1 d . . . H1B2 H 0.241(3) 0.220(3) 0.6942(12) 0.059(10) Uiso 1 1 d . . . H2B2 H 0.343(2) 0.276(2) 0.7341(11) 0.045(9) Uiso 1 1 d . . . H3B2 H 0.325(2) 0.302(2) 0.6718(11) 0.042(8) Uiso 1 1 d . . . B3 B 0.2299(3) 0.2119(3) 0.89068(12) 0.0343(7) Uani 1 1 d . . . H1B3 H 0.279(3) 0.162(3) 0.8757(12) 0.057(10) Uiso 1 1 d . . . H2B3 H 0.166(3) 0.169(2) 0.8991(12) 0.054(10) Uiso 1 1 d . . . H3B3 H 0.197(2) 0.269(2) 0.8640(10) 0.034(8) Uiso 1 1 d . . . B4 B 0.4339(3) 0.3134(3) 0.84356(12) 0.0326(7) Uani 1 1 d . . . H1B4 H 0.362(2) 0.350(2) 0.8291(10) 0.039(8) Uiso 1 1 d . . . H2B4 H 0.493(2) 0.334(2) 0.8249(10) 0.040(8) Uiso 1 1 d . . . H3B4 H 0.424(2) 0.231(2) 0.8468(10) 0.038(8) Uiso 1 1 d . . . C1 C 0.1261(2) 0.3674(2) 0.75302(10) 0.0289(6) Uani 1 1 d . . . H1 H 0.109(2) 0.427(2) 0.7630(10) 0.028(7) Uiso 1 1 d . . . C2 C -0.0505(2) 0.3273(2) 0.79216(9) 0.0295(6) Uani 1 1 d . . . C3 C -0.0264(2) 0.4064(2) 0.82159(12) 0.0459(8) Uani 1 1 d . . . H3A H 0.0309 0.4447 0.8187 0.055 Uiso 1 1 calc R . . C4 C -0.0843(3) 0.4309(3) 0.85533(12) 0.0513(9) Uani 1 1 d . . . H4A H -0.0676 0.4868 0.8746 0.062 Uiso 1 1 calc R . . C5 C -0.1656(2) 0.3752(3) 0.86123(11) 0.0427(8) Uani 1 1 d . . . H5A H -0.2038 0.3907 0.8852 0.051 Uiso 1 1 calc R . . C6 C -0.1906(3) 0.2969(3) 0.83206(14) 0.0566(10) Uani 1 1 d . . . H6A H -0.2474 0.2585 0.8354 0.068 Uiso 1 1 calc R . . C7 C -0.1341(3) 0.2728(2) 0.79758(13) 0.0500(9) Uani 1 1 d . . . H7A H -0.1529 0.2184 0.7775 0.060 Uiso 1 1 calc R . . C8 C -0.0706(2) 0.3051(2) 0.69063(10) 0.0340(6) Uani 1 1 d . . . C9 C -0.1060(3) 0.2266(3) 0.66215(11) 0.0479(8) Uani 1 1 d . . . H9A H -0.0839 0.1635 0.6721 0.057 Uiso 1 1 calc R . . C10 C -0.1742(3) 0.2399(3) 0.61875(13) 0.0618(10) Uani 1 1 d . . . H10A H -0.1998 0.1858 0.5996 0.074 Uiso 1 1 calc R . . C11 C -0.2045(3) 0.3325(3) 0.60371(13) 0.0608(11) Uani 1 1 d . . . H11A H -0.2498 0.3417 0.5739 0.073 Uiso 1 1 calc R . . C12 C -0.1690(2) 0.4109(3) 0.63172(12) 0.0498(9) Uani 1 1 d . . . H12A H -0.1898 0.4742 0.6213 0.060 Uiso 1 1 calc R . . C13 C -0.1030(2) 0.3975(2) 0.67518(11) 0.0389(7) Uani 1 1 d . . . H13A H -0.0796 0.4517 0.6947 0.047 Uiso 1 1 calc R . . C14 C 0.1262(2) 0.4265(2) 0.65026(10) 0.0381(7) Uani 1 1 d . . . C15 C 0.1032(3) 0.3605(3) 0.61348(11) 0.0553(10) Uani 1 1 d . . . H15A H 0.1288 0.2966 0.6179 0.066 Uiso 1 1 calc R . . C16 C 0.0428(3) 0.3867(5) 0.56997(13) 0.0841(17) Uani 1 1 d . . . H16A H 0.0264 0.3406 0.5449 0.101 Uiso 1 1 calc R . . C17 C 0.0067(3) 0.4795(6) 0.56339(16) 0.100(2) Uani 1 1 d . . . H17A H -0.0355 0.4972 0.5338 0.120 Uiso 1 1 calc R . . C18 C 0.0312(3) 0.5472(4) 0.59936(18) 0.0829(16) Uani 1 1 d . . . H18A H 0.0080 0.6117 0.5942 0.099 Uiso 1 1 calc R . . C19 C 0.0904(3) 0.5203(3) 0.64344(14) 0.0557(10) Uani 1 1 d . . . H19A H 0.1061 0.5661 0.6687 0.067 Uiso 1 1 calc R . . C20 C 0.2744(2) 0.4956(2) 0.72865(10) 0.0309(6) Uani 1 1 d . . . C21 C 0.3318(2) 0.5359(2) 0.69786(12) 0.0440(8) Uani 1 1 d . . . H21A H 0.3302 0.5082 0.6671 0.053 Uiso 1 1 calc R . . C22 C 0.3916(3) 0.6165(2) 0.71166(13) 0.0504(9) Uani 1 1 d . . . H22A H 0.4298 0.6441 0.6901 0.061 Uiso 1 1 calc R . . C23 C 0.3960(2) 0.6567(2) 0.75645(13) 0.0467(8) Uani 1 1 d . . . H23A H 0.4377 0.7113 0.7660 0.056 Uiso 1 1 calc R . . C24 C 0.3395(2) 0.6171(2) 0.78736(12) 0.0448(8) Uani 1 1 d . . . H24A H 0.3417 0.6449 0.8182 0.054 Uiso 1 1 calc R . . C25 C 0.2793(2) 0.5368(2) 0.77359(10) 0.0361(7) Uani 1 1 d . . . H25A H 0.2409 0.5097 0.7952 0.043 Uiso 1 1 calc R . . C26 C 0.3965(2) 0.3497(2) 0.94919(10) 0.0322(6) Uani 1 1 d . . . H26 H 0.422(2) 0.375(2) 0.9789(12) 0.044(9) Uiso 1 1 d . . . C27 C 0.2073(2) 0.3227(2) 0.98039(10) 0.0300(6) Uani 1 1 d . . . C28 C 0.2349(2) 0.3490(2) 1.02827(11) 0.0429(7) Uani 1 1 d . . . H28A H 0.3035 0.3416 1.0443 0.052 Uiso 1 1 calc R . . C29 C 0.1639(3) 0.3861(3) 1.05326(12) 0.0514(9) Uani 1 1 d . . . H29A H 0.1841 0.4046 1.0860 0.062 Uiso 1 1 calc R . . C30 C 0.0649(3) 0.3960(3) 1.03061(13) 0.0539(9) Uani 1 1 d . . . H30A H 0.0156 0.4184 1.0480 0.065 Uiso 1 1 calc R . . C31 C 0.0365(2) 0.3733(3) 0.98248(13) 0.0503(9) Uani 1 1 d . . . H31A H -0.0315 0.3835 0.9664 0.060 Uiso 1 1 calc R . . C32 C 0.1073(2) 0.3356(2) 0.95735(11) 0.0402(7) Uani 1 1 d . . . H32A H 0.0871 0.3187 0.9244 0.048 Uiso 1 1 calc R . . C33 C 0.3445(2) 0.1702(2) 0.99240(10) 0.0350(7) Uani 1 1 d . . . C34 C 0.4467(2) 0.1500(2) 1.00623(11) 0.0396(7) Uani 1 1 d . . . H34A H 0.4948 0.1849 0.9924 0.047 Uiso 1 1 calc R . . C35 C 0.4799(3) 0.0786(3) 1.04048(12) 0.0532(9) Uani 1 1 d . . . H35A H 0.5503 0.0650 1.0496 0.064 Uiso 1 1 calc R . . C36 C 0.4112(4) 0.0285(3) 1.06080(14) 0.0664(11) Uani 1 1 d . . . H36A H 0.4339 -0.0207 1.0837 0.080 Uiso 1 1 calc R . . C37 C 0.3088(4) 0.0490(3) 1.04806(16) 0.0760(13) Uani 1 1 d . . . H37A H 0.2613 0.0158 1.0631 0.091 Uiso 1 1 calc R . . C38 C 0.2756(3) 0.1180(3) 1.01349(14) 0.0586(10) Uani 1 1 d . . . H38A H 0.2049 0.1300 1.0039 0.070 Uiso 1 1 calc R . . C39 C 0.6018(2) 0.3331(2) 0.93364(10) 0.0326(6) Uani 1 1 d . . . C40 C 0.6631(2) 0.3916(3) 0.96688(11) 0.0418(7) Uani 1 1 d . . . H40A H 0.6394 0.4538 0.9736 0.050 Uiso 1 1 calc R . . C41 C 0.7577(3) 0.3615(3) 0.99041(12) 0.0572(10) Uani 1 1 d . . . H41A H 0.7987 0.4030 1.0128 0.069 Uiso 1 1 calc R . . C42 C 0.7921(3) 0.2726(3) 0.98151(16) 0.0700(13) Uani 1 1 d . . . H42A H 0.8562 0.2511 0.9986 0.084 Uiso 1 1 calc R . . C43 C 0.7347(3) 0.2134(3) 0.9479(2) 0.0796(14) Uani 1 1 d . . . H43A H 0.7604 0.1524 0.9408 0.096 Uiso 1 1 calc R . . C44 C 0.6386(3) 0.2430(3) 0.92417(15) 0.0567(10) Uani 1 1 d . . . H44A H 0.5984 0.2014 0.9015 0.068 Uiso 1 1 calc R . . C45 C 0.4874(2) 0.4968(2) 0.89958(9) 0.0294(6) Uani 1 1 d . . . C46 C 0.4319(2) 0.5629(2) 0.92065(10) 0.0354(7) Uani 1 1 d . . . H46A H 0.3827 0.5412 0.9383 0.042 Uiso 1 1 calc R . . C47 C 0.4485(3) 0.6616(2) 0.91591(11) 0.0435(8) Uani 1 1 d . . . H47A H 0.4115 0.7071 0.9308 0.052 Uiso 1 1 calc R . . C48 C 0.5188(3) 0.6932(2) 0.88957(11) 0.0446(8) Uani 1 1 d . . . H48A H 0.5303 0.7604 0.8866 0.054 Uiso 1 1 calc R . . C49 C 0.5722(2) 0.6280(2) 0.86758(11) 0.0420(7) Uani 1 1 d . . . H49A H 0.6193 0.6502 0.8489 0.050 Uiso 1 1 calc R . . C50 C 0.5573(2) 0.5293(2) 0.87256(10) 0.0345(6) Uani 1 1 d . . . H50A H 0.5948 0.4844 0.8576 0.041 Uiso 1 1 calc R . . C51 C 0.3079(3) 0.0112(3) 0.74457(12) 0.0616(11) Uani 1 1 d . . . H51A H 0.3134 0.0529 0.7168 0.074 Uiso 1 1 calc R . . H51B H 0.2401 -0.0196 0.7385 0.074 Uiso 1 1 calc R . . C52 C 0.3893(3) -0.0631(3) 0.75187(13) 0.0549(9) Uani 1 1 d . . . H52A H 0.4528 -0.0377 0.7437 0.066 Uiso 1 1 calc R . . H52B H 0.3681 -0.1214 0.7324 0.066 Uiso 1 1 calc R . . C53 C 0.4020(3) -0.0841(3) 0.80453(13) 0.0565(9) Uani 1 1 d . . . H53A H 0.4711 -0.1086 0.8175 0.068 Uiso 1 1 calc R . . H53B H 0.3517 -0.1324 0.8108 0.068 Uiso 1 1 calc R . . C54 C 0.3847(3) 0.0115(2) 0.82647(11) 0.0418(7) Uani 1 1 d . . . H54A H 0.3492 0.0027 0.8538 0.050 Uiso 1 1 calc R . . H54B H 0.4502 0.0444 0.8383 0.050 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 Ca1 0.0303(3) 0.0285(3) 0.0283(3) -0.0023(2) 0.0020(2) 0.0019(2) P1 0.0281(4) 0.0284(4) 0.0272(3) -0.0036(3) 0.0034(3) 0.0001(3) P2 0.0297(4) 0.0291(4) 0.0263(3) -0.0004(3) 0.0063(3) 0.0038(3) P3 0.0271(4) 0.0287(4) 0.0273(3) -0.0004(3) 0.0076(3) -0.0041(3) P4 0.0257(4) 0.0278(4) 0.0261(3) 0.0007(3) 0.0056(3) -0.0037(3) O1 0.0455(13) 0.0331(11) 0.0374(11) -0.0045(9) -0.0015(9) 0.0091(10) B1 0.0350(19) 0.0268(17) 0.0401(19) -0.0043(14) 0.0036(15) -0.0016(14) B2 0.0389(19) 0.0326(18) 0.0391(18) -0.0004(15) 0.0133(15) 0.0102(16) B3 0.0358(18) 0.0364(19) 0.0317(16) -0.0070(14) 0.0088(14) -0.0084(15) B4 0.0344(18) 0.0340(18) 0.0302(16) -0.0025(14) 0.0082(14) -0.0080(15) C1 0.0296(14) 0.0278(15) 0.0296(14) -0.0031(11) 0.0062(11) 0.0019(12) C2 0.0278(14) 0.0328(15) 0.0276(13) 0.0000(11) 0.0048(11) 0.0006(12) C3 0.0402(18) 0.051(2) 0.0503(19) -0.0176(16) 0.0188(15) -0.0153(15) C4 0.048(2) 0.061(2) 0.0492(19) -0.0231(17) 0.0203(16) -0.0112(18) C5 0.0387(17) 0.057(2) 0.0343(16) -0.0004(15) 0.0121(13) 0.0057(16) C6 0.053(2) 0.053(2) 0.072(2) -0.0048(19) 0.0314(19) -0.0178(18) C7 0.053(2) 0.0430(19) 0.059(2) -0.0173(17) 0.0251(17) -0.0150(16) C8 0.0289(15) 0.0437(17) 0.0287(14) -0.0039(13) 0.0036(11) -0.0012(13) C9 0.052(2) 0.049(2) 0.0385(17) -0.0075(15) -0.0027(15) -0.0032(16) C10 0.064(2) 0.073(3) 0.0419(19) -0.0139(19) -0.0060(17) -0.008(2) C11 0.047(2) 0.093(3) 0.0376(18) 0.005(2) -0.0052(15) 0.001(2) C12 0.0348(18) 0.067(2) 0.0468(19) 0.0126(18) 0.0045(14) 0.0108(17) C13 0.0310(16) 0.0476(19) 0.0377(16) -0.0009(14) 0.0053(12) 0.0043(14) C14 0.0296(15) 0.056(2) 0.0299(15) 0.0076(14) 0.0090(12) 0.0071(14) C15 0.0417(19) 0.091(3) 0.0332(17) -0.0064(18) 0.0079(14) 0.0056(19) C16 0.044(2) 0.178(6) 0.0303(19) -0.005(3) 0.0051(16) 0.005(3) C17 0.046(2) 0.211(7) 0.044(2) 0.053(4) 0.0090(19) 0.030(3) C18 0.052(2) 0.123(4) 0.077(3) 0.065(3) 0.020(2) 0.034(3) C19 0.043(2) 0.067(3) 0.059(2) 0.0260(19) 0.0149(16) 0.0158(18) C20 0.0290(15) 0.0266(14) 0.0377(15) 0.0023(12) 0.0079(12) 0.0038(12) C21 0.0478(19) 0.0397(18) 0.0495(19) 0.0012(15) 0.0219(15) 0.0000(15) C22 0.051(2) 0.0415(19) 0.065(2) 0.0066(17) 0.0271(18) -0.0066(16) C23 0.0402(18) 0.0295(16) 0.071(2) 0.0038(16) 0.0111(16) -0.0038(14) C24 0.0451(19) 0.0408(18) 0.0463(18) -0.0035(15) 0.0029(15) -0.0027(15) C25 0.0364(16) 0.0353(16) 0.0369(16) 0.0026(13) 0.0075(13) -0.0003(13) C26 0.0331(15) 0.0380(16) 0.0270(14) -0.0037(12) 0.0095(12) -0.0118(13) C27 0.0276(14) 0.0314(15) 0.0330(14) -0.0011(12) 0.0105(11) -0.0029(12) C28 0.0361(17) 0.052(2) 0.0397(17) -0.0068(15) 0.0054(13) -0.0001(15) C29 0.049(2) 0.067(2) 0.0393(17) -0.0175(17) 0.0129(15) 0.0001(18) C30 0.043(2) 0.064(2) 0.060(2) -0.0115(19) 0.0246(17) 0.0044(18) C31 0.0288(16) 0.066(2) 0.057(2) -0.0053(18) 0.0099(15) 0.0028(16) C32 0.0339(16) 0.0494(19) 0.0374(16) -0.0022(14) 0.0071(13) 0.0001(14) C33 0.0450(18) 0.0260(15) 0.0351(15) 0.0009(12) 0.0101(13) 0.0001(13) C34 0.0436(18) 0.0333(16) 0.0411(16) -0.0004(13) 0.0065(14) 0.0033(14) C35 0.062(2) 0.042(2) 0.050(2) -0.0001(16) -0.0040(17) 0.0143(18) C36 0.097(3) 0.040(2) 0.060(2) 0.0168(18) 0.008(2) 0.009(2) C37 0.091(3) 0.058(3) 0.083(3) 0.031(2) 0.027(3) -0.006(2) C38 0.056(2) 0.051(2) 0.071(2) 0.0230(19) 0.0171(19) -0.0071(18) C39 0.0259(14) 0.0381(16) 0.0354(15) 0.0089(13) 0.0103(12) -0.0016(12) C40 0.0345(16) 0.056(2) 0.0352(16) -0.0009(14) 0.0081(13) -0.0015(15) C41 0.0345(18) 0.088(3) 0.0446(19) 0.0145(19) -0.0028(15) -0.006(2) C42 0.0320(19) 0.080(3) 0.092(3) 0.042(3) -0.0038(19) 0.000(2) C43 0.044(2) 0.043(2) 0.148(4) 0.024(3) 0.009(3) 0.0087(19) C44 0.0379(19) 0.0379(19) 0.091(3) 0.0032(18) 0.0026(18) -0.0009(15) C45 0.0310(15) 0.0286(14) 0.0270(13) 0.0011(11) 0.0018(11) -0.0036(12) C46 0.0368(16) 0.0339(16) 0.0346(15) -0.0002(13) 0.0049(12) -0.0014(13) C47 0.050(2) 0.0323(17) 0.0451(18) -0.0039(14) 0.0016(15) 0.0026(15) C48 0.055(2) 0.0298(16) 0.0438(18) 0.0039(14) -0.0036(15) -0.0071(15) C49 0.0449(18) 0.0414(18) 0.0380(16) 0.0060(14) 0.0033(14) -0.0148(15) C50 0.0383(17) 0.0345(16) 0.0304(14) 0.0029(12) 0.0059(12) -0.0066(13) C51 0.086(3) 0.046(2) 0.0445(19) -0.0160(16) -0.0070(18) 0.023(2) C52 0.069(2) 0.042(2) 0.054(2) -0.0085(16) 0.0131(18) 0.0100(18) C53 0.074(3) 0.0399(19) 0.056(2) 0.0061(16) 0.0131(19) 0.0196(18) C54 0.0481(19) 0.0392(18) 0.0382(16) 0.0056(14) 0.0087(14) 0.0072(15) _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 Ca1 O1 2.359(2) . ? Ca1 C1 2.754(3) . ? Ca1 B3 2.813(3) . ? Ca1 B1 2.815(4) . ? Ca1 B4 2.833(3) . ? Ca1 B2 2.908(4) . ? Ca1 P1 3.3028(9) . ? Ca1 P2 3.3262(9) . ? Ca1 H1B1 2.37(3) . ? Ca1 H3B1 2.62(3) . ? Ca1 H2B2 2.37(3) . ? Ca1 H1B3 2.41(3) . ? Ca1 H3B3 2.34(3) . ? Ca1 H1B4 2.37(3) . ? Ca1 H3B4 2.47(3) . ? P1 C1 1.764(3) . ? P1 C8 1.821(3) . ? P1 C2 1.825(3) . ? P1 B1 1.933(3) . ? P2 C1 1.759(3) . ? P2 C20 1.823(3) . ? P2 C14 1.828(3) . ? P2 B2 1.919(3) . ? P3 C26 1.712(3) . ? P3 C27 1.825(3) . ? P3 C33 1.834(3) . ? P3 B3 1.926(3) . ? P4 C26 1.712(3) . ? P4 C45 1.825(3) . ? P4 C39 1.830(3) . ? P4 B4 1.930(3) . ? O1 C54 1.450(4) . ? O1 C51 1.454(4) . ? B1 H1B1 1.12(3) . ? B1 H2B1 1.07(4) . ? B1 H3B1 1.11(3) . ? B2 H1B2 1.09(4) . ? B2 H2B2 1.09(3) . ? B2 H3B2 1.06(3) . ? B3 H1B3 1.09(4) . ? B3 H2B3 1.11(3) . ? B3 H3B3 1.13(3) . ? B4 H1B4 1.10(3) . ? B4 H2B4 1.07(3) . ? B4 H3B4 1.16(3) . ? C1 H1 0.92(3) . ? C2 C7 1.385(4) . ? C2 C3 1.378(4) . ? C3 C4 1.385(4) . ? C3 H3A 0.9500 . ? C4 C5 1.373(5) . ? C4 H4A 0.9500 . ? C5 C6 1.367(5) . ? C5 H5A 0.9500 . ? C6 C7 1.387(5) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 C9 1.384(4) . ? C8 C13 1.396(4) . ? C9 C10 1.398(5) . ? C9 H9A 0.9500 . ? C10 C11 1.388(6) . ? C10 H10A 0.9500 . ? C11 C12 1.377(5) . ? C11 H11A 0.9500 . ? C12 C13 1.385(4) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 C15 1.377(5) . ? C14 C19 1.387(5) . ? C15 C16 1.388(5) . ? C15 H15A 0.9500 . ? C16 C17 1.376(8) . ? C16 H16A 0.9500 . ? C17 C18 1.378(8) . ? C17 H17A 0.9500 . ? C18 C19 1.397(5) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 C25 1.385(4) . ? C20 C21 1.387(4) . ? C21 C22 1.387(5) . ? C21 H21A 0.9500 . ? C22 C23 1.377(5) . ? C22 H22A 0.9500 . ? C23 C24 1.377(5) . ? C23 H23A 0.9500 . ? C24 C25 1.387(4) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? C26 H26 0.92(3) . ? C27 C32 1.387(4) . ? C27 C28 1.385(4) . ? C28 C29 1.389(4) . ? C28 H28A 0.9500 . ? C29 C30 1.368(5) . ? C29 H29A 0.9500 . ? C30 C31 1.380(5) . ? C30 H30A 0.9500 . ? C31 C32 1.393(4) . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? C33 C34 1.381(4) . ? C33 C38 1.395(4) . ? C34 C35 1.397(4) . ? C34 H34A 0.9500 . ? C35 C36 1.367(6) . ? C35 H35A 0.9500 . ? C36 C37 1.382(6) . ? C36 H36A 0.9500 . ? C37 C38 1.380(5) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? C39 C40 1.388(4) . ? C39 C44 1.388(5) . ? C40 C41 1.381(5) . ? C40 H40A 0.9500 . ? C41 C42 1.357(6) . ? C41 H41A 0.9500 . ? C42 C43 1.377(6) . ? C42 H42A 0.9500 . ? C43 C44 1.396(5) . ? C43 H43A 0.9500 . ? C44 H44A 0.9500 . ? C45 C46 1.385(4) . ? C45 C50 1.395(4) . ? C46 C47 1.398(4) . ? C46 H46A 0.9500 . ? C47 C48 1.380(5) . ? C47 H47A 0.9500 . ? C48 C49 1.375(5) . ? C48 H48A 0.9500 . ? C49 C50 1.393(4) . ? C49 H49A 0.9500 . ? C50 H50A 0.9500 . ? C51 C52 1.487(5) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.498(5) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.501(5) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? 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 O1 Ca1 C1 148.66(8) . . ? O1 Ca1 B3 97.84(9) . . ? C1 Ca1 B3 105.83(10) . . ? O1 Ca1 B1 90.97(9) . . ? C1 Ca1 B1 67.48(9) . . ? B3 Ca1 B1 94.03(10) . . ? O1 Ca1 B4 97.71(9) . . ? C1 Ca1 B4 106.94(10) . . ? B3 Ca1 B4 78.10(10) . . ? B1 Ca1 B4 168.97(10) . . ? O1 Ca1 B2 94.28(8) . . ? C1 Ca1 B2 65.86(9) . . ? B3 Ca1 B2 165.84(11) . . ? B1 Ca1 B2 93.05(11) . . ? B4 Ca1 B2 93.07(10) . . ? O1 Ca1 P1 125.18(6) . . ? C1 Ca1 P1 32.28(6) . . ? B3 Ca1 P1 97.75(8) . . ? B1 Ca1 P1 35.73(7) . . ? B4 Ca1 P1 136.92(8) . . ? B2 Ca1 P1 81.04(7) . . ? O1 Ca1 P2 128.08(5) . . ? C1 Ca1 P2 31.89(6) . . ? B3 Ca1 P2 134.00(8) . . ? B1 Ca1 P2 83.85(7) . . ? B4 Ca1 P2 95.99(7) . . ? B2 Ca1 P2 35.05(7) . . ? P1 Ca1 P2 56.25(2) . . ? O1 Ca1 H1B1 89.6(7) . . ? C1 Ca1 H1B1 79.0(7) . . ? B3 Ca1 H1B1 71.4(7) . . ? B1 Ca1 H1B1 23.0(7) . . ? B4 Ca1 H1B1 149.4(7) . . ? B2 Ca1 H1B1 116.1(7) . . ? P1 Ca1 H1B1 47.7(7) . . ? P2 Ca1 H1B1 102.7(7) . . ? O1 Ca1 H3B1 77.3(7) . . ? C1 Ca1 H3B1 74.4(7) . . ? B3 Ca1 H3B1 114.3(7) . . ? B1 Ca1 H3B1 23.3(7) . . ? B4 Ca1 H3B1 167.0(7) . . ? B2 Ca1 H3B1 75.5(7) . . ? P1 Ca1 H3B1 48.4(7) . . ? P2 Ca1 H3B1 78.3(6) . . ? H1B1 Ca1 H3B1 43.5(9) . . ? O1 Ca1 H2B2 88.7(8) . . ? C1 Ca1 H2B2 80.1(8) . . ? B3 Ca1 H2B2 151.9(8) . . ? B1 Ca1 H2B2 113.2(8) . . ? B4 Ca1 H2B2 73.9(8) . . ? B2 Ca1 H2B2 20.8(8) . . ? P1 Ca1 H2B2 100.7(8) . . ? P2 Ca1 H2B2 48.3(8) . . ? H1B1 Ca1 H2B2 136.2(11) . . ? H3B1 Ca1 H2B2 93.8(10) . . ? O1 Ca1 H1B3 76.3(9) . . ? C1 Ca1 H1B3 128.3(9) . . ? B3 Ca1 H1B3 22.5(9) . . ? B1 Ca1 H1B3 101.0(8) . . ? B4 Ca1 H1B3 74.7(8) . . ? B2 Ca1 H1B3 163.2(8) . . ? P1 Ca1 H1B3 115.8(8) . . ? P2 Ca1 H1B3 155.3(9) . . ? H1B1 Ca1 H1B3 78.3(11) . . ? H3B1 Ca1 H1B3 115.1(10) . . ? H2B2 Ca1 H1B3 142.9(11) . . ? O1 Ca1 H3B3 120.2(7) . . ? C1 Ca1 H3B3 83.1(7) . . ? B3 Ca1 H3B3 23.0(7) . . ? B1 Ca1 H3B3 88.2(7) . . ? B4 Ca1 H3B3 81.6(7) . . ? B2 Ca1 H3B3 145.5(7) . . ? P1 Ca1 H3B3 80.1(7) . . ? P2 Ca1 H3B3 111.3(7) . . ? H1B1 Ca1 H3B3 69.2(10) . . ? H3B1 Ca1 H3B3 111.4(10) . . ? H2B2 Ca1 H3B3 144.5(11) . . ? H1B3 Ca1 H3B3 45.5(11) . . ? O1 Ca1 H1B4 119.6(8) . . ? C1 Ca1 H1B4 85.3(8) . . ? B3 Ca1 H1B4 79.2(7) . . ? B1 Ca1 H1B4 149.2(8) . . ? B4 Ca1 H1B4 22.1(8) . . ? B2 Ca1 H1B4 88.4(7) . . ? P1 Ca1 H1B4 114.8(8) . . ? P2 Ca1 H1B4 79.8(7) . . ? H1B1 Ca1 H1B4 141.2(10) . . ? H3B1 Ca1 H1B4 157.9(10) . . ? H2B2 Ca1 H1B4 73.8(10) . . ? H1B3 Ca1 H1B4 84.3(11) . . ? H3B3 Ca1 H1B4 73.9(10) . . ? O1 Ca1 H3B4 76.0(7) . . ? C1 Ca1 H3B4 130.8(7) . . ? B3 Ca1 H3B4 71.7(7) . . ? B1 Ca1 H3B4 158.7(7) . . ? B4 Ca1 H3B4 24.0(7) . . ? B2 Ca1 H3B4 104.5(7) . . ? P1 Ca1 H3B4 158.2(7) . . ? P2 Ca1 H3B4 117.4(7) . . ? H1B1 Ca1 H3B4 137.9(10) . . ? H3B1 Ca1 H3B4 153.2(10) . . ? H2B2 Ca1 H3B4 83.6(10) . . ? H1B3 Ca1 H3B4 60.0(11) . . ? H3B3 Ca1 H3B4 84.2(10) . . ? H1B4 Ca1 H3B4 45.5(10) . . ? C1 P1 C8 114.09(13) . . ? C1 P1 C2 105.43(13) . . ? C8 P1 C2 103.05(13) . . ? C1 P1 B1 113.46(15) . . ? C8 P1 B1 111.15(15) . . ? C2 P1 B1 108.82(14) . . ? C1 P1 Ca1 56.46(9) . . ? C8 P1 Ca1 144.97(9) . . ? C2 P1 Ca1 111.97(9) . . ? B1 P1 Ca1 58.23(11) . . ? C1 P2 C20 105.41(13) . . ? C1 P2 C14 114.99(13) . . ? C20 P2 C14 102.60(14) . . ? C1 P2 B2 113.68(15) . . ? C20 P2 B2 109.06(15) . . ? C14 P2 B2 110.23(15) . . ? C1 P2 Ca1 55.81(9) . . ? C20 P2 Ca1 107.46(9) . . ? C14 P2 Ca1 149.92(11) . . ? B2 P2 Ca1 60.48(11) . . ? C26 P3 C27 108.23(14) . . ? C26 P3 C33 110.62(15) . . ? C27 P3 C33 98.94(13) . . ? C26 P3 B3 120.42(14) . . ? C27 P3 B3 107.95(14) . . ? C33 P3 B3 108.51(15) . . ? C26 P4 C45 108.77(14) . . ? C26 P4 C39 108.78(14) . . ? C45 P4 C39 100.27(13) . . ? C26 P4 B4 120.75(15) . . ? C45 P4 B4 106.53(13) . . ? C39 P4 B4 109.76(15) . . ? C54 O1 C51 108.2(2) . . ? C54 O1 Ca1 127.82(17) . . ? C51 O1 Ca1 123.97(18) . . ? P1 B1 Ca1 86.03(12) . . ? P1 B1 H1B1 103.1(15) . . ? Ca1 B1 H1B1 55.7(15) . . ? P1 B1 H2B1 108.8(18) . . ? Ca1 B1 H2B1 163.4(18) . . ? H1B1 B1 H2B1 112(2) . . ? P1 B1 H3B1 107.7(16) . . ? Ca1 B1 H3B1 68.5(15) . . ? H1B1 B1 H3B1 113(2) . . ? H2B1 B1 H3B1 112(2) . . ? P2 B2 Ca1 84.47(12) . . ? P2 B2 H1B2 106.4(19) . . ? Ca1 B2 H1B2 74.0(18) . . ? P2 B2 H2B2 108.3(17) . . ? Ca1 B2 H2B2 50.8(16) . . ? H1B2 B2 H2B2 109(2) . . ? P2 B2 H3B2 108.3(17) . . ? Ca1 B2 H3B2 161.3(17) . . ? H1B2 B2 H3B2 114(2) . . ? H2B2 B2 H3B2 111(2) . . ? P3 B3 Ca1 133.65(16) . . ? P3 B3 H1B3 110.7(18) . . ? Ca1 B3 H1B3 57.8(18) . . ? P3 B3 H2B3 107.8(17) . . ? Ca1 B3 H2B3 118.6(17) . . ? H1B3 B3 H2B3 108(3) . . ? P3 B3 H3B3 111.6(15) . . ? Ca1 B3 H3B3 54.3(14) . . ? H1B3 B3 H3B3 112(2) . . ? H2B3 B3 H3B3 107(2) . . ? P4 B4 Ca1 132.52(16) . . ? P4 B4 H1B4 102.8(15) . . ? Ca1 B4 H1B4 54.4(16) . . ? P4 B4 H2B4 106.0(16) . . ? Ca1 B4 H2B4 120.9(16) . . ? H1B4 B4 H2B4 112(2) . . ? P4 B4 H3B4 108.8(14) . . ? Ca1 B4 H3B4 60.2(15) . . ? H1B4 B4 H3B4 113(2) . . ? H2B4 B4 H3B4 114(2) . . ? P2 C1 P1 124.98(16) . . ? P2 C1 Ca1 92.29(11) . . ? P1 C1 Ca1 91.25(12) . . ? P2 C1 H1 105.7(18) . . ? P1 C1 H1 110.2(18) . . ? Ca1 C1 H1 134.3(17) . . ? C7 C2 C3 118.0(3) . . ? C7 C2 P1 117.7(2) . . ? C3 C2 P1 124.4(2) . . ? C4 C3 C2 121.0(3) . . ? C4 C3 H3A 119.5 . . ? C2 C3 H3A 119.5 . . ? C5 C4 C3 120.7(3) . . ? C5 C4 H4A 119.7 . . ? C3 C4 H4A 119.7 . . ? C6 C5 C4 118.8(3) . . ? C6 C5 H5A 120.6 . . ? C4 C5 H5A 120.6 . . ? C5 C6 C7 120.9(3) . . ? C5 C6 H6A 119.5 . . ? C7 C6 H6A 119.5 . . ? C2 C7 C6 120.6(3) . . ? C2 C7 H7A 119.7 . . ? C6 C7 H7A 119.7 . . ? C9 C8 C13 119.1(3) . . ? C9 C8 P1 120.7(2) . . ? C13 C8 P1 120.1(2) . . ? C8 C9 C10 120.2(3) . . ? C8 C9 H9A 119.9 . . ? C10 C9 H9A 119.9 . . ? C11 C10 C9 119.7(3) . . ? C11 C10 H10A 120.1 . . ? C9 C10 H10A 120.1 . . ? C12 C11 C10 120.3(3) . . ? C12 C11 H11A 119.8 . . ? C10 C11 H11A 119.8 . . ? C13 C12 C11 119.9(3) . . ? C13 C12 H12A 120.1 . . ? C11 C12 H12A 120.1 . . ? C12 C13 C8 120.7(3) . . ? C12 C13 H13A 119.7 . . ? C8 C13 H13A 119.7 . . ? C15 C14 C19 119.7(3) . . ? C15 C14 P2 119.9(3) . . ? C19 C14 P2 120.3(3) . . ? C14 C15 C16 120.5(4) . . ? C14 C15 H15A 119.8 . . ? C16 C15 H15A 119.8 . . ? C15 C16 C17 119.7(5) . . ? C15 C16 H16A 120.1 . . ? C17 C16 H16A 120.1 . . ? C18 C17 C16 120.6(4) . . ? C18 C17 H17A 119.7 . . ? C16 C17 H17A 119.7 . . ? C17 C18 C19 119.6(5) . . ? C17 C18 H18A 120.2 . . ? C19 C18 H18A 120.2 . . ? C14 C19 C18 119.8(4) . . ? C14 C19 H19A 120.1 . . ? C18 C19 H19A 120.1 . . ? C25 C20 C21 118.5(3) . . ? C25 C20 P2 123.2(2) . . ? C21 C20 P2 118.3(2) . . ? C22 C21 C20 120.5(3) . . ? C22 C21 H21A 119.7 . . ? C20 C21 H21A 119.7 . . ? C23 C22 C21 120.4(3) . . ? C23 C22 H22A 119.8 . . ? C21 C22 H22A 119.8 . . ? C24 C23 C22 119.6(3) . . ? C24 C23 H23A 120.2 . . ? C22 C23 H23A 120.2 . . ? C23 C24 C25 120.2(3) . . ? C23 C24 H24A 119.9 . . ? C25 C24 H24A 119.9 . . ? C24 C25 C20 120.8(3) . . ? C24 C25 H25A 119.6 . . ? C20 C25 H25A 119.6 . . ? P3 C26 P4 129.74(18) . . ? P3 C26 H26 114(2) . . ? P4 C26 H26 114(2) . . ? C32 C27 C28 118.7(3) . . ? C32 C27 P3 121.5(2) . . ? C28 C27 P3 119.7(2) . . ? C29 C28 C27 121.0(3) . . ? C29 C28 H28A 119.5 . . ? C27 C28 H28A 119.5 . . ? C30 C29 C28 119.8(3) . . ? C30 C29 H29A 120.1 . . ? C28 C29 H29A 120.1 . . ? C29 C30 C31 120.1(3) . . ? C29 C30 H30A 120.0 . . ? C31 C30 H30A 120.0 . . ? C30 C31 C32 120.3(3) . . ? C30 C31 H31A 119.9 . . ? C32 C31 H31A 119.9 . . ? C27 C32 C31 120.0(3) . . ? C27 C32 H32A 120.0 . . ? C31 C32 H32A 120.0 . . ? C34 C33 C38 118.5(3) . . ? C34 C33 P3 120.6(2) . . ? C38 C33 P3 120.8(3) . . ? C33 C34 C35 120.5(3) . . ? C33 C34 H34A 119.7 . . ? C35 C34 H34A 119.7 . . ? C36 C35 C34 120.1(4) . . ? C36 C35 H35A 119.9 . . ? C34 C35 H35A 119.9 . . ? C35 C36 C37 120.1(3) . . ? C35 C36 H36A 119.9 . . ? C37 C36 H36A 119.9 . . ? C38 C37 C36 119.9(4) . . ? C38 C37 H37A 120.1 . . ? C36 C37 H37A 120.1 . . ? C37 C38 C33 120.9(4) . . ? C37 C38 H38A 119.6 . . ? C33 C38 H38A 119.6 . . ? C40 C39 C44 118.1(3) . . ? C40 C39 P4 121.4(2) . . ? C44 C39 P4 120.2(2) . . ? C41 C40 C39 121.4(3) . . ? C41 C40 H40A 119.3 . . ? C39 C40 H40A 119.3 . . ? C42 C41 C40 119.9(4) . . ? C42 C41 H41A 120.0 . . ? C40 C41 H41A 120.0 . . ? C41 C42 C43 120.3(4) . . ? C41 C42 H42A 119.8 . . ? C43 C42 H42A 119.8 . . ? C42 C43 C44 120.1(4) . . ? C42 C43 H43A 120.0 . . ? C44 C43 H43A 120.0 . . ? C39 C44 C43 120.1(4) . . ? C39 C44 H44A 120.0 . . ? C43 C44 H44A 120.0 . . ? C46 C45 C50 119.7(3) . . ? C46 C45 P4 120.9(2) . . ? C50 C45 P4 119.4(2) . . ? C45 C46 C47 119.9(3) . . ? C45 C46 H46A 120.1 . . ? C47 C46 H46A 120.1 . . ? C48 C47 C46 120.0(3) . . ? C48 C47 H47A 120.0 . . ? C46 C47 H47A 120.0 . . ? C49 C48 C47 120.3(3) . . ? C49 C48 H48A 119.8 . . ? C47 C48 H48A 119.8 . . ? C48 C49 C50 120.2(3) . . ? C48 C49 H49A 119.9 . . ? C50 C49 H49A 119.9 . . ? C49 C50 C45 119.8(3) . . ? C49 C50 H50A 120.1 . . ? C45 C50 H50A 120.1 . . ? O1 C51 C52 106.0(3) . . ? O1 C51 H51A 110.5 . . ? C52 C51 H51A 110.5 . . ? O1 C51 H51B 110.5 . . ? C52 C51 H51B 110.5 . . ? H51A C51 H51B 108.7 . . ? C51 C52 C53 102.4(3) . . ? C51 C52 H52A 111.3 . . ? C53 C52 H52A 111.3 . . ? C51 C52 H52B 111.3 . . ? C53 C52 H52B 111.3 . . ? H52A C52 H52B 109.2 . . ? C52 C53 C54 104.1(3) . . ? C52 C53 H53A 110.9 . . ? C54 C53 H53A 110.9 . . ? C52 C53 H53B 110.9 . . ? C54 C53 H53B 110.9 . . ? H53A C53 H53B 109.0 . . ? O1 C54 C53 106.2(3) . . ? O1 C54 H54A 110.5 . . ? C53 C54 H54A 110.5 . . ? O1 C54 H54B 110.5 . . ? C53 C54 H54B 110.5 . . ? H54A C54 H54B 108.7 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.467 _refine_diff_density_min -0.264 _refine_diff_density_rms 0.059