Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 ---------- X-Sun-Content-Length: 107387 X-Sun-Charset: us-ascii X-Sun-Content-Lines: 3295 data_global #======================================================================== # 0. AUDIT DETAILS _audit_creation_date ' 2001' _audit_creation_method 'SHELX-97' _audit_update_record ; ? ; #====================================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name 'Prof. F. Gordon A. Stone' _publ_contact_author_address ; Department of Chemistry Baylor University PO Box 97348 Waco TX, 76798-7348 ; _publ_contact_author_email Gordon_Stone@baylor.edu _publ_contact_author_fax '254 710 2403' _publ_contact_author_phone '254 710 4427' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_category ? _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission for publication in J. Chem. Soc., Dalton Trans. as a Regular Paper. Manuscript number: ? Title: Monocarbollide complexes of molybdenum and tungsten: functionalization through reaction at a cage boron centre Date of submission January 2001 ; #=========================================================================== #== # 2. PROCESSING SUMMARY (JOURNAL OFFICE ONLY) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_Cambridge 186 _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #==================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? ; _publ_section_title_footnote ; ? ; # The loop structure below should contain the names and adresses of all # authors, in the required order of publication. Repeat as necessary. # add authors in order from front of paper remove ? from the next 3 lines e.g. loop_ _publ_author_name _publ_author_address 'Du, Shaowu' ; Department of Chemistry and Biochemistry Baylor University Waco TX, 76798-7348 USA ; 'Franken, Andreas' ; Department of Chemistry and Biochemistry Baylor University Waco TX, 76798-7348 USA ; 'Jelliss, Paul A' ; Department of Chemistry and Biochemistry Baylor University Waco TX, 76798-7348 USA ; 'Kautz, Jason A' ; Department of Chemistry and Biochemistry Baylor University Waco TX, 76798-7348 USA ; 'Stone, F Gordon A' ; Department of Chemistry and Biochemistry Baylor University Waco TX, 76798-7348 USA ; 'Yu, Pui-Yin' ; Department of Chemistry and Biochemistry Baylor University Waco TX, 76798-7348 USA ; #=========================================================================== #== data_24 _database_code_CSD 157559 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H34 B10 Mo N O3 P' _chemical_formula_weight 703.60 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' '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' 'Mo' 'Mo' -1.6832 0.6857 '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 '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5591(14) _cell_length_b 11.8898(12) _cell_length_c 18.4841(16) _cell_angle_alpha 104.286(9) _cell_angle_beta 97.586(12) _cell_angle_gamma 104.489(11) _cell_volume 1726.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 20 _exptl_crystal_description needles _exptl_crystal_colour yellow _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.353 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 716 _exptl_absorpt_coefficient_mu 0.460 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.92037 _exptl_absorpt_correction_T_max 0.97155 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 9.63 _diffrn_reflns_number 6495 _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_sigmaI/netI 0.0465 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 24.96 _reflns_number_total 6050 _reflns_number_gt 4870 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4 (1989)' _computing_cell_refinement 'Enraf-Nonius CAD4 (1989)' _computing_data_reduction 'XCAD4 Siemens Software (Harms, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL-PC (Bruker, 1995)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0409P)^2^+0.2998P] 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 6050 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0567 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.0877 _refine_ls_wR_factor_gt 0.0797 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.002 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo Mo 0.04407(3) 0.16531(3) 0.762421(15) 0.03236(9) Uani 1 1 d . . . C1 C -0.0047(4) 0.0374(3) 0.63278(18) 0.0411(8) Uani 1 1 d . . . H1 H -0.0352 0.0939 0.5973 0.049 Uiso 1 1 calc R . . B2 B 0.1932(5) 0.0689(4) 0.6776(2) 0.0397(9) Uani 1 1 d . . . H2 H 0.2955 0.1428 0.6735 0.048 Uiso 1 1 calc R . . B3 B 0.1797(4) 0.0160(3) 0.7607(2) 0.0356(8) Uani 1 1 d . . . B4 B -0.0314(4) -0.0396(3) 0.7654(2) 0.0391(9) Uani 1 1 d . . . H4 H -0.0764 -0.0398 0.8184 0.047 Uiso 1 1 calc R . . B5 B -0.1450(5) -0.0208(3) 0.6814(2) 0.0431(9) Uani 1 1 d . . . H5 H -0.2671 -0.0060 0.6790 0.052 Uiso 1 1 calc R . . B6 B 0.1029(5) -0.0586(4) 0.5968(2) 0.0473(10) Uani 1 1 d . . . H6 H 0.1457 -0.0648 0.5428 0.057 Uiso 1 1 calc R . . B7 B 0.2204(5) -0.0754(3) 0.6774(2) 0.0421(9) Uani 1 1 d . . . H7 H 0.3410 -0.0919 0.6763 0.051 Uiso 1 1 calc R . . B8 B 0.0807(5) -0.1432(3) 0.7291(2) 0.0424(9) Uani 1 1 d . . . H8 H 0.1102 -0.2049 0.7608 0.051 Uiso 1 1 calc R . . B9 B -0.1204(5) -0.1643(4) 0.6809(2) 0.0489(10) Uani 1 1 d . . . H9 H -0.2246 -0.2401 0.6813 0.059 Uiso 1 1 calc R . . B10 B -0.1066(5) -0.1131(4) 0.5991(2) 0.0491(10) Uani 1 1 d . . . H10 H -0.2011 -0.1546 0.5461 0.059 Uiso 1 1 calc R . . B11 B 0.0326(5) -0.1887(4) 0.6286(2) 0.0486(10) Uani 1 1 d . . . H11 H 0.0295 -0.2801 0.5954 0.058 Uiso 1 1 calc R . . C2 C 0.0857(5) 0.2023(3) 0.8735(2) 0.0496(9) Uani 1 1 d . . . O2 O 0.1110(4) 0.2198(3) 0.93862(15) 0.0768(9) Uani 1 1 d . . . C3 C -0.1711(5) 0.1797(3) 0.7911(2) 0.0472(8) Uani 1 1 d . . . O3 O -0.2894(3) 0.1862(3) 0.81035(16) 0.0691(8) Uani 1 1 d . . . C4 C 0.2627(5) 0.2968(3) 0.7973(2) 0.0529(9) Uani 1 1 d . . . O4 O 0.3876(4) 0.3686(3) 0.82175(18) 0.0852(10) Uani 1 1 d . . . P P -0.01423(10) 0.33264(7) 0.70857(5) 0.03431(19) Uani 1 1 d . . . C11 C -0.1759(4) 0.2832(3) 0.62243(17) 0.0397(8) Uani 1 1 d . . . C12 C -0.3220(4) 0.1955(3) 0.6153(2) 0.0540(9) Uani 1 1 d . . . H12 H -0.3375 0.1597 0.6543 0.065 Uiso 1 1 calc R . . C13 C -0.4450(5) 0.1606(4) 0.5512(2) 0.0628(11) Uani 1 1 d . . . H13 H -0.5430 0.1017 0.5473 0.075 Uiso 1 1 calc R . . C14 C -0.4248(5) 0.2111(5) 0.4937(2) 0.0718(13) Uani 1 1 d . . . H14 H -0.5079 0.1865 0.4503 0.086 Uiso 1 1 calc R . . C15 C -0.2832(6) 0.2972(5) 0.5000(2) 0.0766(14) Uani 1 1 d . . . H15 H -0.2698 0.3322 0.4606 0.092 Uiso 1 1 calc R . . C16 C -0.1571(5) 0.3351(4) 0.5639(2) 0.0602(11) Uani 1 1 d . . . H16 H -0.0605 0.3950 0.5672 0.072 Uiso 1 1 calc R . . C21 C -0.0820(4) 0.4436(3) 0.77533(18) 0.0410(8) Uani 1 1 d . . . C22 C -0.0238(5) 0.4734(3) 0.8528(2) 0.0548(10) Uani 1 1 d . . . H22 H 0.0536 0.4392 0.8714 0.066 Uiso 1 1 calc R . . C23 C -0.0797(6) 0.5540(3) 0.9034(2) 0.0640(11) Uani 1 1 d . . . H23 H -0.0401 0.5731 0.9556 0.077 Uiso 1 1 calc R . . C24 C -0.1923(5) 0.6051(4) 0.8768(2) 0.0680(12) Uani 1 1 d . . . H24 H -0.2305 0.6584 0.9109 0.082 Uiso 1 1 calc R . . C25 C -0.2484(6) 0.5784(5) 0.8009(3) 0.0889(16) Uani 1 1 d . . . H25 H -0.3240 0.6144 0.7828 0.107 Uiso 1 1 calc R . . C26 C -0.1941(5) 0.4976(4) 0.7499(2) 0.0713(13) Uani 1 1 d . . . H26 H -0.2339 0.4797 0.6977 0.086 Uiso 1 1 calc R . . C31 C 0.1615(4) 0.4228(3) 0.68141(18) 0.0381(7) Uani 1 1 d . . . C32 C 0.2170(5) 0.5476(3) 0.7067(2) 0.0525(9) Uani 1 1 d . . . H32 H 0.1652 0.5900 0.7403 0.063 Uiso 1 1 calc R . . C33 C 0.3497(5) 0.6107(4) 0.6826(2) 0.0651(11) Uani 1 1 d . . . H33 H 0.3863 0.6950 0.7001 0.078 Uiso 1 1 calc R . . C34 C 0.4268(5) 0.5499(4) 0.6335(2) 0.0629(11) Uani 1 1 d . . . H34 H 0.5163 0.5928 0.6179 0.076 Uiso 1 1 calc R . . C35 C 0.3728(5) 0.4264(4) 0.6071(3) 0.0642(11) Uani 1 1 d . . . H35 H 0.4247 0.3851 0.5731 0.077 Uiso 1 1 calc R . . C36 C 0.2411(5) 0.3624(3) 0.6308(2) 0.0550(10) Uani 1 1 d . . . H36 H 0.2052 0.2780 0.6128 0.066 Uiso 1 1 calc R . . C5 C 0.3276(4) 0.0515(3) 0.82750(18) 0.0369(7) Uani 1 1 d . . . N N 0.4368(3) 0.0740(2) 0.87634(15) 0.0410(6) Uani 1 1 d . . . C41 C 0.5715(4) 0.0810(3) 0.93144(18) 0.0411(8) Uani 1 1 d . . . C42 C 0.6377(4) -0.0158(3) 0.9186(2) 0.0483(9) Uani 1 1 d . . . C43 C 0.7672(4) -0.0088(4) 0.9754(2) 0.0612(11) Uani 1 1 d . . . H43 H 0.8157 -0.0714 0.9693 0.073 Uiso 1 1 calc R . . C44 C 0.8242(5) 0.0870(5) 1.0391(2) 0.0691(13) Uani 1 1 d . . . H44 H 0.9095 0.0883 1.0764 0.083 Uiso 1 1 calc R . . C45 C 0.7582(5) 0.1821(4) 1.0495(2) 0.0644(12) Uani 1 1 d . . . H45 H 0.7998 0.2469 1.0938 0.077 Uiso 1 1 calc R . . C46 C 0.6295(4) 0.1837(4) 0.9950(2) 0.0516(9) Uani 1 1 d . . . C47 C 0.5739(5) -0.1205(4) 0.8485(2) 0.0638(11) Uani 1 1 d . . . H47A H 0.6355 -0.1775 0.8500 0.096 Uiso 1 1 calc R . . H47B H 0.5855 -0.0923 0.8045 0.096 Uiso 1 1 calc R . . H47C H 0.4596 -0.1594 0.8455 0.096 Uiso 1 1 calc R . . C48 C 0.5580(6) 0.2873(4) 1.0040(3) 0.0797(13) Uani 1 1 d . . . H48A H 0.6146 0.3488 1.0510 0.120 Uiso 1 1 calc R . . H48B H 0.4430 0.2592 1.0047 0.120 Uiso 1 1 calc R . . H48C H 0.5703 0.3207 0.9621 0.120 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 Mo 0.03278(16) 0.03526(15) 0.03043(15) 0.00978(11) 0.00480(11) 0.01312(11) C1 0.0410(19) 0.049(2) 0.0335(17) 0.0105(15) 0.0011(15) 0.0191(16) B2 0.039(2) 0.047(2) 0.035(2) 0.0114(17) 0.0087(17) 0.0155(18) B3 0.0296(19) 0.038(2) 0.039(2) 0.0114(16) 0.0037(16) 0.0105(16) B4 0.033(2) 0.041(2) 0.046(2) 0.0153(17) 0.0087(17) 0.0116(17) B5 0.034(2) 0.045(2) 0.047(2) 0.0095(18) 0.0013(17) 0.0136(18) B6 0.051(2) 0.053(2) 0.038(2) 0.0054(18) 0.0094(19) 0.023(2) B7 0.043(2) 0.047(2) 0.039(2) 0.0082(18) 0.0064(17) 0.0229(19) B8 0.045(2) 0.035(2) 0.049(2) 0.0133(18) 0.0089(19) 0.0161(18) B9 0.041(2) 0.038(2) 0.061(3) 0.0102(19) 0.004(2) 0.0073(18) B10 0.042(2) 0.048(2) 0.046(2) 0.0007(19) -0.0068(19) 0.0143(19) B11 0.048(2) 0.041(2) 0.049(2) 0.0015(18) 0.005(2) 0.0161(19) C2 0.058(2) 0.052(2) 0.040(2) 0.0104(17) 0.0067(18) 0.0250(18) O2 0.101(2) 0.101(2) 0.0329(15) 0.0142(15) 0.0094(15) 0.0452(19) C3 0.050(2) 0.053(2) 0.049(2) 0.0253(17) 0.0182(18) 0.0180(18) O3 0.0551(17) 0.090(2) 0.081(2) 0.0371(17) 0.0389(16) 0.0300(16) C4 0.050(2) 0.053(2) 0.055(2) 0.0224(19) -0.0025(19) 0.0148(19) O4 0.0556(19) 0.075(2) 0.099(2) 0.0333(18) -0.0220(17) -0.0142(16) P 0.0365(5) 0.0358(4) 0.0319(4) 0.0089(3) 0.0056(4) 0.0146(4) C11 0.0425(19) 0.047(2) 0.0333(17) 0.0087(15) 0.0067(15) 0.0238(16) C12 0.046(2) 0.056(2) 0.058(2) 0.0173(19) -0.0010(18) 0.0183(18) C13 0.046(2) 0.065(3) 0.066(3) 0.004(2) -0.007(2) 0.020(2) C14 0.049(3) 0.114(4) 0.044(2) -0.003(2) -0.001(2) 0.040(3) C15 0.067(3) 0.140(4) 0.042(2) 0.037(3) 0.011(2) 0.053(3) C16 0.049(2) 0.093(3) 0.042(2) 0.025(2) 0.0067(18) 0.023(2) C21 0.045(2) 0.0412(19) 0.0369(18) 0.0066(15) 0.0087(15) 0.0177(16) C22 0.072(3) 0.052(2) 0.042(2) 0.0087(17) 0.0024(19) 0.030(2) C23 0.095(3) 0.054(2) 0.039(2) 0.0016(18) 0.011(2) 0.029(2) C24 0.076(3) 0.073(3) 0.056(3) -0.003(2) 0.017(2) 0.042(2) C25 0.107(4) 0.106(4) 0.063(3) -0.002(3) 0.005(3) 0.081(3) C26 0.085(3) 0.091(3) 0.047(2) 0.005(2) 0.000(2) 0.062(3) C31 0.0390(18) 0.0389(18) 0.0380(18) 0.0147(14) 0.0033(15) 0.0134(15) C32 0.066(3) 0.040(2) 0.048(2) 0.0101(16) 0.0117(19) 0.0121(18) C33 0.073(3) 0.046(2) 0.059(3) 0.0145(19) 0.003(2) -0.006(2) C34 0.043(2) 0.070(3) 0.078(3) 0.040(2) 0.008(2) 0.003(2) C35 0.058(3) 0.066(3) 0.090(3) 0.038(2) 0.039(2) 0.029(2) C36 0.064(2) 0.042(2) 0.071(3) 0.0220(19) 0.033(2) 0.0214(19) C5 0.0374(19) 0.0393(18) 0.0393(18) 0.0151(15) 0.0121(16) 0.0147(15) N 0.0329(15) 0.0530(17) 0.0382(16) 0.0172(13) 0.0045(13) 0.0124(13) C41 0.0247(16) 0.062(2) 0.0382(18) 0.0225(17) 0.0041(14) 0.0090(15) C42 0.0333(19) 0.069(2) 0.052(2) 0.0292(19) 0.0151(16) 0.0180(18) C43 0.038(2) 0.093(3) 0.068(3) 0.041(3) 0.011(2) 0.028(2) C44 0.033(2) 0.124(4) 0.061(3) 0.050(3) 0.0058(19) 0.021(2) C45 0.041(2) 0.093(3) 0.043(2) 0.016(2) -0.0015(18) -0.002(2) C46 0.037(2) 0.065(2) 0.050(2) 0.0196(19) 0.0095(17) 0.0071(18) C47 0.056(2) 0.071(3) 0.069(3) 0.019(2) 0.018(2) 0.026(2) C48 0.076(3) 0.071(3) 0.075(3) 0.003(2) 0.000(2) 0.017(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 Mo C2 1.954(4) . y Mo C3 2.018(4) . y Mo C4 2.020(4) . y Mo B3 2.348(4) . y Mo B4 2.376(4) . y Mo B5 2.386(4) . y Mo B2 2.403(4) . y Mo C1 2.419(3) . y Mo P 2.5575(9) . y C1 B2 1.690(5) . ? C1 B10 1.695(5) . ? C1 B5 1.703(5) . ? C1 B6 1.705(5) . ? B2 B6 1.766(5) . ? B2 B7 1.787(5) . ? B2 B3 1.805(5) . ? B3 C5 1.538(5) . y B3 B8 1.779(5) . ? B3 B7 1.783(5) . ? B3 B4 1.783(5) . ? B4 B9 1.787(5) . ? B4 B8 1.800(5) . ? B4 B5 1.814(5) . ? B5 B10 1.765(6) . ? B5 B9 1.769(6) . ? B6 B10 1.757(6) . ? B6 B7 1.767(5) . ? B6 B11 1.782(6) . ? B7 B11 1.774(6) . ? B7 B8 1.787(6) . ? B8 B9 1.757(6) . ? B8 B11 1.762(6) . ? B9 B11 1.766(6) . ? B9 B10 1.772(6) . ? B10 B11 1.770(6) . ? C2 O2 1.151(4) . y C3 O3 1.131(4) . y C4 O4 1.141(4) . y P C31 1.822(3) . ? P C11 1.829(3) . ? P C21 1.835(3) . ? C11 C16 1.379(5) . ? C11 C12 1.380(5) . ? C12 C13 1.377(5) . ? C13 C14 1.353(6) . ? C14 C15 1.347(6) . ? C15 C16 1.385(5) . ? C21 C26 1.375(5) . ? C21 C22 1.377(5) . ? C22 C23 1.388(5) . ? C23 C24 1.362(6) . ? C24 C25 1.351(6) . ? C25 C26 1.387(5) . ? C31 C32 1.376(5) . ? C31 C36 1.391(5) . ? C32 C33 1.387(5) . ? C33 C34 1.362(6) . ? C34 C35 1.362(5) . ? C35 C36 1.381(5) . ? C5 N 1.137(4) . y N C41 1.406(4) . y C41 C42 1.389(5) . ? C41 C46 1.397(5) . ? C42 C43 1.393(5) . ? C42 C47 1.485(5) . ? C43 C44 1.354(6) . ? C44 C45 1.369(6) . ? C45 C46 1.399(5) . ? C46 C48 1.491(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Mo C3 74.95(15) . . y C2 Mo C4 76.35(16) . . y C3 Mo C4 126.14(16) . . y C2 Mo B3 87.64(13) . . y C3 Mo B3 132.16(13) . . y C4 Mo B3 90.50(14) . . y C2 Mo B4 83.81(14) . . y C3 Mo B4 89.02(14) . . y C4 Mo B4 131.50(13) . . y B3 Mo B4 44.36(12) . . ? C2 Mo B5 121.82(15) . . y C3 Mo B5 78.52(14) . . y C4 Mo B5 154.36(15) . . y B3 Mo B5 73.72(13) . . ? B4 Mo B5 44.78(13) . . ? C2 Mo B2 127.02(14) . . y C3 Mo B2 150.36(14) . . y C4 Mo B2 81.81(15) . . y B3 Mo B2 44.63(13) . . ? B4 Mo B2 75.76(13) . . ? B5 Mo B2 72.74(14) . . ? C2 Mo C1 155.46(13) . . y C3 Mo C1 110.35(13) . . y C4 Mo C1 114.59(14) . . y B3 Mo C1 70.98(12) . . ? B4 Mo C1 72.56(13) . . ? B5 Mo C1 41.52(13) . . ? B2 Mo C1 41.03(12) . . ? C2 Mo P 115.95(10) . . y C3 Mo P 76.06(10) . . y C4 Mo P 77.09(10) . . y B3 Mo P 149.04(9) . . y B4 Mo P 150.14(9) . . y B5 Mo P 106.12(10) . . y B2 Mo P 104.92(9) . . y C1 Mo P 88.38(8) . . y B2 C1 B10 114.0(3) . . ? B2 C1 B5 113.6(3) . . ? B10 C1 B5 62.6(2) . . ? B2 C1 B6 62.7(2) . . ? B10 C1 B6 62.2(2) . . ? B5 C1 B6 113.8(3) . . ? B2 C1 Mo 69.00(16) . . ? B10 C1 Mo 126.8(2) . . ? B5 C1 Mo 68.21(17) . . ? B6 C1 Mo 127.4(2) . . ? C1 B2 B6 59.1(2) . . ? C1 B2 B7 104.9(3) . . ? B6 B2 B7 59.6(2) . . ? C1 B2 B3 104.7(3) . . ? B6 B2 B3 107.2(3) . . ? B7 B2 B3 59.5(2) . . ? C1 B2 Mo 69.98(17) . . ? B6 B2 Mo 125.1(2) . . ? B7 B2 Mo 121.9(2) . . ? B3 B2 Mo 66.06(16) . . ? C5 B3 B8 112.1(3) . . ? C5 B3 B7 109.6(3) . . ? B8 B3 B7 60.2(2) . . ? C5 B3 B4 125.3(3) . . ? B8 B3 B4 60.7(2) . . ? B7 B3 B4 109.8(3) . . ? C5 B3 B2 122.5(3) . . ? B8 B3 B2 108.0(3) . . ? B7 B3 B2 59.7(2) . . ? B4 B3 B2 109.7(3) . . ? C5 B3 Mo 114.2(2) . . y B8 B3 Mo 124.8(2) . . ? B7 B3 Mo 125.1(2) . . ? B4 B3 Mo 68.64(17) . . ? B2 B3 Mo 69.30(17) . . ? B3 B4 B9 105.3(3) . . ? B3 B4 B8 59.5(2) . . ? B9 B4 B8 58.7(2) . . ? B3 B4 B5 104.3(3) . . ? B9 B4 B5 58.8(2) . . ? B8 B4 B5 105.0(3) . . ? B3 B4 Mo 67.00(16) . . ? B9 B4 Mo 122.3(2) . . ? B8 B4 Mo 122.2(2) . . ? B5 B4 Mo 67.90(17) . . ? C1 B5 B10 58.5(2) . . ? C1 B5 B9 105.3(3) . . ? B10 B5 B9 60.2(2) . . ? C1 B5 B4 107.5(3) . . ? B10 B5 B4 109.1(3) . . ? B9 B5 B4 59.8(2) . . ? C1 B5 Mo 70.28(17) . . ? B10 B5 Mo 125.0(2) . . ? B9 B5 Mo 122.7(2) . . ? B4 B5 Mo 67.32(17) . . ? C1 B6 B10 58.6(2) . . ? C1 B6 B2 58.2(2) . . ? B10 B6 B2 107.4(3) . . ? C1 B6 B7 105.2(3) . . ? B10 B6 B7 107.8(3) . . ? B2 B6 B7 60.8(2) . . ? C1 B6 B11 105.1(3) . . ? B10 B6 B11 60.0(2) . . ? B2 B6 B11 108.5(3) . . ? B7 B6 B11 60.0(2) . . ? B6 B7 B11 60.5(2) . . ? B6 B7 B3 108.1(3) . . ? B11 B7 B3 107.2(3) . . ? B6 B7 B2 59.6(2) . . ? B11 B7 B2 107.9(3) . . ? B3 B7 B2 60.7(2) . . ? B6 B7 B8 108.1(3) . . ? B11 B7 B8 59.3(2) . . ? B3 B7 B8 59.8(2) . . ? B2 B7 B8 108.4(3) . . ? B9 B8 B11 60.2(2) . . ? B9 B8 B3 106.7(3) . . ? B11 B8 B3 107.9(3) . . ? B9 B8 B7 107.5(3) . . ? B11 B8 B7 60.0(2) . . ? B3 B8 B7 60.0(2) . . ? B9 B8 B4 60.3(2) . . ? B11 B8 B4 109.6(3) . . ? B3 B8 B4 59.8(2) . . ? B7 B8 B4 108.8(3) . . ? B8 B9 B11 60.0(2) . . ? B8 B9 B5 108.8(3) . . ? B11 B9 B5 108.1(3) . . ? B8 B9 B10 108.2(3) . . ? B11 B9 B10 60.0(2) . . ? B5 B9 B10 59.8(2) . . ? B8 B9 B4 61.0(2) . . ? B11 B9 B4 110.0(3) . . ? B5 B9 B4 61.3(2) . . ? B10 B9 B4 110.0(3) . . ? C1 B10 B6 59.2(2) . . ? C1 B10 B5 58.9(2) . . ? B6 B10 B5 108.3(3) . . ? C1 B10 B11 106.1(3) . . ? B6 B10 B11 60.7(2) . . ? B5 B10 B11 108.2(3) . . ? C1 B10 B9 105.5(3) . . ? B6 B10 B9 108.4(3) . . ? B5 B10 B9 60.0(2) . . ? B11 B10 B9 59.8(2) . . ? B8 B11 B9 59.7(2) . . ? B8 B11 B10 108.1(3) . . ? B9 B11 B10 60.2(2) . . ? B8 B11 B7 60.7(2) . . ? B9 B11 B7 107.7(3) . . ? B10 B11 B7 107.0(3) . . ? B8 B11 B6 108.5(3) . . ? B9 B11 B6 107.6(3) . . ? B10 B11 B6 59.3(2) . . ? B7 B11 B6 59.6(2) . . ? O2 C2 Mo 177.4(3) . . y O3 C3 Mo 176.6(3) . . y O4 C4 Mo 174.9(3) . . y C31 P C11 102.94(15) . . ? C31 P C21 104.99(15) . . ? C11 P C21 103.18(15) . . ? C31 P Mo 114.60(10) . . y C11 P Mo 116.30(11) . . y C21 P Mo 113.39(11) . . y C16 C11 C12 118.3(3) . . ? C16 C11 P 121.0(3) . . ? C12 C11 P 120.8(3) . . ? C13 C12 C11 120.6(4) . . ? C14 C13 C12 120.7(4) . . ? C15 C14 C13 119.3(4) . . ? C14 C15 C16 121.6(4) . . ? C11 C16 C15 119.5(4) . . ? C26 C21 C22 118.2(3) . . ? C26 C21 P 121.3(3) . . ? C22 C21 P 120.6(3) . . ? C21 C22 C23 120.5(4) . . ? C24 C23 C22 120.3(4) . . ? C25 C24 C23 119.9(4) . . ? C24 C25 C26 120.4(4) . . ? C21 C26 C25 120.8(4) . . ? C32 C31 C36 118.2(3) . . ? C32 C31 P 123.5(3) . . ? C36 C31 P 118.3(3) . . ? C31 C32 C33 120.5(4) . . ? C34 C33 C32 120.5(4) . . ? C35 C34 C33 120.0(4) . . ? C34 C35 C36 120.1(4) . . ? C35 C36 C31 120.7(4) . . ? N C5 B3 177.8(3) . . y C5 N C41 170.1(3) . . y C42 C41 C46 124.6(3) . . ? C42 C41 N 117.2(3) . . ? C46 C41 N 118.3(3) . . ? C41 C42 C43 116.1(4) . . ? C41 C42 C47 121.8(3) . . ? C43 C42 C47 122.1(4) . . ? C44 C43 C42 121.5(4) . . ? C43 C44 C45 121.0(4) . . ? C44 C45 C46 121.4(4) . . ? C41 C46 C45 115.4(4) . . ? C41 C46 C48 122.1(3) . . ? C45 C46 C48 122.5(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.96 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.321 _refine_diff_density_min -0.457 _refine_diff_density_rms 0.059 #===END data_28 _database_code_CSD 157560 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H50 B10 O4 P2 W' _chemical_formula_weight 1044.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'W' 'W' -0.8490 6.8722 '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 '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.298(4) _cell_length_b 10.916(2) _cell_length_c 23.439(3) _cell_angle_alpha 78.861(14) _cell_angle_beta 83.08(2) _cell_angle_gamma 75.48(2) _cell_volume 2495.4(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15 _cell_measurement_theta_max 22 _exptl_crystal_description plates _exptl_crystal_colour yellow _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.390 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 2.420 _exptl_absorpt_correction_type 'Numerical (Bruker, 1995)' _exptl_absorpt_correction_T_min 0.37168 _exptl_absorpt_correction_T_max 0.81430 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method w-4/3q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 15.83 _diffrn_reflns_number 6886 _diffrn_reflns_av_R_equivalents 0.0283 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 22.46 _reflns_number_total 6447 _reflns_number_gt 5583 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4 (1989)' _computing_cell_refinement 'Enraf-Nonius CAD4 (1989)' _computing_data_reduction 'XCAD4 Siemens Software (Harms, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL-PC (Bruker, 1995)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0363P)^2^+1.6716P] 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 6447 _refine_ls_number_parameters 586 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0406 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0705 _refine_ls_wR_factor_gt 0.0656 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W W 0.20242(2) 0.41072(2) 0.323556(8) 0.04237(9) Uani 1 1 d . . . C1 C 0.3106(6) 0.2759(5) 0.2554(2) 0.0582(14) Uani 1 1 d . . . H1 H 0.3591 0.1859 0.2827 0.070 Uiso 1 1 calc R . . B2 B 0.1357(6) 0.3158(5) 0.2508(2) 0.0454(14) Uani 1 1 d . . . H2 H 0.0679 0.2553 0.2734 0.054 Uiso 1 1 calc R . . B3 B 0.0818(6) 0.4900(6) 0.2364(3) 0.0516(16) Uani 1 1 d . . . B4 B 0.2346(7) 0.5461(6) 0.2351(2) 0.0540(16) Uani 1 1 d . . . H4 H 0.2315 0.6392 0.2473 0.065 Uiso 1 1 calc R . . B5 B 0.3691(6) 0.4107(5) 0.2454(2) 0.0405(13) Uani 1 1 d . . . H5 H 0.4595 0.4130 0.2654 0.049 Uiso 1 1 calc R . . B6 B 0.2490(7) 0.2662(6) 0.1909(2) 0.0514(16) Uani 1 1 d . . . H6 H 0.2541 0.1745 0.1769 0.062 Uiso 1 1 calc R . . B7 B 0.1111(7) 0.3986(6) 0.1782(2) 0.0526(16) Uani 1 1 d . . . H7 H 0.0258 0.3937 0.1553 0.063 Uiso 1 1 calc R . . B8 B 0.1727(7) 0.5389(6) 0.1687(3) 0.0581(17) Uani 1 1 d . . . H8 H 0.1282 0.6272 0.1394 0.070 Uiso 1 1 calc R . . B9 B 0.3466(7) 0.4927(6) 0.1757(3) 0.0565(17) Uani 1 1 d . . . H9 H 0.4157 0.5504 0.1517 0.068 Uiso 1 1 calc R . . B10 B 0.3937(7) 0.3245(6) 0.1891(2) 0.0545(16) Uani 1 1 d . . . H10 H 0.4934 0.2712 0.1740 0.065 Uiso 1 1 calc R . . B11 B 0.2694(7) 0.4032(6) 0.1405(3) 0.0558(17) Uani 1 1 d . . . H11 H 0.2868 0.4022 0.0933 0.067 Uiso 1 1 calc R . . C2 C 0.3141(7) 0.4962(6) 0.3598(2) 0.0693(17) Uani 1 1 d . . . O2 O 0.3777(6) 0.5533(5) 0.3760(2) 0.1057(17) Uani 1 1 d . . . C3 C 0.0836(7) 0.5723(6) 0.3433(2) 0.0686(17) Uani 1 1 d . . . O3 O 0.0174(5) 0.6685(5) 0.3530(2) 0.1063(17) Uani 1 1 d . . . C4 C 0.0517(6) 0.3487(5) 0.3723(2) 0.0551(14) Uani 1 1 d . . . O4 O -0.0381(4) 0.3147(4) 0.39936(18) 0.0747(12) Uani 1 1 d . . . P1 P 0.32174(14) 0.22739(13) 0.39836(5) 0.0468(3) Uani 1 1 d . . . C11 C 0.3362(6) 0.2820(5) 0.4658(2) 0.0557(14) Uani 1 1 d . . . C12 C 0.2238(7) 0.3529(7) 0.4926(3) 0.084(2) Uani 1 1 d . . . H12 H 0.1403 0.3652 0.4783 0.101 Uiso 1 1 calc R . . C13 C 0.2332(9) 0.4065(8) 0.5410(3) 0.109(3) Uani 1 1 d . . . H13 H 0.1564 0.4536 0.5588 0.131 Uiso 1 1 calc R . . C14 C 0.3550(11) 0.3894(9) 0.5619(3) 0.108(3) Uani 1 1 d . . . H14 H 0.3620 0.4280 0.5931 0.129 Uiso 1 1 calc R . . C15 C 0.4664(9) 0.3166(8) 0.5375(3) 0.098(2) Uani 1 1 d . . . H15 H 0.5489 0.3030 0.5529 0.117 Uiso 1 1 calc R . . C16 C 0.4580(7) 0.2620(6) 0.4895(2) 0.0725(17) Uani 1 1 d . . . H16 H 0.5350 0.2116 0.4733 0.087 Uiso 1 1 calc R . . C21 C 0.4976(5) 0.1508(6) 0.3772(2) 0.0520(14) Uani 1 1 d . . . C22 C 0.5421(6) 0.0200(6) 0.3832(2) 0.0650(16) Uani 1 1 d . . . H22 H 0.4831 -0.0321 0.3987 0.078 Uiso 1 1 calc R . . C23 C 0.6748(7) -0.0355(8) 0.3664(3) 0.087(2) Uani 1 1 d . . . H23 H 0.7036 -0.1244 0.3702 0.105 Uiso 1 1 calc R . . C24 C 0.7610(8) 0.0385(10) 0.3446(3) 0.102(3) Uani 1 1 d . . . H24 H 0.8495 0.0006 0.3334 0.123 Uiso 1 1 calc R . . C25 C 0.7205(7) 0.1691(10) 0.3387(3) 0.097(3) Uani 1 1 d . . . H25 H 0.7817 0.2194 0.3241 0.116 Uiso 1 1 calc R . . C26 C 0.5872(6) 0.2276(7) 0.3546(2) 0.0731(17) Uani 1 1 d . . . H26 H 0.5590 0.3166 0.3500 0.088 Uiso 1 1 calc R . . C31 C 0.2452(5) 0.0899(5) 0.4217(2) 0.0477(13) Uani 1 1 d . . . C32 C 0.1998(6) 0.0393(5) 0.3801(2) 0.0609(15) Uani 1 1 d . . . H32 H 0.2041 0.0787 0.3412 0.073 Uiso 1 1 calc R . . C33 C 0.1485(6) -0.0688(6) 0.3955(3) 0.0757(18) Uani 1 1 d . . . H33 H 0.1206 -0.1028 0.3669 0.091 Uiso 1 1 calc R . . C34 C 0.1386(7) -0.1257(6) 0.4524(3) 0.082(2) Uani 1 1 d . . . H34 H 0.1030 -0.1980 0.4628 0.098 Uiso 1 1 calc R . . C35 C 0.1811(7) -0.0764(6) 0.4941(3) 0.081(2) Uani 1 1 d . . . H35 H 0.1738 -0.1155 0.5330 0.097 Uiso 1 1 calc R . . C36 C 0.2349(6) 0.0309(6) 0.4797(2) 0.0659(16) Uani 1 1 d . . . H36 H 0.2640 0.0632 0.5086 0.079 Uiso 1 1 calc R . . O5 O -0.0507(4) 0.5706(4) 0.24281(18) 0.0721(11) Uani 1 1 d . . . C6 C -0.1577(8) 0.5192(8) 0.2630(4) 0.122(3) Uani 1 1 d . . . H6A H -0.1462 0.4790 0.3034 0.147 Uiso 1 1 calc R . . H6B H -0.1557 0.4517 0.2412 0.147 Uiso 1 1 calc R . . C7 C -0.2880(8) 0.6040(10) 0.2604(4) 0.161(5) Uani 1 1 d . . . H7A H -0.3550 0.5567 0.2759 0.241 Uiso 1 1 calc R . . H7B H -0.3031 0.6425 0.2206 0.241 Uiso 1 1 calc R . . H7C H -0.2935 0.6700 0.2830 0.241 Uiso 1 1 calc R . . P2 P 0.72034(14) -0.01701(13) 0.10032(6) 0.0480(3) Uani 1 1 d . . . C41 C 0.6629(6) 0.1323(5) 0.0538(2) 0.0544(14) Uani 1 1 d . . . C42 C 0.5282(6) 0.1817(5) 0.0466(2) 0.0577(14) Uani 1 1 d . . . H42 H 0.4647 0.1407 0.0683 0.069 Uiso 1 1 calc R . . C43 C 0.4881(7) 0.2926(6) 0.0070(3) 0.0773(18) Uani 1 1 d . . . H43 H 0.3972 0.3264 0.0017 0.093 Uiso 1 1 calc R . . C44 C 0.5831(9) 0.3535(7) -0.0249(3) 0.086(2) Uani 1 1 d . . . H44 H 0.5559 0.4284 -0.0514 0.103 Uiso 1 1 calc R . . C45 C 0.7158(9) 0.3040(7) -0.0175(3) 0.095(2) Uani 1 1 d . . . H45 H 0.7791 0.3456 -0.0390 0.115 Uiso 1 1 calc R . . C46 C 0.7577(7) 0.1936(7) 0.0211(3) 0.0814(19) Uani 1 1 d . . . H46 H 0.8489 0.1596 0.0254 0.098 Uiso 1 1 calc R . . C51 C 0.7887(5) -0.1386(6) 0.0552(2) 0.0585(15) Uani 1 1 d . . . C52 C 0.8017(6) -0.1054(7) -0.0049(3) 0.0758(18) Uani 1 1 d . . . H52 H 0.7760 -0.0200 -0.0227 0.091 Uiso 1 1 calc R . . C53 C 0.8545(7) -0.2024(10) -0.0388(3) 0.100(3) Uani 1 1 d . . . H53 H 0.8647 -0.1820 -0.0792 0.119 Uiso 1 1 calc R . . C54 C 0.8900(8) -0.3252(10) -0.0118(4) 0.119(3) Uani 1 1 d . . . H54 H 0.9251 -0.3891 -0.0343 0.142 Uiso 1 1 calc R . . C55 C 0.8766(9) -0.3591(8) 0.0468(4) 0.121(3) Uani 1 1 d . . . H55 H 0.9030 -0.4447 0.0641 0.145 Uiso 1 1 calc R . . C56 C 0.8237(7) -0.2663(7) 0.0807(3) 0.089(2) Uani 1 1 d . . . H56 H 0.8115 -0.2894 0.1209 0.107 Uiso 1 1 calc R . . C61 C 0.8460(5) -0.0003(5) 0.1435(2) 0.0468(12) Uani 1 1 d . . . C62 C 0.9347(7) -0.1075(6) 0.1694(3) 0.090(2) Uani 1 1 d . . . H62 H 0.9354 -0.1883 0.1619 0.108 Uiso 1 1 calc R . . C63 C 1.0224(7) -0.0942(7) 0.2066(4) 0.098(2) Uani 1 1 d . . . H63 H 1.0821 -0.1664 0.2244 0.118 Uiso 1 1 calc R . . C64 C 1.0225(6) 0.0238(7) 0.2175(3) 0.0756(18) Uani 1 1 d . . . H64 H 1.0841 0.0322 0.2415 0.091 Uiso 1 1 calc R . . C65 C 0.9328(6) 0.1289(6) 0.1933(3) 0.0668(16) Uani 1 1 d . . . H65 H 0.9322 0.2092 0.2013 0.080 Uiso 1 1 calc R . . C66 C 0.8422(6) 0.1175(5) 0.1569(2) 0.0593(15) Uani 1 1 d . . . H66 H 0.7787 0.1895 0.1415 0.071 Uiso 1 1 calc R . . C71 C 0.5862(5) -0.0644(4) 0.1489(2) 0.0442(12) Uani 1 1 d . . . C72 C 0.5683(5) -0.0407(5) 0.2051(2) 0.0516(13) Uani 1 1 d . . . H72 H 0.6240 0.0022 0.2178 0.062 Uiso 1 1 calc R . . C73 C 0.4676(6) -0.0806(5) 0.2425(2) 0.0592(15) Uani 1 1 d . . . H73 H 0.4553 -0.0643 0.2805 0.071 Uiso 1 1 calc R . . C74 C 0.3860(6) -0.1436(6) 0.2246(3) 0.0689(17) Uani 1 1 d . . . H74 H 0.3203 -0.1723 0.2507 0.083 Uiso 1 1 calc R . . C75 C 0.3999(6) -0.1649(6) 0.1686(3) 0.0728(18) Uani 1 1 d . . . H75 H 0.3418 -0.2057 0.1563 0.087 Uiso 1 1 calc R . . C76 C 0.5005(6) -0.1259(5) 0.1296(3) 0.0631(15) Uani 1 1 d . . . H76 H 0.5106 -0.1405 0.0914 0.076 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 W 0.05230(14) 0.04272(13) 0.03756(12) -0.01136(8) 0.00310(8) -0.02076(9) C1 0.067(4) 0.058(3) 0.054(3) -0.017(3) -0.005(3) -0.017(3) B2 0.056(4) 0.044(3) 0.041(3) -0.006(3) -0.006(3) -0.022(3) B3 0.052(4) 0.045(4) 0.054(4) -0.004(3) -0.007(3) -0.006(3) B4 0.078(5) 0.043(3) 0.044(3) -0.006(3) 0.006(3) -0.026(3) B5 0.042(3) 0.050(3) 0.036(3) -0.012(3) 0.002(2) -0.020(3) B6 0.073(5) 0.043(3) 0.042(3) -0.009(3) -0.008(3) -0.017(3) B7 0.061(4) 0.055(4) 0.043(3) -0.003(3) -0.013(3) -0.014(3) B8 0.073(5) 0.047(4) 0.048(4) 0.005(3) -0.004(3) -0.013(3) B9 0.065(4) 0.057(4) 0.050(4) -0.007(3) 0.009(3) -0.026(3) B10 0.061(4) 0.060(4) 0.044(3) -0.019(3) 0.008(3) -0.015(3) B11 0.078(5) 0.056(4) 0.036(3) -0.007(3) 0.005(3) -0.024(4) C2 0.097(5) 0.069(4) 0.058(4) -0.020(3) -0.003(3) -0.042(4) O2 0.140(5) 0.110(4) 0.104(4) -0.036(3) -0.022(3) -0.077(4) C3 0.088(5) 0.062(4) 0.061(4) -0.023(3) 0.016(3) -0.028(4) O3 0.121(4) 0.069(3) 0.127(4) -0.052(3) 0.035(3) -0.014(3) C4 0.058(4) 0.053(3) 0.055(3) -0.006(3) -0.004(3) -0.016(3) O4 0.059(3) 0.082(3) 0.080(3) -0.004(2) 0.016(2) -0.028(2) P1 0.0515(9) 0.0602(9) 0.0342(7) -0.0104(6) -0.0012(6) -0.0219(7) C11 0.068(4) 0.071(4) 0.035(3) -0.013(3) -0.002(3) -0.027(3) C12 0.074(5) 0.127(6) 0.058(4) -0.040(4) 0.006(3) -0.024(4) C13 0.124(7) 0.145(8) 0.065(5) -0.056(5) 0.017(5) -0.028(6) C14 0.146(8) 0.142(8) 0.059(5) -0.042(5) -0.010(5) -0.057(7) C15 0.113(7) 0.135(7) 0.067(5) -0.029(5) -0.027(4) -0.052(6) C16 0.083(5) 0.089(5) 0.058(4) -0.023(3) -0.011(3) -0.032(4) C21 0.045(3) 0.080(4) 0.034(3) -0.009(3) -0.005(2) -0.021(3) C22 0.057(4) 0.086(5) 0.048(3) -0.013(3) 0.000(3) -0.011(3) C23 0.071(5) 0.104(6) 0.074(5) -0.022(4) 0.006(4) 0.000(4) C24 0.057(5) 0.156(8) 0.074(5) -0.016(5) -0.001(4) 0.007(6) C25 0.058(5) 0.166(8) 0.064(4) -0.001(5) 0.009(3) -0.040(5) C26 0.062(4) 0.095(5) 0.059(4) 0.004(3) -0.003(3) -0.026(4) C31 0.040(3) 0.057(3) 0.048(3) -0.007(3) -0.003(2) -0.015(3) C32 0.071(4) 0.060(4) 0.052(3) 0.000(3) -0.007(3) -0.023(3) C33 0.085(5) 0.061(4) 0.088(5) -0.001(4) -0.021(4) -0.032(4) C34 0.074(5) 0.068(4) 0.101(5) 0.015(4) -0.011(4) -0.035(4) C35 0.079(5) 0.088(5) 0.070(4) 0.025(4) 0.000(4) -0.040(4) C36 0.064(4) 0.084(4) 0.047(3) -0.001(3) 0.001(3) -0.023(3) O5 0.058(3) 0.064(3) 0.088(3) -0.013(2) 0.004(2) -0.008(2) C6 0.074(6) 0.095(6) 0.171(9) 0.019(6) 0.017(5) -0.013(5) C7 0.069(6) 0.177(10) 0.175(10) 0.058(8) 0.014(6) 0.007(6) P2 0.0460(8) 0.0537(8) 0.0481(8) -0.0139(6) 0.0026(6) -0.0173(7) C41 0.058(4) 0.066(4) 0.042(3) -0.007(3) 0.006(3) -0.025(3) C42 0.061(4) 0.059(4) 0.050(3) -0.007(3) 0.005(3) -0.013(3) C43 0.079(5) 0.087(5) 0.056(4) -0.011(4) -0.005(3) -0.002(4) C44 0.125(7) 0.074(5) 0.045(4) 0.008(3) 0.000(4) -0.014(5) C45 0.105(6) 0.102(6) 0.068(5) 0.023(4) 0.012(4) -0.041(5) C46 0.075(5) 0.096(5) 0.069(4) 0.008(4) 0.001(3) -0.032(4) C51 0.045(3) 0.076(4) 0.063(4) -0.034(3) -0.004(3) -0.012(3) C52 0.061(4) 0.109(5) 0.065(4) -0.034(4) -0.002(3) -0.020(4) C53 0.071(5) 0.154(8) 0.081(5) -0.064(6) -0.002(4) -0.008(5) C54 0.083(6) 0.148(9) 0.130(8) -0.096(7) -0.023(5) 0.024(6) C55 0.132(8) 0.106(6) 0.123(7) -0.069(6) -0.038(6) 0.025(5) C56 0.104(6) 0.076(5) 0.090(5) -0.045(4) -0.017(4) 0.000(4) C61 0.040(3) 0.047(3) 0.055(3) -0.012(3) 0.002(2) -0.013(3) C62 0.072(5) 0.060(4) 0.148(7) -0.036(4) -0.041(5) -0.005(4) C63 0.071(5) 0.075(5) 0.155(7) -0.035(5) -0.056(5) 0.004(4) C64 0.062(4) 0.085(5) 0.091(5) -0.024(4) -0.015(4) -0.027(4) C65 0.075(4) 0.057(4) 0.081(4) -0.015(3) -0.013(4) -0.033(3) C66 0.066(4) 0.048(3) 0.066(4) -0.004(3) -0.013(3) -0.018(3) C71 0.042(3) 0.041(3) 0.053(3) -0.010(2) -0.002(2) -0.014(2) C72 0.049(3) 0.054(3) 0.057(3) -0.013(3) 0.003(3) -0.020(3) C73 0.062(4) 0.055(3) 0.062(4) -0.017(3) 0.007(3) -0.016(3) C74 0.063(4) 0.065(4) 0.079(4) -0.014(3) 0.019(3) -0.025(3) C75 0.065(4) 0.076(4) 0.092(5) -0.023(4) 0.007(3) -0.043(4) C76 0.068(4) 0.068(4) 0.065(4) -0.021(3) -0.001(3) -0.031(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 W C3 1.979(7) . y W C4 1.993(6) . y W C2 1.999(6) . y W B4 2.343(6) . y W B5 2.354(5) . y W C1 2.370(5) . y W B2 2.405(5) . y W B3 2.419(6) . y W P1 2.5533(15) . y C1 B5 1.692(7) . ? C1 B10 1.738(8) . ? C1 B6 1.739(7) . ? C1 B2 1.755(8) . ? B2 B7 1.780(8) . ? B2 B6 1.790(8) . ? B2 B3 1.819(8) . ? B3 O5 1.434(7) . y B3 B7 1.797(9) . ? B3 B8 1.801(8) . ? B3 B4 1.821(9) . ? B4 B5 1.754(9) . ? B4 B8 1.773(9) . ? B4 B9 1.788(8) . ? B5 B9 1.716(8) . ? B5 B10 1.724(8) . ? B6 B10 1.753(9) . ? B6 B11 1.758(8) . ? B6 B7 1.761(9) . ? B7 B11 1.765(9) . ? B7 B8 1.766(9) . ? B8 B9 1.754(10) . ? B8 B11 1.762(9) . ? B9 B10 1.753(9) . ? B9 B11 1.769(9) . ? B10 B11 1.760(9) . ? C2 O2 1.148(6) . y C3 O3 1.147(7) . y C4 O4 1.156(6) . y P1 C11 1.827(5) . ? P1 C31 1.829(5) . ? P1 C21 1.846(6) . ? C11 C12 1.379(8) . ? C11 C16 1.384(8) . ? C12 C13 1.395(9) . ? C13 C14 1.358(11) . ? C14 C15 1.355(10) . ? C15 C16 1.390(8) . ? C21 C22 1.371(8) . ? C21 C26 1.390(8) . ? C22 C23 1.392(8) . ? C23 C24 1.340(10) . ? C24 C25 1.365(11) . ? C25 C26 1.399(9) . ? C31 C32 1.386(7) . ? C31 C36 1.392(7) . ? C32 C33 1.379(7) . ? C33 C34 1.363(8) . ? C34 C35 1.364(9) . ? C35 C36 1.386(8) . ? O5 C6 1.355(8) . y C6 C7 1.427(10) . y P2 C41 1.783(6) . ? P2 C71 1.796(5) . ? P2 C61 1.800(5) . ? P2 C51 1.809(5) . ? C41 C42 1.374(7) . ? C41 C46 1.392(8) . ? C42 C43 1.381(8) . ? C43 C44 1.384(9) . ? C44 C45 1.356(9) . ? C45 C46 1.367(9) . ? C51 C56 1.381(8) . ? C51 C52 1.383(8) . ? C52 C53 1.407(9) . ? C53 C54 1.347(11) . ? C54 C55 1.352(11) . ? C55 C56 1.372(9) . ? C61 C66 1.373(7) . ? C61 C62 1.376(8) . ? C62 C63 1.380(8) . ? C63 C64 1.360(8) . ? C64 C65 1.355(8) . ? C65 C66 1.380(7) . ? C71 C72 1.372(7) . ? C71 C76 1.394(7) . ? C72 C73 1.376(7) . ? C73 C74 1.356(8) . ? C74 C75 1.362(8) . ? C75 C76 1.390(8) . ? 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 C3 W C4 77.9(2) . . y C3 W C2 72.9(3) . . y C4 W C2 118.7(2) . . y C3 W B4 81.5(2) . . y C4 W B4 138.2(2) . . y C2 W B4 88.6(2) . . y C3 W B5 121.7(2) . . y C4 W B5 154.3(2) . . y C2 W B5 85.0(2) . . y B4 W B5 43.9(2) . . ? C3 W C1 151.7(2) . . y C4 W C1 112.9(2) . . y C2 W C1 118.4(2) . . y B4 W C1 73.4(2) . . ? B5 W C1 41.96(18) . . ? C3 W B2 117.8(2) . . y C4 W B2 83.3(2) . . y C2 W B2 157.9(2) . . y B4 W B2 74.9(2) . . ? B5 W B2 72.89(19) . . ? C1 W B2 43.13(19) . . ? C3 W B3 79.1(2) . . y C4 W B3 95.3(2) . . y C2 W B3 128.9(2) . . y B4 W B3 44.9(2) . . ? B5 W B3 74.5(2) . . ? C1 W B3 74.0(2) . . ? B2 W B3 44.31(19) . . ? C3 W P1 124.16(18) . . y C4 W P1 76.48(16) . . y C2 W P1 77.52(18) . . y B4 W P1 143.86(17) . . y B5 W P1 101.15(14) . . y C1 W P1 84.12(14) . . y B2 W P1 107.30(14) . . y B3 W P1 151.57(15) . . y B5 C1 B10 60.3(3) . . ? B5 C1 B6 108.8(4) . . ? B10 C1 B6 60.6(3) . . ? B5 C1 B2 110.2(4) . . ? B10 C1 B2 111.2(4) . . ? B6 C1 B2 61.6(3) . . ? B5 C1 W 68.5(3) . . ? B10 C1 W 125.5(3) . . ? B6 C1 W 126.5(4) . . ? B2 C1 W 69.5(3) . . ? C1 B2 B7 105.0(4) . . ? C1 B2 B6 58.7(3) . . ? B7 B2 B6 59.1(3) . . ? C1 B2 B3 107.4(4) . . ? B7 B2 B3 59.9(3) . . ? B6 B2 B3 108.0(4) . . ? C1 B2 W 67.4(2) . . ? B7 B2 W 122.3(3) . . ? B6 B2 W 121.9(3) . . ? B3 B2 W 68.3(3) . . ? O5 B3 B7 115.7(5) . . ? O5 B3 B8 112.7(4) . . ? B7 B3 B8 58.8(3) . . ? O5 B3 B2 129.3(5) . . ? B7 B3 B2 59.0(3) . . ? B8 B3 B2 105.0(4) . . ? O5 B3 B4 123.2(5) . . ? B7 B3 B4 105.1(4) . . ? B8 B3 B4 58.6(3) . . ? B2 B3 B4 104.9(4) . . ? O5 B3 W 116.9(4) . . ? B7 B3 W 120.7(4) . . ? B8 B3 W 118.9(4) . . ? B2 B3 W 67.4(3) . . ? B4 B3 W 65.3(3) . . ? B5 B4 B8 104.4(4) . . ? B5 B4 B9 58.0(3) . . ? B8 B4 B9 59.0(4) . . ? B5 B4 B3 107.8(4) . . ? B8 B4 B3 60.1(3) . . ? B9 B4 B3 108.3(4) . . ? B5 B4 W 68.4(3) . . ? B8 B4 W 124.3(4) . . ? B9 B4 W 122.9(4) . . ? B3 B4 W 69.8(3) . . ? C1 B5 B9 110.0(4) . . ? C1 B5 B10 61.2(3) . . ? B9 B5 B10 61.3(3) . . ? C1 B5 B4 109.6(4) . . ? B9 B5 B4 62.0(3) . . ? B10 B5 B4 111.8(4) . . ? C1 B5 W 69.5(3) . . ? B9 B5 W 126.0(4) . . ? B10 B5 W 127.2(3) . . ? B4 B5 W 67.7(3) . . ? C1 B6 B10 59.7(3) . . ? C1 B6 B11 107.0(4) . . ? B10 B6 B11 60.2(4) . . ? C1 B6 B7 106.6(4) . . ? B10 B6 B7 108.2(4) . . ? B11 B6 B7 60.2(4) . . ? C1 B6 B2 59.6(3) . . ? B10 B6 B2 108.8(4) . . ? B11 B6 B2 108.9(4) . . ? B7 B6 B2 60.2(3) . . ? B6 B7 B11 59.8(3) . . ? B6 B7 B8 107.4(5) . . ? B11 B7 B8 59.9(4) . . ? B6 B7 B2 60.7(3) . . ? B11 B7 B2 109.0(4) . . ? B8 B7 B2 108.2(4) . . ? B6 B7 B3 110.4(4) . . ? B11 B7 B3 110.3(4) . . ? B8 B7 B3 60.7(3) . . ? B2 B7 B3 61.1(3) . . ? B9 B8 B11 60.4(4) . . ? B9 B8 B7 108.2(5) . . ? B11 B8 B7 60.1(4) . . ? B9 B8 B4 60.9(4) . . ? B11 B8 B4 109.6(5) . . ? B7 B8 B4 108.5(4) . . ? B9 B8 B3 110.7(4) . . ? B11 B8 B3 110.3(4) . . ? B7 B8 B3 60.5(3) . . ? B4 B8 B3 61.2(3) . . ? B5 B9 B10 59.6(3) . . ? B5 B9 B8 106.8(4) . . ? B10 B9 B8 107.9(5) . . ? B5 B9 B11 106.9(4) . . ? B10 B9 B11 59.9(4) . . ? B8 B9 B11 60.0(4) . . ? B5 B9 B4 60.0(3) . . ? B10 B9 B4 108.8(4) . . ? B8 B9 B4 60.1(4) . . ? B11 B9 B4 108.6(4) . . ? B5 B10 C1 58.5(3) . . ? B5 B10 B6 106.7(4) . . ? C1 B10 B6 59.7(3) . . ? B5 B10 B9 59.1(3) . . ? C1 B10 B9 106.2(4) . . ? B6 B10 B9 108.2(5) . . ? B5 B10 B11 107.0(4) . . ? C1 B10 B11 107.0(5) . . ? B6 B10 B11 60.1(3) . . ? B9 B10 B11 60.5(4) . . ? B6 B11 B10 59.8(3) . . ? B6 B11 B8 107.6(4) . . ? B10 B11 B8 107.3(4) . . ? B6 B11 B7 60.0(3) . . ? B10 B11 B7 107.7(4) . . ? B8 B11 B7 60.1(4) . . ? B6 B11 B9 107.3(4) . . ? B10 B11 B9 59.6(4) . . ? B8 B11 B9 59.6(4) . . ? B7 B11 B9 107.6(4) . . ? O2 C2 W 173.7(5) . . y O3 C3 W 177.4(5) . . y O4 C4 W 178.1(5) . . y C11 P1 C31 104.9(2) . . ? C11 P1 C21 102.8(2) . . ? C31 P1 C21 102.6(2) . . ? C11 P1 W 111.72(19) . . y C31 P1 W 117.01(16) . . y C21 P1 W 116.20(17) . . y C12 C11 C16 117.8(5) . . ? C12 C11 P1 119.5(4) . . ? C16 C11 P1 122.6(5) . . ? C11 C12 C13 121.1(7) . . ? C14 C13 C12 119.7(8) . . ? C15 C14 C13 120.4(7) . . ? C14 C15 C16 120.4(7) . . ? C11 C16 C15 120.6(7) . . ? C22 C21 C26 119.1(6) . . ? C22 C21 P1 121.6(4) . . ? C26 C21 P1 119.3(5) . . ? C21 C22 C23 120.6(6) . . ? C24 C23 C22 120.2(7) . . ? C23 C24 C25 120.7(7) . . ? C24 C25 C26 120.3(7) . . ? C21 C26 C25 119.1(7) . . ? C32 C31 C36 118.4(5) . . ? C32 C31 P1 119.2(4) . . ? C36 C31 P1 122.3(4) . . ? C33 C32 C31 121.0(5) . . ? C34 C33 C32 120.2(6) . . ? C33 C34 C35 119.8(6) . . ? C34 C35 C36 121.2(6) . . ? C35 C36 C31 119.4(6) . . ? C6 O5 B3 120.8(5) . . y O5 C6 C7 117.3(7) . . y C41 P2 C71 111.8(2) . . ? C41 P2 C61 108.8(2) . . ? C71 P2 C61 108.2(2) . . ? C41 P2 C51 108.3(3) . . ? C71 P2 C51 108.6(2) . . ? C61 P2 C51 111.2(2) . . ? C42 C41 C46 120.0(5) . . ? C42 C41 P2 121.1(4) . . ? C46 C41 P2 118.7(5) . . ? C41 C42 C43 119.5(5) . . ? C42 C43 C44 120.0(6) . . ? C45 C44 C43 120.1(6) . . ? C44 C45 C46 120.8(6) . . ? C45 C46 C41 119.6(7) . . ? C56 C51 C52 119.6(6) . . ? C56 C51 P2 119.8(5) . . ? C52 C51 P2 120.6(5) . . ? C51 C52 C53 119.2(7) . . ? C54 C53 C52 119.0(7) . . ? C53 C54 C55 122.4(8) . . ? C54 C55 C56 119.6(8) . . ? C55 C56 C51 120.2(7) . . ? C66 C61 C62 119.6(5) . . ? C66 C61 P2 119.7(4) . . ? C62 C61 P2 120.1(4) . . ? C61 C62 C63 119.5(6) . . ? C64 C63 C62 120.6(6) . . ? C65 C64 C63 120.0(6) . . ? C64 C65 C66 120.4(5) . . ? C61 C66 C65 119.8(5) . . ? C72 C71 C76 120.0(5) . . ? C72 C71 P2 120.1(4) . . ? C76 C71 P2 119.9(4) . . ? C71 C72 C73 119.6(5) . . ? C74 C73 C72 120.9(5) . . ? C73 C74 C75 120.3(5) . . ? C74 C75 C76 120.4(5) . . ? C75 C76 C71 118.8(5) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 22.46 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.715 _refine_diff_density_min -0.524 _refine_diff_density_rms 0.068 #===END data_31 _database_code_CSD 157561 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H37 B10 O4 P W' _chemical_formula_weight 748.49 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' 'W' 'W' -0.8490 6.8722 '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 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 11.916(2) _cell_length_b 13.606(2) _cell_length_c 20.455(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.272(10) _cell_angle_gamma 90.00 _cell_volume 3313.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15 _cell_measurement_theta_max 20 _exptl_crystal_description plates _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.500 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 3.566 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.4693 _exptl_absorpt_correction_T_max 0.7635 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method w-5/3q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 6.26 _diffrn_reflns_number 5493 _diffrn_reflns_av_R_equivalents 0.0364 _diffrn_reflns_av_sigmaI/netI 0.0667 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 24.00 _reflns_number_total 5211 _reflns_number_gt 3631 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+3.8073P] 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 5211 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0766 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.0818 _refine_ls_wR_factor_gt 0.0799 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W W 0.33395(3) 0.19066(3) 0.087780(17) 0.04154(12) Uani 1 d . . . C1 C 0.1742(8) 0.0880(6) 0.0982(5) 0.069(3) Uani 1 d . . . H1 H 0.1033 0.1343 0.0811 0.082 Uiso 1 calc R . . B2 B 0.2371(9) 0.1108(8) 0.1720(6) 0.059(3) Uani 1 d . . . H2 H 0.2115 0.1698 0.2051 0.070 Uiso 1 calc R . . B3 B 0.3772(9) 0.0684(9) 0.1655(5) 0.056(3) Uani 1 d . . . B4 B 0.3979(9) 0.0259(7) 0.0846(5) 0.056(3) Uani 1 d . . . H4 H 0.4788 0.0269 0.0605 0.067 Uiso 1 calc R . . B5 B 0.2625(10) 0.0410(7) 0.0436(6) 0.056(3) Uani 1 d . . . H5 H 0.2520 0.0537 -0.0094 0.067 Uiso 1 calc R . . B6 B 0.1500(10) 0.0077(8) 0.1605(6) 0.072(4) Uani 1 d . . . H6 H 0.0698 0.0023 0.1851 0.086 Uiso 1 calc R . . B7 B 0.2786(10) -0.0077(8) 0.2035(6) 0.069(3) Uani 1 d . . . H7 H 0.2839 -0.0233 0.2563 0.083 Uiso 1 calc R . . B8 B 0.3735(10) -0.0604(9) 0.1499(6) 0.071(3) Uani 1 d . . . H8 H 0.4394 -0.1113 0.1679 0.085 Uiso 1 calc R . . B9 B 0.3054(11) -0.0729(8) 0.0736(6) 0.075(4) Uani 1 d . . . H9 H 0.3284 -0.1322 0.0400 0.090 Uiso 1 calc R . . B10 B 0.1655(12) -0.0354(8) 0.0807(7) 0.085(4) Uani 1 d . . . H10 H 0.0953 -0.0700 0.0527 0.102 Uiso 1 calc R . . B11 B 0.2333(11) -0.0962(8) 0.1457(6) 0.077(4) Uani 1 d . . . H11 H 0.2078 -0.1705 0.1601 0.093 Uiso 1 calc R . . C2 C 0.4931(9) 0.2227(7) 0.0889(5) 0.071(3) Uani 1 d . . . O2 O 0.5881(6) 0.2414(6) 0.0910(4) 0.106(3) Uani 1 d . . . C3 C 0.3512(8) 0.2930(7) 0.1553(5) 0.066(3) Uani 1 d . . . O3 O 0.3678(7) 0.3494(6) 0.1971(4) 0.100(3) Uani 1 d . . . C4 C 0.3743(8) 0.2146(6) -0.0070(5) 0.059(3) Uani 1 d . . . O4 O 0.3996(6) 0.2251(6) -0.0594(3) 0.085(2) Uani 1 d . . . O5 O 0.4762(6) 0.1032(5) 0.2137(3) 0.079(2) Uani 1 d . . . C5 C 0.4481(12) 0.1352(11) 0.2791(6) 0.139(6) Uani 1 d . . . H5A H 0.3778 0.1697 0.2769 0.208 Uiso 1 calc R . . H5B H 0.5059 0.1782 0.2965 0.208 Uiso 1 calc R . . H5C H 0.4422 0.0790 0.3071 0.208 Uiso 1 calc R . . C6 C 0.5843(10) 0.0521(10) 0.2100(6) 0.111(5) Uani 1 d . . . H6A H 0.5926 0.0288 0.1656 0.134 Uiso 1 calc R . . H6B H 0.5842 -0.0048 0.2386 0.134 Uiso 1 calc R . . C7 C 0.6812(12) 0.1151(12) 0.2288(7) 0.131(6) Uani 1 d . . . H7A H 0.6762 0.1336 0.2744 0.157 Uiso 1 calc R . . H7B H 0.6772 0.1748 0.2029 0.157 Uiso 1 calc R . . C8 C 0.7952(17) 0.0653(17) 0.2193(10) 0.173(9) Uani 1 d . . . H8A H 0.8552 0.1083 0.2352 0.208 Uiso 1 calc R . . H8B H 0.7995 0.0049 0.2445 0.208 Uiso 1 calc R . . C9 C 0.8096(16) 0.0438(18) 0.1518(13) 0.245(14) Uani 1 d . . . H9A H 0.8801 0.0109 0.1470 0.368 Uiso 1 calc R . . H9B H 0.8088 0.1039 0.1272 0.368 Uiso 1 calc R . . H9C H 0.7495 0.0021 0.1359 0.368 Uiso 1 calc R . . P P 0.19463(17) 0.32290(16) 0.05055(10) 0.0388(5) Uani 1 d . . . C11 C 0.0625(6) 0.3232(6) 0.0926(4) 0.041(2) Uani 1 d . . . C12 C -0.0399(7) 0.3101(8) 0.0606(4) 0.063(2) Uani 1 d . . . H12 H -0.0423 0.2993 0.0157 0.076 Uiso 1 calc R . . C13 C -0.1388(8) 0.3124(10) 0.0927(5) 0.092(4) Uani 1 d . . . H13 H -0.2067 0.3016 0.0697 0.111 Uiso 1 calc R . . C14 C -0.1374(9) 0.3302(7) 0.1573(6) 0.069(3) Uani 1 d . . . H14 H -0.2043 0.3340 0.1790 0.083 Uiso 1 calc R . . C15 C -0.0388(10) 0.3426(6) 0.1904(5) 0.066(3) Uani 1 d . . . H15 H -0.0379 0.3537 0.2353 0.080 Uiso 1 calc R . . C16 C 0.0617(8) 0.3390(6) 0.1584(4) 0.057(3) Uani 1 d . . . H16 H 0.1292 0.3474 0.1821 0.068 Uiso 1 calc R . . C21 C 0.1504(6) 0.3184(6) -0.0360(3) 0.0421(19) Uani 1 d . . . C22 C 0.1527(8) 0.3998(6) -0.0752(4) 0.057(3) Uani 1 d . . . H22 H 0.1775 0.4594 -0.0578 0.068 Uiso 1 calc R . . C23 C 0.1187(9) 0.3945(7) -0.1406(4) 0.066(3) Uani 1 d . . . H23 H 0.1228 0.4497 -0.1672 0.079 Uiso 1 calc R . . C24 C 0.0793(8) 0.3081(9) -0.1657(4) 0.070(3) Uani 1 d . . . H24 H 0.0546 0.3052 -0.2093 0.084 Uiso 1 calc R . . C25 C 0.0751(8) 0.2247(7) -0.1278(5) 0.066(3) Uani 1 d . . . H25 H 0.0491 0.1656 -0.1454 0.079 Uiso 1 calc R . . C26 C 0.1108(7) 0.2313(6) -0.0626(4) 0.056(3) Uani 1 d . . . H26 H 0.1081 0.1757 -0.0362 0.067 Uiso 1 calc R . . C31 C 0.2457(7) 0.4486(6) 0.0622(4) 0.041(2) Uani 1 d . . . C32 C 0.3570(8) 0.4718(6) 0.0540(4) 0.058(3) Uani 1 d . . . H32 H 0.4068 0.4219 0.0438 0.070 Uiso 1 calc R . . C33 C 0.3960(9) 0.5653(7) 0.0603(5) 0.068(3) Uani 1 d . . . H33 H 0.4715 0.5788 0.0547 0.081 Uiso 1 calc R . . C34 C 0.3242(10) 0.6392(7) 0.0750(5) 0.068(3) Uani 1 d . . . H34 H 0.3505 0.7034 0.0790 0.082 Uiso 1 calc R . . C35 C 0.2146(10) 0.6192(7) 0.0838(5) 0.066(3) Uani 1 d . . . H35 H 0.1661 0.6697 0.0945 0.079 Uiso 1 calc R . . C36 C 0.1745(8) 0.5251(6) 0.0769(4) 0.057(3) Uani 1 d . . . H36 H 0.0987 0.5126 0.0822 0.069 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W 0.04237(19) 0.03658(18) 0.04549(19) 0.0078(2) -0.00055(13) 0.0005(2) C1 0.067(7) 0.040(6) 0.098(8) 0.021(6) -0.002(6) -0.006(5) B2 0.059(7) 0.050(7) 0.068(8) 0.009(6) 0.016(6) -0.002(6) B3 0.068(7) 0.058(7) 0.042(6) 0.022(6) -0.012(5) -0.003(6) B4 0.060(7) 0.042(6) 0.067(8) 0.015(6) 0.007(6) 0.016(5) B5 0.088(9) 0.025(5) 0.053(7) 0.009(5) 0.001(6) -0.001(5) B6 0.071(8) 0.045(7) 0.101(10) 0.016(7) 0.029(7) -0.006(6) B7 0.097(10) 0.042(6) 0.069(8) 0.022(6) 0.018(7) 0.002(6) B8 0.086(9) 0.054(7) 0.075(8) 0.020(7) 0.012(7) 0.016(7) B9 0.111(12) 0.034(6) 0.081(10) 0.006(6) 0.026(8) 0.013(7) B10 0.090(10) 0.047(8) 0.114(12) 0.011(7) -0.024(9) -0.023(7) B11 0.097(10) 0.038(7) 0.098(10) 0.019(7) 0.018(8) -0.006(7) C2 0.065(7) 0.072(7) 0.076(7) 0.041(6) -0.009(6) 0.008(6) O2 0.050(5) 0.149(8) 0.118(7) 0.042(6) -0.013(5) -0.021(5) C3 0.072(7) 0.041(6) 0.084(8) 0.016(6) -0.021(6) -0.002(5) O3 0.142(7) 0.077(5) 0.077(5) -0.019(4) -0.040(5) -0.017(5) C4 0.064(6) 0.047(6) 0.067(7) 0.015(5) 0.014(5) 0.013(5) O4 0.088(5) 0.122(7) 0.048(4) 0.017(4) 0.020(4) 0.015(5) O5 0.088(5) 0.080(5) 0.068(5) 0.019(4) -0.022(4) 0.002(4) C5 0.188(15) 0.161(14) 0.064(9) -0.005(9) -0.043(9) -0.001(12) C6 0.096(10) 0.109(11) 0.127(11) 0.043(9) -0.022(9) 0.023(9) C7 0.098(11) 0.168(15) 0.121(12) 0.011(11) -0.055(9) -0.023(11) C8 0.121(15) 0.19(2) 0.21(2) 0.073(19) -0.049(17) -0.012(15) C9 0.111(15) 0.23(3) 0.39(4) -0.09(3) -0.08(2) 0.053(15) P 0.0442(12) 0.0331(12) 0.0388(12) 0.0009(10) -0.0009(9) -0.0004(11) C11 0.053(5) 0.029(5) 0.043(5) 0.007(4) 0.001(4) 0.004(4) C12 0.051(5) 0.091(7) 0.047(5) -0.007(6) 0.003(4) -0.009(6) C13 0.058(7) 0.149(11) 0.071(7) 0.006(9) 0.011(6) -0.026(8) C14 0.058(7) 0.058(7) 0.094(9) 0.010(6) 0.027(6) 0.005(5) C15 0.102(9) 0.052(6) 0.047(6) 0.013(5) 0.031(6) 0.022(6) C16 0.059(6) 0.066(7) 0.045(5) -0.005(5) -0.001(5) 0.015(5) C21 0.047(5) 0.042(5) 0.037(4) 0.000(5) 0.001(4) -0.001(5) C22 0.088(7) 0.050(6) 0.033(6) 0.004(4) 0.003(5) -0.006(5) C23 0.104(9) 0.054(7) 0.040(6) 0.013(5) 0.007(6) -0.005(6) C24 0.087(7) 0.085(8) 0.038(5) 0.004(7) -0.002(5) 0.001(7) C25 0.081(7) 0.061(7) 0.055(6) -0.018(5) -0.016(5) -0.014(5) C26 0.070(6) 0.045(5) 0.051(6) 0.011(4) -0.015(5) -0.014(5) C31 0.045(5) 0.039(5) 0.040(5) 0.001(4) -0.005(4) 0.000(4) C32 0.071(7) 0.032(5) 0.073(7) -0.001(5) 0.013(5) -0.008(5) C33 0.079(7) 0.043(6) 0.082(7) 0.005(6) 0.007(6) -0.021(6) C34 0.107(9) 0.036(5) 0.061(7) 0.008(5) -0.011(7) -0.019(7) C35 0.095(9) 0.038(6) 0.064(7) -0.003(5) -0.014(6) 0.014(6) C36 0.062(6) 0.046(6) 0.064(6) -0.001(5) -0.014(5) 0.007(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W C2 1.957(10) . ? W C3 1.968(10) . ? W C4 2.012(9) . ? W B3 2.340(9) . ? W B4 2.377(9) . ? W B5 2.379(9) . ? W B2 2.380(8) . ? W C1 2.380(9) . ? W P 2.546(2) . ? C1 B2 1.687(15) . ? C1 B5 1.691(14) . ? C1 B6 1.712(14) . ? C1 B10 1.720(14) . ? B2 B6 1.755(15) . ? B2 B3 1.777(15) . ? B2 B7 1.799(14) . ? B3 O5 1.575(11) . ? B3 B7 1.768(15) . ? B3 B4 1.780(15) . ? B3 B8 1.781(16) . ? B4 B9 1.747(16) . ? B4 B5 1.801(15) . ? B4 B8 1.810(15) . ? B5 B9 1.737(14) . ? B5 B10 1.751(16) . ? B6 B7 1.749(17) . ? B6 B10 1.753(18) . ? B6 B11 1.760(16) . ? B7 B11 1.757(17) . ? B7 B8 1.758(16) . ? B8 B9 1.739(17) . ? B8 B11 1.739(17) . ? B9 B10 1.755(17) . ? B9 B11 1.766(17) . ? B10 B11 1.738(17) . ? C2 O2 1.149(9) . ? C3 O3 1.154(10) . ? C4 O4 1.155(9) . ? O5 C5 1.459(11) . ? O5 C6 1.476(11) . ? C6 C7 1.477(15) . ? C7 C8 1.54(2) . ? C8 C9 1.43(2) . ? P C11 1.824(8) . ? P C31 1.828(8) . ? P C21 1.828(7) . ? C11 C16 1.364(10) . ? C11 C12 1.373(10) . ? C12 C13 1.371(11) . ? C13 C14 1.344(13) . ? C14 C15 1.343(13) . ? C15 C16 1.389(12) . ? C21 C22 1.369(10) . ? C21 C26 1.379(11) . ? C22 C23 1.383(11) . ? C23 C24 1.360(13) . ? C24 C25 1.375(12) . ? C25 C26 1.387(11) . ? C31 C32 1.380(11) . ? C31 C36 1.383(11) . ? C32 C33 1.359(11) . ? C33 C34 1.361(13) . ? C34 C35 1.353(13) . ? C35 C36 1.372(12) . ? 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 C2 W C3 76.0(4) . . ? C2 W C4 73.7(4) . . ? C3 W C4 122.7(3) . . ? C2 W B3 87.8(3) . . ? C3 W B3 90.3(3) . . ? C4 W B3 135.0(3) . . ? C2 W B4 84.1(4) . . ? C3 W B4 131.5(3) . . ? C4 W B4 92.0(3) . . ? B3 W B4 44.4(4) . . ? C2 W B5 122.1(4) . . ? C3 W B5 154.4(4) . . ? C4 W B5 81.8(3) . . ? B3 W B5 73.5(4) . . ? B4 W B5 44.6(4) . . ? C2 W B2 126.3(4) . . ? C3 W B2 81.4(4) . . ? C4 W B2 154.0(4) . . ? B3 W B2 44.2(4) . . ? B4 W B2 75.7(4) . . ? B5 W B2 73.0(4) . . ? C2 W C1 156.2(3) . . ? C3 W C1 114.3(4) . . ? C4 W C1 113.0(3) . . ? B3 W C1 71.2(4) . . ? B4 W C1 72.9(4) . . ? B5 W C1 41.7(3) . . ? B2 W C1 41.6(4) . . ? C2 W P 117.9(2) . . ? C3 W P 76.1(2) . . ? C4 W P 77.0(2) . . ? B3 W P 145.8(3) . . ? B4 W P 150.3(3) . . ? B5 W P 105.8(2) . . ? B2 W P 102.4(2) . . ? C1 W P 85.8(2) . . ? B2 C1 B5 113.3(8) . . ? B2 C1 B6 62.2(6) . . ? B5 C1 B6 112.3(7) . . ? B2 C1 B10 112.8(8) . . ? B5 C1 B10 61.8(7) . . ? B6 C1 B10 61.4(7) . . ? B2 C1 W 69.1(5) . . ? B5 C1 W 69.0(5) . . ? B6 C1 W 126.9(7) . . ? B10 C1 W 126.6(7) . . ? C1 B2 B6 59.6(6) . . ? C1 B2 B3 105.0(8) . . ? B6 B2 B3 106.4(8) . . ? C1 B2 B7 105.1(8) . . ? B6 B2 B7 58.9(6) . . ? B3 B2 B7 59.3(6) . . ? C1 B2 W 69.3(5) . . ? B6 B2 W 124.8(7) . . ? B3 B2 W 67.0(5) . . ? B7 B2 W 122.3(7) . . ? O5 B3 B7 113.0(7) . . ? O5 B3 B2 122.6(8) . . ? B7 B3 B2 61.0(6) . . ? O5 B3 B4 123.4(8) . . ? B7 B3 B4 109.7(8) . . ? B2 B3 B4 109.9(7) . . ? O5 B3 B8 114.7(7) . . ? B7 B3 B8 59.4(6) . . ? B2 B3 B8 108.4(8) . . ? B4 B3 B8 61.1(6) . . ? O5 B3 W 110.9(6) . . ? B7 B3 W 125.5(7) . . ? B2 B3 W 68.8(5) . . ? B4 B3 W 68.6(4) . . ? B8 B3 W 124.9(7) . . ? B9 B4 B3 105.1(8) . . ? B9 B4 B5 58.6(6) . . ? B3 B4 B5 104.0(7) . . ? B9 B4 B8 58.5(7) . . ? B3 B4 B8 59.5(6) . . ? B5 B4 B8 104.5(8) . . ? B9 B4 W 122.0(7) . . ? B3 B4 W 67.1(5) . . ? B5 B4 W 67.7(4) . . ? B8 B4 W 122.1(7) . . ? C1 B5 B9 106.6(8) . . ? C1 B5 B10 59.9(6) . . ? B9 B5 B10 60.4(6) . . ? C1 B5 B4 107.7(8) . . ? B9 B5 B4 59.2(6) . . ? B10 B5 B4 108.9(8) . . ? C1 B5 W 69.3(5) . . ? B9 B5 W 122.4(7) . . ? B10 B5 W 125.3(7) . . ? B4 B5 W 67.6(5) . . ? C1 B6 B7 106.3(8) . . ? C1 B6 B10 59.5(6) . . ? B7 B6 B10 107.8(9) . . ? C1 B6 B2 58.2(6) . . ? B7 B6 B2 61.8(6) . . ? B10 B6 B2 108.0(8) . . ? C1 B6 B11 105.8(8) . . ? B7 B6 B11 60.1(7) . . ? B10 B6 B11 59.3(7) . . ? B2 B6 B11 109.3(8) . . ? B6 B7 B11 60.3(7) . . ? B6 B7 B8 108.0(9) . . ? B11 B7 B8 59.3(7) . . ? B6 B7 B3 107.1(8) . . ? B11 B7 B3 107.4(8) . . ? B8 B7 B3 60.7(7) . . ? B6 B7 B2 59.3(6) . . ? B11 B7 B2 107.5(8) . . ? B8 B7 B2 108.5(8) . . ? B3 B7 B2 59.7(6) . . ? B9 B8 B11 61.0(7) . . ? B9 B8 B7 108.1(9) . . ? B11 B8 B7 60.3(7) . . ? B9 B8 B3 105.4(8) . . ? B11 B8 B3 107.6(8) . . ? B7 B8 B3 60.0(6) . . ? B9 B8 B4 58.9(6) . . ? B11 B8 B4 109.1(8) . . ? B7 B8 B4 108.8(8) . . ? B3 B8 B4 59.4(6) . . ? B5 B9 B8 110.5(9) . . ? B5 B9 B4 62.2(6) . . ? B8 B9 B4 62.6(7) . . ? B5 B9 B10 60.2(7) . . ? B8 B9 B10 107.9(9) . . ? B4 B9 B10 111.2(8) . . ? B5 B9 B11 108.0(8) . . ? B8 B9 B11 59.5(7) . . ? B4 B9 B11 110.8(9) . . ? B10 B9 B11 59.2(7) . . ? C1 B10 B11 106.4(9) . . ? C1 B10 B5 58.3(6) . . ? B11 B10 B5 108.6(9) . . ? C1 B10 B6 59.0(6) . . ? B11 B10 B6 60.6(7) . . ? B5 B10 B6 107.5(8) . . ? C1 B10 B9 104.6(8) . . ? B11 B10 B9 60.7(7) . . ? B5 B10 B9 59.4(7) . . ? B6 B10 B9 108.1(9) . . ? B10 B11 B8 108.7(8) . . ? B10 B11 B7 108.1(8) . . ? B8 B11 B7 60.4(7) . . ? B10 B11 B6 60.1(7) . . ? B8 B11 B6 108.3(8) . . ? B7 B11 B6 59.6(7) . . ? B10 B11 B9 60.1(7) . . ? B8 B11 B9 59.5(7) . . ? B7 B11 B9 107.0(8) . . ? B6 B11 B9 107.2(8) . . ? O2 C2 W 178.6(8) . . ? O3 C3 W 174.7(8) . . ? O4 C4 W 176.9(7) . . ? C5 O5 C6 115.8(8) . . ? C5 O5 B3 117.6(8) . . ? C6 O5 B3 117.5(8) . . ? O5 C6 C7 112.9(12) . . ? C6 C7 C8 113.3(14) . . ? C9 C8 C7 110.7(17) . . ? C11 P C31 103.0(4) . . ? C11 P C21 103.6(3) . . ? C31 P C21 103.8(4) . . ? C11 P W 115.2(2) . . ? C31 P W 114.4(3) . . ? C21 P W 115.2(3) . . ? C16 C11 C12 116.7(8) . . ? C16 C11 P 120.4(6) . . ? C12 C11 P 122.9(6) . . ? C13 C12 C11 122.3(8) . . ? C14 C13 C12 119.8(9) . . ? C15 C14 C13 119.8(9) . . ? C14 C15 C16 120.7(9) . . ? C11 C16 C15 120.7(9) . . ? C22 C21 C26 118.6(7) . . ? C22 C21 P 121.9(6) . . ? C26 C21 P 119.5(6) . . ? C21 C22 C23 120.9(8) . . ? C24 C23 C22 119.5(9) . . ? C23 C24 C25 121.4(8) . . ? C24 C25 C26 118.2(8) . . ? C21 C26 C25 121.4(8) . . ? C32 C31 C36 117.1(8) . . ? C32 C31 P 120.9(6) . . ? C36 C31 P 121.9(7) . . ? C33 C32 C31 121.9(9) . . ? C32 C33 C34 119.9(10) . . ? C35 C34 C33 119.9(9) . . ? C34 C35 C36 120.6(10) . . ? C35 C36 C31 120.7(9) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 0.856 _refine_diff_density_min -0.626 _refine_diff_density_rms 0.018 #===END data_33 _database_code_CSD 157562 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27.50 H38 B10 N O3 P W' _chemical_formula_weight 753.51 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' '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' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.042(3) _cell_length_b 21.716(3) _cell_length_c 17.268(3) _cell_angle_alpha 90.00 _cell_angle_beta 129.571(14) _cell_angle_gamma 90.00 _cell_volume 6660(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 20 _exptl_crystal_description needles _exptl_crystal_colour yellow _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.521 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2984 _exptl_absorpt_coefficient_mu 3.591 _exptl_absorpt_correction_type Semi-Empirical _exptl_absorpt_correction_T_min 0.923 _exptl_absorpt_correction_T_max 0.844 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method /w-2/q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 5.04 _diffrn_reflns_number 11854 _diffrn_reflns_av_R_equivalents 0.0531 _diffrn_reflns_av_sigmaI/netI 0.0703 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 24.99 _reflns_number_total 5798 _reflns_number_gt 3945 _reflns_threshold_expression >2sigma(I) _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^)+(0.0301P)^2^+0.6149P] 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 5798 _refine_ls_number_parameters 387 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0763 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.0724 _refine_ls_wR_factor_gt 0.0646 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W W 0.680744(14) 0.536736(11) 0.312598(19) 0.03721(9) Uani 1 1 d . . . C1 C 0.8149(3) 0.5375(3) 0.4452(5) 0.0537(17) Uani 1 1 d . . . H1 H 0.8299 0.4884 0.4639 0.064 Uiso 1 1 calc R . . B2 B 0.7702(4) 0.5729(4) 0.4818(6) 0.0463(19) Uani 1 1 d . . . H2 H 0.7553 0.5502 0.5242 0.056 Uiso 1 1 calc R . . B3 B 0.7154(4) 0.6334(3) 0.3934(6) 0.0447(19) Uani 1 1 d . . . B4 B 0.7278(4) 0.6297(3) 0.2991(6) 0.048(2) Uani 1 1 d . . . H4 H 0.6853 0.6460 0.2210 0.057 Uiso 1 1 calc R . . B5 B 0.7909(4) 0.5659(4) 0.3369(6) 0.052(2) Uani 1 1 d . . . H5 H 0.7893 0.5378 0.2823 0.062 Uiso 1 1 calc R . . B6 B 0.8670(5) 0.5872(4) 0.5437(7) 0.057(2) Uani 1 1 d . . . H6 H 0.9120 0.5733 0.6226 0.069 Uiso 1 1 calc R . . B7 B 0.8054(4) 0.6495(4) 0.5089(6) 0.052(2) Uani 1 1 d . . . H7 H 0.8102 0.6775 0.5663 0.062 Uiso 1 1 calc R . . B8 B 0.7816(4) 0.6840(4) 0.4002(6) 0.053(2) Uani 1 1 d . . . H8 H 0.7712 0.7339 0.3858 0.064 Uiso 1 1 calc R . . B9 B 0.8266(5) 0.6414(4) 0.3649(6) 0.058(2) Uani 1 1 d . . . H9 H 0.8456 0.6630 0.3266 0.069 Uiso 1 1 calc R . . B10 B 0.8784(5) 0.5831(4) 0.4522(7) 0.062(2) Uani 1 1 d . . . H10 H 0.9313 0.5663 0.4713 0.075 Uiso 1 1 calc R . . B11 B 0.8717(5) 0.6548(4) 0.4915(6) 0.055(2) Uani 1 1 d . . . H11 H 0.9205 0.6862 0.5375 0.066 Uiso 1 1 calc R . . C2 C 0.5799(4) 0.5727(3) 0.2194(5) 0.0533(18) Uani 1 1 d . . . O2 O 0.5221(3) 0.5965(2) 0.1666(4) 0.0815(18) Uani 1 1 d . . . C3 C 0.6259(4) 0.5061(3) 0.3591(5) 0.0478(17) Uani 1 1 d . . . O3 O 0.5918(3) 0.4906(2) 0.3830(4) 0.0724(16) Uani 1 1 d . . . C4 C 0.6452(4) 0.5164(3) 0.1744(6) 0.0499(18) Uani 1 1 d . . . O4 O 0.6246(3) 0.5088(2) 0.0954(4) 0.0764(17) Uani 1 1 d . . . P P 0.69375(9) 0.41969(7) 0.31601(13) 0.0398(4) Uani 1 1 d . . . C11 C 0.7771(3) 0.3962(3) 0.3313(5) 0.0461(17) Uani 1 1 d . . . C12 C 0.7798(4) 0.4093(3) 0.2553(6) 0.061(2) Uani 1 1 d . . . H12 H 0.7377 0.4260 0.1949 0.073 Uiso 1 1 calc R . . C13 C 0.8445(5) 0.3979(4) 0.2681(7) 0.078(2) Uani 1 1 d . . . H13 H 0.8458 0.4064 0.2162 0.093 Uiso 1 1 calc R . . C14 C 0.9063(5) 0.3743(4) 0.3563(7) 0.080(3) Uani 1 1 d . . . H14 H 0.9503 0.3674 0.3654 0.097 Uiso 1 1 calc R . . C15 C 0.9044(4) 0.3606(4) 0.4312(7) 0.086(3) Uani 1 1 d . . . H15 H 0.9470 0.3440 0.4912 0.104 Uiso 1 1 calc R . . C16 C 0.8402(4) 0.3710(3) 0.4199(6) 0.065(2) Uani 1 1 d . . . H16 H 0.8393 0.3611 0.4718 0.078 Uiso 1 1 calc R . . C21 C 0.6163(3) 0.3794(3) 0.2040(4) 0.0381(15) Uani 1 1 d . . . C22 C 0.5431(4) 0.4014(3) 0.1505(5) 0.0528(18) Uani 1 1 d . . . H22 H 0.5352 0.4384 0.1701 0.063 Uiso 1 1 calc R . . C23 C 0.4822(4) 0.3700(3) 0.0693(5) 0.061(2) Uani 1 1 d . . . H23 H 0.4335 0.3852 0.0347 0.074 Uiso 1 1 calc R . . C24 C 0.4936(4) 0.3162(3) 0.0396(6) 0.063(2) Uani 1 1 d . . . H24 H 0.4525 0.2945 -0.0153 0.075 Uiso 1 1 calc R . . C25 C 0.5648(4) 0.2940(3) 0.0900(6) 0.064(2) Uani 1 1 d . . . H25 H 0.5724 0.2575 0.0690 0.076 Uiso 1 1 calc R . . C26 C 0.6253(4) 0.3251(3) 0.1713(5) 0.0549(19) Uani 1 1 d . . . H26 H 0.6736 0.3093 0.2053 0.066 Uiso 1 1 calc R . . C31 C 0.7030(4) 0.3790(3) 0.4165(5) 0.0483(17) Uani 1 1 d . . . C32 C 0.6690(4) 0.3234(3) 0.4001(6) 0.062(2) Uani 1 1 d . . . H32 H 0.6390 0.3056 0.3362 0.075 Uiso 1 1 calc R . . C33 C 0.6795(5) 0.2935(4) 0.4796(7) 0.079(3) Uani 1 1 d . . . H33 H 0.6567 0.2553 0.4685 0.094 Uiso 1 1 calc R . . C34 C 0.7223(5) 0.3188(4) 0.5730(7) 0.071(2) Uani 1 1 d . . . H34 H 0.7289 0.2981 0.6254 0.085 Uiso 1 1 calc R . . C35 C 0.7554(5) 0.3740(4) 0.5895(6) 0.079(3) Uani 1 1 d . . . H35 H 0.7846 0.3918 0.6533 0.094 Uiso 1 1 calc R . . C36 C 0.7460(4) 0.4041(3) 0.5118(5) 0.064(2) Uani 1 1 d . . . H36 H 0.7692 0.4422 0.5238 0.077 Uiso 1 1 calc R . . N N 0.6527(4) 0.6682(3) 0.3879(6) 0.081(2) Uani 1 1 d . . . C5 C 0.6108(6) 0.7046(6) 0.3401(11) 0.142(6) Uani 1 1 d . . . H5A H 0.5801 0.7189 0.3540 0.171 Uiso 1 1 calc R . . C6 C 0.6025(6) 0.7315(5) 0.2531(8) 0.109(4) Uani 1 1 d . . . H6A H 0.5639 0.7627 0.2208 0.163 Uiso 1 1 calc R . . H6B H 0.5886 0.6994 0.2055 0.163 Uiso 1 1 calc R . . H6C H 0.6496 0.7496 0.2773 0.163 Uiso 1 1 calc R . . C7 C 0.6493(4) 0.6477(4) 0.4776(7) 0.088(3) Uani 1 1 d . . . H7A H 0.6857 0.6156 0.5181 0.132 Uiso 1 1 calc R . . H7B H 0.5996 0.6326 0.4474 0.132 Uiso 1 1 calc R . . H7C H 0.6606 0.6828 0.5193 0.132 Uiso 1 1 calc R . . C91 C 0.5000 0.2102(4) 0.2500 0.304(10) Uani 1 2 d SD . . H91A H 0.5066 0.2414 0.2945 0.456 Uiso 1 1 calc R . . H91B H 0.4485 0.2099 0.1894 0.456 Uiso 1 1 calc R . . H91C H 0.5322 0.2189 0.2340 0.456 Uiso 1 1 calc R . . C92 C 0.5191(4) 0.1510(4) 0.2981(6) 0.304(10) Uani 1 1 d D . . H92A H 0.4871 0.1425 0.3152 0.365 Uiso 1 1 calc R . . H92B H 0.5710 0.1514 0.3597 0.365 Uiso 1 1 calc R . . C93 C 0.5087(4) 0.1003(4) 0.2279(6) 0.304(10) Uani 1 1 d . . . H93A H 0.5447 0.1025 0.2163 0.365 Uiso 1 1 calc R . . H93B H 0.4576 0.0972 0.1649 0.365 Uiso 1 1 calc R . . C94 C 0.5287(4) 0.0503(4) 0.3079(4) 0.304(10) Uani 1 1 d . . . H94A H 0.5400 0.0106 0.2946 0.365 Uiso 1 1 calc R . . H94B H 0.5699 0.0632 0.3760 0.365 Uiso 1 1 calc R . . C95 C 0.4587(4) 0.0503(4) 0.2879(6) 0.304(10) Uani 1 1 d . . . H95A H 0.4605 0.0213 0.3314 0.456 Uiso 1 1 calc R . . H95B H 0.4193 0.0388 0.2191 0.456 Uiso 1 1 calc R . . H95C H 0.4488 0.0907 0.2995 0.456 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 W 0.03688(13) 0.03474(13) 0.04056(14) -0.00342(16) 0.02496(11) -0.00335(15) C1 0.047(4) 0.047(4) 0.059(4) -0.009(4) 0.031(4) -0.009(4) B2 0.048(5) 0.047(5) 0.041(5) -0.008(4) 0.027(4) -0.010(4) B3 0.041(4) 0.046(5) 0.047(5) -0.010(4) 0.028(4) -0.009(4) B4 0.050(5) 0.044(5) 0.052(5) -0.006(4) 0.033(4) -0.013(4) B5 0.054(5) 0.052(5) 0.061(6) -0.015(4) 0.042(5) -0.010(4) B6 0.048(5) 0.056(5) 0.048(5) -0.003(4) 0.022(4) -0.011(4) B7 0.054(5) 0.047(5) 0.054(5) -0.015(4) 0.034(4) -0.010(4) B8 0.052(5) 0.045(5) 0.057(5) -0.009(4) 0.032(5) -0.012(4) B9 0.058(5) 0.067(6) 0.059(6) -0.015(5) 0.043(5) -0.025(5) B10 0.045(5) 0.073(6) 0.073(6) -0.016(5) 0.039(5) -0.012(4) B11 0.055(5) 0.053(5) 0.061(6) -0.016(4) 0.039(5) -0.022(4) C2 0.052(5) 0.045(4) 0.057(5) -0.006(4) 0.032(4) -0.005(4) O2 0.049(3) 0.072(4) 0.097(5) 0.011(3) 0.035(3) 0.010(3) C3 0.042(4) 0.043(4) 0.054(4) -0.009(3) 0.029(4) -0.005(3) O3 0.080(4) 0.067(3) 0.105(5) -0.001(3) 0.075(4) -0.007(3) C4 0.055(4) 0.042(4) 0.048(4) 0.007(3) 0.031(4) -0.002(3) O4 0.100(4) 0.076(4) 0.045(3) 0.005(3) 0.042(3) 0.007(3) P 0.0407(10) 0.0365(9) 0.0418(10) 0.0004(8) 0.0261(9) 0.0021(7) C11 0.040(4) 0.043(4) 0.051(4) -0.006(3) 0.027(4) 0.004(3) C12 0.054(5) 0.076(5) 0.053(5) 0.001(4) 0.034(4) 0.019(4) C13 0.064(6) 0.101(7) 0.083(6) -0.015(5) 0.053(5) 0.001(5) C14 0.046(5) 0.103(7) 0.086(7) -0.028(6) 0.039(5) 0.004(5) C15 0.041(5) 0.112(8) 0.067(6) 0.001(5) 0.016(5) 0.025(5) C16 0.052(5) 0.071(5) 0.061(5) 0.011(4) 0.031(4) 0.021(4) C21 0.048(4) 0.031(3) 0.039(4) 0.000(3) 0.029(3) -0.001(3) C22 0.049(4) 0.040(4) 0.062(5) -0.012(3) 0.032(4) 0.001(3) C23 0.043(4) 0.051(5) 0.068(5) -0.004(4) 0.026(4) -0.003(3) C24 0.057(5) 0.051(5) 0.060(5) -0.014(4) 0.028(4) -0.015(4) C25 0.075(5) 0.045(4) 0.074(6) -0.024(4) 0.049(5) -0.004(4) C26 0.056(5) 0.051(4) 0.061(5) -0.010(4) 0.039(4) 0.004(4) C31 0.059(4) 0.047(4) 0.051(4) 0.009(3) 0.040(4) 0.012(3) C32 0.089(6) 0.047(5) 0.064(5) 0.010(4) 0.054(5) 0.003(4) C33 0.112(7) 0.060(5) 0.087(7) 0.003(5) 0.074(6) -0.009(5) C34 0.088(6) 0.072(6) 0.077(6) 0.032(5) 0.063(6) 0.024(5) C35 0.101(7) 0.074(6) 0.052(5) 0.011(4) 0.045(5) 0.008(5) C36 0.083(6) 0.055(5) 0.052(5) 0.004(4) 0.043(5) -0.003(4) N 0.049(4) 0.051(4) 0.112(7) -0.034(4) 0.037(5) -0.007(3) C5 0.063(7) 0.093(10) 0.186(15) -0.086(10) 0.040(9) -0.024(6) C6 0.104(8) 0.083(8) 0.101(9) 0.007(6) 0.047(7) 0.001(6) C7 0.073(6) 0.097(7) 0.120(8) -0.062(6) 0.074(6) -0.037(5) C91 0.257(3) 0.260(4) 0.133(2) 0.000 0.0(12) 0.000 C92 0.257(3) 0.260(4) 0.133(2) 0.000 0.0(12) 0.000 C93 0.257(3) 0.260(4) 0.133(2) 0.000 0.0(12) 0.000 C94 0.257(3) 0.260(4) 0.133(2) 0.000 0.0(12) 0.000 C95 0.257(3) 0.260(4) 0.133(2) 0.000 0.0(12) 0.000 _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 W C2 1.968(8) . ? W C3 1.993(7) . ? W C4 2.020(8) . ? W B3 2.370(7) . ? W B4 2.376(7) . ? W B5 2.375(8) . ? W B2 2.400(7) . ? W C1 2.403(6) . ? W P 2.555(2) . ? C1 B5 1.686(10) . ? C1 B2 1.690(10) . ? C1 B6 1.695(10) . ? C1 B10 1.700(10) . ? B2 B7 1.772(10) . ? B2 B6 1.774(11) . ? B2 B3 1.780(11) . ? B3 N 1.578(10) . ? B3 B7 1.761(10) . ? B3 B8 1.815(10) . ? B3 B4 1.819(11) . ? B4 B8 1.786(10) . ? B4 B9 1.792(11) . ? B4 B5 1.795(11) . ? B5 B10 1.739(11) . ? B5 B9 1.750(11) . ? B6 B10 1.755(12) . ? B6 B11 1.757(11) . ? B6 B7 1.761(11) . ? B7 B11 1.733(11) . ? B7 B8 1.746(12) . ? B8 B11 1.732(12) . ? B8 B9 1.757(12) . ? B9 B10 1.726(12) . ? B9 B11 1.739(11) . ? B10 B11 1.738(12) . ? C2 O2 1.142(7) . ? C3 O3 1.150(7) . ? C4 O4 1.136(8) . ? P C21 1.807(6) . ? P C31 1.828(7) . ? P C11 1.830(6) . ? C11 C12 1.377(9) . ? C11 C16 1.378(9) . ? C12 C13 1.378(9) . ? C13 C14 1.352(11) . ? C14 C15 1.349(11) . ? C15 C16 1.377(10) . ? C21 C26 1.373(8) . ? C21 C22 1.387(8) . ? C22 C23 1.371(9) . ? C23 C24 1.361(9) . ? C24 C25 1.360(9) . ? C25 C26 1.363(9) . ? C31 C32 1.362(9) . ? C31 C36 1.376(9) . ? C32 C33 1.387(10) . ? C33 C34 1.353(10) . ? C34 C35 1.346(10) . ? C35 C36 1.374(9) . ? N C5 1.129(12) . ? N C7 1.629(11) . ? C5 C6 1.48(2) . ? C91 C92 1.439(3) . ? C92 C93 1.540(5) . ? C93 C94 1.577(7) . ? C93 C95 1.418(4) . ? 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 C2 W C3 74.5(3) . . ? C2 W C4 75.2(3) . . ? C3 W C4 121.1(3) . . ? C2 W B3 85.0(3) . . ? C3 W B3 97.2(3) . . ? C4 W B3 128.7(3) . . ? C2 W B4 87.8(3) . . ? C3 W B4 140.6(3) . . ? C4 W B4 86.3(3) . . ? B3 W B4 45.4(3) . . ? C2 W B5 128.2(3) . . ? C3 W B5 153.7(3) . . ? C4 W B5 81.4(3) . . ? B3 W B5 74.8(3) . . ? B4 W B5 44.6(3) . . ? C2 W B2 121.2(3) . . ? C3 W B2 84.0(3) . . ? C4 W B2 154.2(3) . . ? B3 W B2 44.2(3) . . ? B4 W B2 75.5(3) . . ? B5 W B2 72.9(3) . . ? C2 W C1 155.9(3) . . ? C3 W C1 112.5(3) . . ? C4 W C1 115.7(3) . . ? B3 W C1 71.7(3) . . ? B4 W C1 72.3(3) . . ? B5 W C1 41.4(2) . . ? B2 W C1 41.4(2) . . ? C2 W P 118.3(2) . . ? C3 W P 75.64(19) . . ? C4 W P 76.27(18) . . ? B3 W P 151.5(2) . . ? B4 W P 142.58(19) . . ? B5 W P 99.4(2) . . ? B2 W P 107.51(19) . . ? C1 W P 85.66(18) . . ? B5 C1 B2 113.5(6) . . ? B5 C1 B6 113.5(6) . . ? B2 C1 B6 63.2(4) . . ? B5 C1 B10 61.8(5) . . ? B2 C1 B10 114.1(6) . . ? B6 C1 B10 62.3(5) . . ? B5 C1 W 68.6(3) . . ? B2 C1 W 68.9(3) . . ? B6 C1 W 128.0(5) . . ? B10 C1 W 126.6(5) . . ? C1 B2 B7 103.8(5) . . ? C1 B2 B6 58.5(4) . . ? B7 B2 B6 59.5(4) . . ? C1 B2 B3 106.3(6) . . ? B7 B2 B3 59.4(4) . . ? B6 B2 B3 108.5(5) . . ? C1 B2 W 69.6(3) . . ? B7 B2 W 121.5(5) . . ? B6 B2 W 124.4(5) . . ? B3 B2 W 67.0(3) . . ? N B3 B7 110.5(6) . . ? N B3 B2 121.9(6) . . ? B7 B3 B2 60.0(4) . . ? N B3 B8 114.3(5) . . ? B7 B3 B8 58.4(4) . . ? B2 B3 B8 106.4(5) . . ? N B3 B4 128.6(6) . . ? B7 B3 B4 106.1(5) . . ? B2 B3 B4 107.6(5) . . ? B8 B3 B4 58.9(4) . . ? N B3 W 115.6(4) . . ? B7 B3 W 123.7(5) . . ? B2 B3 W 68.9(3) . . ? B8 B3 W 121.9(5) . . ? B4 B3 W 67.7(3) . . ? B8 B4 B9 58.8(4) . . ? B8 B4 B5 104.8(6) . . ? B9 B4 B5 58.4(4) . . ? B8 B4 B3 60.4(4) . . ? B9 B4 B3 106.6(5) . . ? B5 B4 B3 105.1(5) . . ? B8 B4 W 122.6(5) . . ? B9 B4 W 122.1(5) . . ? B5 B4 W 67.9(3) . . ? B3 B4 W 66.9(3) . . ? C1 B5 B10 59.5(4) . . ? C1 B5 B9 105.7(6) . . ? B10 B5 B9 59.3(5) . . ? C1 B5 B4 107.5(6) . . ? B10 B5 B4 109.1(6) . . ? B9 B5 B4 60.7(4) . . ? C1 B5 W 70.0(3) . . ? B10 B5 W 125.8(5) . . ? B9 B5 W 123.8(5) . . ? B4 B5 W 67.5(3) . . ? C1 B6 B10 59.0(4) . . ? C1 B6 B11 104.5(6) . . ? B10 B6 B11 59.3(5) . . ? C1 B6 B7 104.1(6) . . ? B10 B6 B7 106.3(6) . . ? B11 B6 B7 59.0(5) . . ? C1 B6 B2 58.3(4) . . ? B10 B6 B2 107.4(6) . . ? B11 B6 B2 107.5(6) . . ? B7 B6 B2 60.2(4) . . ? B11 B7 B8 59.7(5) . . ? B11 B7 B6 60.4(5) . . ? B8 B7 B6 109.0(6) . . ? B11 B7 B3 110.2(6) . . ? B8 B7 B3 62.3(4) . . ? B6 B7 B3 110.0(6) . . ? B11 B7 B2 108.6(6) . . ? B8 B7 B2 109.8(6) . . ? B6 B7 B2 60.3(4) . . ? B3 B7 B2 60.5(4) . . ? B11 B8 B7 59.8(5) . . ? B11 B8 B9 59.8(5) . . ? B7 B8 B9 107.2(6) . . ? B11 B8 B4 109.1(6) . . ? B7 B8 B4 108.2(6) . . ? B9 B8 B4 60.8(4) . . ? B11 B8 B3 107.8(6) . . ? B7 B8 B3 59.3(4) . . ? B9 B8 B3 108.3(6) . . ? B4 B8 B3 60.7(4) . . ? B10 B9 B11 60.2(5) . . ? B10 B9 B5 60.0(5) . . ? B11 B9 B5 107.5(6) . . ? B10 B9 B8 108.2(6) . . ? B11 B9 B8 59.4(5) . . ? B5 B9 B8 108.0(6) . . ? B10 B9 B4 109.8(6) . . ? B11 B9 B4 108.5(6) . . ? B5 B9 B4 60.9(4) . . ? B8 B9 B4 60.4(4) . . ? C1 B10 B9 106.2(6) . . ? C1 B10 B11 105.1(6) . . ? B9 B10 B11 60.3(5) . . ? C1 B10 B5 58.7(4) . . ? B9 B10 B5 60.7(5) . . ? B11 B10 B5 108.1(6) . . ? C1 B10 B6 58.7(4) . . ? B9 B10 B6 109.3(6) . . ? B11 B10 B6 60.4(5) . . ? B5 B10 B6 108.0(6) . . ? B8 B11 B7 60.5(5) . . ? B8 B11 B10 108.8(6) . . ? B7 B11 B10 108.3(6) . . ? B8 B11 B9 60.8(5) . . ? B7 B11 B9 108.6(6) . . ? B10 B11 B9 59.5(5) . . ? B8 B11 B6 109.9(6) . . ? B7 B11 B6 60.6(5) . . ? B10 B11 B6 60.3(5) . . ? B9 B11 B6 108.6(6) . . ? O2 C2 W 176.4(6) . . ? O3 C3 W 176.8(6) . . ? O4 C4 W 175.5(6) . . ? C21 P C31 102.6(3) . . ? C21 P C11 104.3(3) . . ? C31 P C11 104.5(3) . . ? C21 P W 115.7(2) . . ? C31 P W 116.2(2) . . ? C11 P W 112.1(2) . . ? C12 C11 C16 118.6(7) . . ? C12 C11 P 118.9(5) . . ? C16 C11 P 122.2(6) . . ? C13 C12 C11 120.5(7) . . ? C14 C13 C12 119.9(8) . . ? C15 C14 C13 120.4(8) . . ? C14 C15 C16 120.9(8) . . ? C15 C16 C11 119.7(8) . . ? C26 C21 C22 117.1(6) . . ? C26 C21 P 123.1(5) . . ? C22 C21 P 119.7(5) . . ? C23 C22 C21 121.6(6) . . ? C24 C23 C22 119.4(7) . . ? C25 C24 C23 120.2(7) . . ? C24 C25 C26 120.3(6) . . ? C25 C26 C21 121.4(6) . . ? C32 C31 C36 118.5(7) . . ? C32 C31 P 121.6(6) . . ? C36 C31 P 119.9(5) . . ? C31 C32 C33 119.4(7) . . ? C34 C33 C32 121.3(8) . . ? C35 C34 C33 119.6(8) . . ? C34 C35 C36 119.9(8) . . ? C35 C36 C31 121.3(7) . . ? C5 N B3 134.9(12) . . ? C5 N C7 112.2(11) . . ? B3 N C7 113.9(7) . . ? N C5 C6 122.9(14) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.830 _refine_diff_density_min -0.480 _refine_diff_density_rms 0.102 #===END data_23 _database_code_CSD 157563 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H34 B10 N O3 P W' _chemical_formula_weight 743.47 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' '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' 'W' 'W' -0.8490 6.8722 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.679(2) _cell_length_b 18.962(4) _cell_length_c 18.669(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.23(3) _cell_angle_gamma 90.00 _cell_volume 3382.0(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 20 _exptl_crystal_description blocks _exptl_crystal_colour yellow _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1464 _exptl_absorpt_coefficient_mu 3.492 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.3286 _exptl_absorpt_correction_T_max 0.3938 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 4.25 _diffrn_reflns_number 6293 _diffrn_reflns_av_R_equivalents 0.0287 _diffrn_reflns_av_sigmaI/netI 0.0724 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 24.94 _reflns_number_total 5918 _reflns_number_gt 3908 _reflns_threshold_expression >2sigma(I) _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^)+(0.0777P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5918 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0930 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.0964 _refine_ls_wR_factor_gt 0.0805 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.002 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W W 0.09421(4) 0.148895(19) 0.27674(2) 0.03985(15) Uani 1 1 d . . . C1 C -0.0208(10) 0.0933(5) 0.1690(5) 0.048(2) Uani 1 1 d . . . H1 H 0.0241 0.0399 0.1716 0.058 Uiso 1 1 calc R . . B2 B -0.1388(12) 0.1140(6) 0.2261(6) 0.048(3) Uani 1 1 d . . . H2 H -0.1750 0.0787 0.2660 0.058 Uiso 1 1 calc R . . B3 B -0.1190(13) 0.2059(6) 0.2379(6) 0.046(3) Uani 1 1 d . . . B4 B 0.0121(13) 0.2404(7) 0.1915(7) 0.054(3) Uani 1 1 d . . . H4 H 0.0730 0.2883 0.2081 0.064 Uiso 1 1 calc R . . B5 B 0.0778(15) 0.1643(6) 0.1498(6) 0.056(3) Uani 1 1 d . . . H5 H 0.1865 0.1607 0.1397 0.067 Uiso 1 1 calc R . . B6 B -0.1900(14) 0.0992(7) 0.1304(8) 0.068(4) Uani 1 1 d . . . H6 H -0.2535 0.0531 0.1101 0.082 Uiso 1 1 calc R . . B7 B -0.2611(14) 0.1713(7) 0.1723(6) 0.059(4) Uani 1 1 d . . . H7 H -0.3715 0.1733 0.1797 0.071 Uiso 1 1 calc R . . B8 B -0.1669(14) 0.2476(7) 0.1515(7) 0.055(3) Uani 1 1 d . . . H8 H -0.2179 0.2995 0.1454 0.066 Uiso 1 1 calc R . . B9 B -0.0429(15) 0.2218(8) 0.0977(7) 0.065(4) Uani 1 1 d . . . H9 H -0.0110 0.2564 0.0560 0.077 Uiso 1 1 calc R . . B10 B -0.0589(14) 0.1307(8) 0.0852(6) 0.061(4) Uani 1 1 d . . . H10 H -0.0370 0.1055 0.0351 0.073 Uiso 1 1 calc R . . B11 B -0.2113(14) 0.1820(8) 0.0859(7) 0.064(4) Uani 1 1 d . . . H11 H -0.2899 0.1910 0.0372 0.076 Uiso 1 1 calc R . . C2 C 0.2864(12) 0.1853(6) 0.2733(6) 0.059(3) Uani 1 1 d . . . O2 O 0.3941(9) 0.2094(5) 0.2717(5) 0.084(3) Uani 1 1 d . . . C3 C 0.1230(14) 0.2248(6) 0.3489(6) 0.068(3) Uani 1 1 d . . . O3 O 0.1352(13) 0.2715(5) 0.3888(6) 0.125(4) Uani 1 1 d . . . C4 C 0.0461(11) 0.1072(6) 0.3684(5) 0.050(3) Uani 1 1 d . . . O4 O 0.0128(9) 0.0882(5) 0.4205(5) 0.088(3) Uani 1 1 d . . . P P 0.2455(3) 0.03834(13) 0.29127(13) 0.0392(6) Uani 1 1 d . . . C11 C 0.4109(10) 0.0455(5) 0.3538(5) 0.045(2) Uani 1 1 d . . . C12 C 0.4150(12) 0.0853(6) 0.4173(5) 0.057(3) Uani 1 1 d . . . H12 H 0.3356 0.1092 0.4263 0.069 Uiso 1 1 calc R . . C13 C 0.5379(15) 0.0890(7) 0.4664(6) 0.076(4) Uani 1 1 d . . . H13 H 0.5406 0.1154 0.5086 0.091 Uiso 1 1 calc R . . C14 C 0.6550(13) 0.0546(8) 0.4539(7) 0.075(4) Uani 1 1 d . . . H14 H 0.7366 0.0571 0.4878 0.090 Uiso 1 1 calc R . . C15 C 0.6528(12) 0.0168(8) 0.3921(7) 0.081(4) Uani 1 1 d . . . H15 H 0.7329 -0.0067 0.3835 0.097 Uiso 1 1 calc R . . C16 C 0.5315(11) 0.0131(7) 0.3418(6) 0.068(3) Uani 1 1 d . . . H16 H 0.5319 -0.0118 0.2989 0.082 Uiso 1 1 calc R . . C21 C 0.1671(9) -0.0414(5) 0.3208(5) 0.041(2) Uani 1 1 d . . . C22 C 0.0221(11) -0.0498(6) 0.3111(7) 0.072(4) Uani 1 1 d . . . H22 H -0.0350 -0.0128 0.2918 0.087 Uiso 1 1 calc R . . C23 C -0.0389(12) -0.1117(7) 0.3294(8) 0.087(4) Uani 1 1 d . . . H23 H -0.1358 -0.1163 0.3214 0.104 Uiso 1 1 calc R . . C24 C 0.0426(13) -0.1657(6) 0.3590(7) 0.072(4) Uani 1 1 d . . . H24 H 0.0019 -0.2068 0.3730 0.087 Uiso 1 1 calc R . . C25 C 0.1868(13) -0.1592(5) 0.3683(6) 0.063(3) Uani 1 1 d . . . H25 H 0.2435 -0.1965 0.3874 0.076 Uiso 1 1 calc R . . C26 C 0.2450(11) -0.0987(5) 0.3497(5) 0.051(3) Uani 1 1 d . . . H26 H 0.3421 -0.0954 0.3566 0.062 Uiso 1 1 calc R . . C31 C 0.2984(10) 0.0107(5) 0.2056(5) 0.046(2) Uani 1 1 d . . . C32 C 0.2348(11) -0.0458(6) 0.1672(5) 0.055(3) Uani 1 1 d . . . H32 H 0.1720 -0.0737 0.1874 0.066 Uiso 1 1 calc R . . C33 C 0.2639(13) -0.0610(8) 0.0994(6) 0.075(4) Uani 1 1 d . . . H33 H 0.2202 -0.0992 0.0739 0.090 Uiso 1 1 calc R . . C34 C 0.3565(15) -0.0207(8) 0.0687(6) 0.082(4) Uani 1 1 d . . . H34 H 0.3764 -0.0316 0.0228 0.099 Uiso 1 1 calc R . . C35 C 0.4204(12) 0.0367(8) 0.1066(6) 0.077(4) Uani 1 1 d . . . H35 H 0.4853 0.0636 0.0870 0.093 Uiso 1 1 calc R . . C36 C 0.3876(11) 0.0532(7) 0.1725(6) 0.065(3) Uani 1 1 d . . . H36 H 0.4253 0.0936 0.1962 0.078 Uiso 1 1 calc R . . N N -0.1772(10) 0.2457(5) 0.2983(5) 0.059(2) Uani 1 1 d . . . C5 C -0.2148(13) 0.2754(6) 0.3433(6) 0.065(3) Uani 1 1 d . . . C6 C -0.2650(15) 0.3156(7) 0.4031(7) 0.071(3) Uani 1 1 d . . . C7 C -0.239(3) 0.3887(8) 0.3914(11) 0.191(12) Uani 1 1 d . . . H7A H -0.1403 0.3964 0.3951 0.286 Uiso 1 1 calc R . . H7B H -0.2749 0.4164 0.4274 0.286 Uiso 1 1 calc R . . H7C H -0.2851 0.4023 0.3440 0.286 Uiso 1 1 calc R . . C8 C -0.4178(18) 0.3057(13) 0.3964(11) 0.190(12) Uani 1 1 d . . . H8A H -0.4378 0.2570 0.4046 0.285 Uiso 1 1 calc R . . H8B H -0.4617 0.3191 0.3485 0.285 Uiso 1 1 calc R . . H8C H -0.4532 0.3345 0.4316 0.285 Uiso 1 1 calc R . . C9 C -0.198(3) 0.2845(11) 0.4724(8) 0.185(12) Uani 1 1 d . . . H9A H -0.2242 0.2357 0.4740 0.278 Uiso 1 1 calc R . . H9B H -0.2291 0.3092 0.5119 0.278 Uiso 1 1 calc R . . H9C H -0.0985 0.2883 0.4765 0.278 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 W 0.0463(2) 0.0331(2) 0.0404(2) -0.0043(2) 0.00761(15) -0.0050(2) C1 0.047(6) 0.045(6) 0.052(6) -0.012(5) 0.003(5) 0.003(5) B2 0.037(6) 0.046(7) 0.061(8) 0.009(6) 0.008(6) -0.002(5) B3 0.057(8) 0.039(6) 0.048(7) -0.010(5) 0.021(6) 0.003(5) B4 0.060(8) 0.043(7) 0.059(7) 0.011(6) 0.013(6) -0.006(6) B5 0.066(8) 0.057(8) 0.048(7) 0.007(6) 0.020(6) 0.006(6) B6 0.054(8) 0.049(8) 0.088(10) -0.026(7) -0.024(7) 0.015(6) B7 0.049(7) 0.083(10) 0.042(6) 0.001(6) -0.002(5) 0.024(7) B8 0.066(8) 0.043(7) 0.056(7) 0.005(6) 0.008(6) 0.012(6) B9 0.068(9) 0.071(9) 0.056(8) 0.019(7) 0.015(7) 0.011(7) B10 0.057(8) 0.085(10) 0.036(6) -0.009(6) -0.006(5) 0.010(7) B11 0.048(8) 0.075(9) 0.065(9) 0.000(7) 0.000(6) 0.021(7) C2 0.057(7) 0.047(6) 0.071(8) 0.008(6) 0.002(6) -0.010(6) O2 0.061(6) 0.085(7) 0.101(7) 0.010(5) -0.003(5) -0.035(5) C3 0.085(9) 0.057(7) 0.056(7) -0.011(6) -0.008(6) 0.003(7) O3 0.183(12) 0.078(7) 0.100(7) -0.053(6) -0.018(7) 0.007(7) C4 0.052(7) 0.056(7) 0.043(6) -0.007(5) 0.012(5) -0.002(5) O4 0.093(7) 0.112(8) 0.066(6) 0.026(5) 0.034(5) 0.010(6) P 0.0377(13) 0.0398(14) 0.0401(13) -0.0049(10) 0.0063(11) -0.0053(11) C11 0.045(6) 0.049(6) 0.040(5) 0.002(5) 0.002(4) -0.013(5) C12 0.063(7) 0.057(7) 0.048(6) -0.014(5) -0.006(5) -0.001(6) C13 0.096(10) 0.069(8) 0.055(7) -0.010(6) -0.008(7) -0.008(8) C14 0.054(8) 0.094(10) 0.071(8) 0.003(8) -0.008(6) -0.015(8) C15 0.044(7) 0.117(12) 0.078(9) 0.003(8) 0.000(6) 0.015(7) C16 0.048(7) 0.095(10) 0.058(7) -0.020(7) 0.000(6) 0.003(7) C21 0.040(5) 0.035(5) 0.045(5) -0.002(4) 0.003(4) -0.005(4) C22 0.048(7) 0.041(6) 0.130(11) 0.023(7) 0.019(7) 0.002(5) C23 0.033(6) 0.067(8) 0.158(14) 0.006(9) 0.012(7) -0.017(6) C24 0.069(8) 0.037(7) 0.110(10) 0.012(6) 0.015(7) -0.008(6) C25 0.073(8) 0.041(7) 0.075(8) 0.006(5) 0.011(6) 0.013(6) C26 0.049(6) 0.046(6) 0.057(6) 0.008(5) 0.002(5) -0.003(5) C31 0.046(6) 0.055(6) 0.039(5) -0.009(5) 0.015(4) 0.003(5) C32 0.059(7) 0.057(6) 0.046(6) -0.015(5) 0.002(5) -0.003(6) C33 0.069(8) 0.096(10) 0.056(7) -0.024(7) -0.001(6) 0.004(8) C34 0.082(10) 0.114(12) 0.048(7) -0.018(7) 0.001(7) 0.033(9) C35 0.058(8) 0.120(12) 0.058(7) -0.004(8) 0.023(6) 0.004(8) C36 0.061(7) 0.082(8) 0.059(7) -0.016(6) 0.029(6) -0.016(7) N 0.077(7) 0.052(5) 0.049(5) -0.009(4) 0.016(5) 0.008(5) C5 0.082(9) 0.046(6) 0.067(8) -0.009(6) 0.016(7) 0.003(6) C6 0.097(10) 0.057(7) 0.066(8) -0.017(6) 0.033(7) 0.003(7) C7 0.38(4) 0.057(10) 0.173(19) -0.044(12) 0.15(2) -0.007(17) C8 0.094(14) 0.30(3) 0.18(2) -0.16(2) 0.046(14) -0.011(17) C9 0.31(3) 0.19(2) 0.063(11) 0.008(12) 0.053(15) 0.12(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W C3 1.961(11) . ? W C2 1.996(12) . ? W C4 2.006(11) . ? W B3 2.339(12) . ? W B5 2.367(12) . ? W C1 2.383(9) . ? W B2 2.395(11) . ? W B4 2.401(12) . ? W P 2.546(3) . ? C1 B6 1.684(15) . ? C1 B10 1.704(15) . ? C1 B5 1.721(16) . ? C1 B2 1.728(15) . ? B2 B3 1.762(17) . ? B2 B7 1.791(16) . ? B2 B6 1.797(18) . ? B3 N 1.538(13) . ? B3 B4 1.772(16) . ? B3 B8 1.789(16) . ? B3 B7 1.811(17) . ? B4 B8 1.779(18) . ? B4 B9 1.782(18) . ? B4 B5 1.802(17) . ? B5 B10 1.761(17) . ? B5 B9 1.771(18) . ? B6 B10 1.74(2) . ? B6 B7 1.768(17) . ? B6 B11 1.77(2) . ? B7 B11 1.769(18) . ? B7 B8 1.785(19) . ? B8 B11 1.750(18) . ? B8 B9 1.753(18) . ? B9 B10 1.747(19) . ? B9 B11 1.78(2) . ? B10 B11 1.769(18) . ? C2 O2 1.142(12) . ? C3 O3 1.150(13) . ? C4 O4 1.131(11) . ? P C21 1.816(9) . ? P C11 1.829(9) . ? P C31 1.832(9) . ? C11 C16 1.369(14) . ? C11 C12 1.401(13) . ? C12 C13 1.383(15) . ? C13 C14 1.359(17) . ? C14 C15 1.357(17) . ? C15 C16 1.382(15) . ? C21 C26 1.383(13) . ? C21 C22 1.395(13) . ? C22 C23 1.380(15) . ? C23 C24 1.355(16) . ? C24 C25 1.385(16) . ? C25 C26 1.346(14) . ? C31 C32 1.378(13) . ? C31 C36 1.395(14) . ? C32 C33 1.372(14) . ? C33 C34 1.373(18) . ? C34 C35 1.388(18) . ? C35 C36 1.356(14) . ? N C5 1.119(12) . ? C5 C6 1.495(15) . ? C6 C7 1.432(19) . ? C6 C9 1.47(2) . ? C6 C8 1.48(2) . ? 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 C3 W C2 74.8(5) . . ? C3 W C4 74.3(5) . . ? C2 W C4 120.6(4) . . ? C3 W B3 84.0(4) . . ? C2 W B3 127.6(4) . . ? C4 W B3 97.6(4) . . ? C3 W B5 125.2(5) . . ? C2 W B5 80.7(5) . . ? C4 W B5 156.2(4) . . ? B3 W B5 73.6(4) . . ? C3 W C1 154.2(4) . . ? C2 W C1 115.9(4) . . ? C4 W C1 113.9(4) . . ? B3 W C1 70.9(4) . . ? B5 W C1 42.5(4) . . ? C3 W B2 119.7(5) . . ? C2 W B2 155.1(4) . . ? C4 W B2 84.0(4) . . ? B3 W B2 43.7(4) . . ? B5 W B2 74.4(4) . . ? C1 W B2 42.4(4) . . ? C3 W B4 85.4(5) . . ? C2 W B4 86.5(4) . . ? C4 W B4 138.8(4) . . ? B3 W B4 43.9(4) . . ? B5 W B4 44.4(4) . . ? C1 W B4 72.5(4) . . ? B2 W B4 75.3(4) . . ? C3 W P 121.0(4) . . ? C2 W P 76.4(3) . . ? C4 W P 78.0(3) . . ? B3 W P 151.3(3) . . ? B5 W P 98.8(3) . . ? C1 W P 84.7(2) . . ? B2 W P 107.7(3) . . ? B4 W P 142.1(3) . . ? B6 C1 B10 61.8(8) . . ? B6 C1 B5 113.1(9) . . ? B10 C1 B5 61.9(7) . . ? B6 C1 B2 63.5(7) . . ? B10 C1 B2 113.9(8) . . ? B5 C1 B2 113.2(8) . . ? B6 C1 W 128.5(7) . . ? B10 C1 W 126.5(7) . . ? B5 C1 W 68.3(5) . . ? B2 C1 W 69.2(5) . . ? C1 B2 B3 103.4(8) . . ? C1 B2 B7 103.6(8) . . ? B3 B2 B7 61.3(7) . . ? C1 B2 B6 57.0(6) . . ? B3 B2 B6 106.6(8) . . ? B7 B2 B6 59.1(7) . . ? C1 B2 W 68.4(5) . . ? B3 B2 W 66.5(6) . . ? B7 B2 W 123.4(8) . . ? B6 B2 W 121.8(7) . . ? N B3 B2 122.1(9) . . ? N B3 B4 123.6(9) . . ? B2 B3 B4 112.1(8) . . ? N B3 B8 111.8(8) . . ? B2 B3 B8 108.5(8) . . ? B4 B3 B8 59.9(7) . . ? N B3 B7 110.2(9) . . ? B2 B3 B7 60.1(6) . . ? B4 B3 B7 109.2(8) . . ? B8 B3 B7 59.4(7) . . ? N B3 W 114.1(7) . . ? B2 B3 W 69.8(5) . . ? B4 B3 W 69.9(6) . . ? B8 B3 W 124.9(7) . . ? B7 B3 W 125.4(7) . . ? B3 B4 B8 60.5(7) . . ? B3 B4 B9 106.4(9) . . ? B8 B4 B9 59.0(7) . . ? B3 B4 B5 104.2(8) . . ? B8 B4 B5 105.5(9) . . ? B9 B4 B5 59.2(7) . . ? B3 B4 W 66.2(6) . . ? B8 B4 W 122.0(7) . . ? B9 B4 W 121.6(8) . . ? B5 B4 W 66.8(5) . . ? C1 B5 B10 58.6(7) . . ? C1 B5 B9 104.9(9) . . ? B10 B5 B9 59.3(8) . . ? C1 B5 B4 106.9(8) . . ? B10 B5 B4 107.9(9) . . ? B9 B5 B4 59.8(7) . . ? C1 B5 W 69.2(5) . . ? B10 B5 W 124.3(8) . . ? B9 B5 W 123.9(8) . . ? B4 B5 W 68.8(5) . . ? C1 B6 B10 59.7(7) . . ? C1 B6 B7 106.5(9) . . ? B10 B6 B7 108.4(10) . . ? C1 B6 B11 107.0(10) . . ? B10 B6 B11 60.5(8) . . ? B7 B6 B11 59.9(7) . . ? C1 B6 B2 59.4(6) . . ? B10 B6 B2 108.9(9) . . ? B7 B6 B2 60.3(7) . . ? B11 B6 B2 108.7(9) . . ? B6 B7 B11 60.2(8) . . ? B6 B7 B2 60.6(7) . . ? B11 B7 B2 109.2(9) . . ? B6 B7 B8 106.3(10) . . ? B11 B7 B8 59.0(8) . . ? B2 B7 B8 107.4(9) . . ? B6 B7 B3 105.7(8) . . ? B11 B7 B3 106.7(9) . . ? B2 B7 B3 58.6(6) . . ? B8 B7 B3 59.7(7) . . ? B11 B8 B9 61.0(8) . . ? B11 B8 B4 110.7(9) . . ? B9 B8 B4 60.6(7) . . ? B11 B8 B3 108.5(9) . . ? B9 B8 B3 106.9(8) . . ? B4 B8 B3 59.5(6) . . ? B11 B8 B7 60.0(7) . . ? B9 B8 B7 108.7(9) . . ? B4 B8 B7 110.1(9) . . ? B3 B8 B7 60.9(7) . . ? B10 B9 B8 107.3(10) . . ? B10 B9 B5 60.1(7) . . ? B8 B9 B5 108.0(9) . . ? B10 B9 B4 109.4(9) . . ? B8 B9 B4 60.4(7) . . ? B5 B9 B4 61.0(7) . . ? B10 B9 B11 60.2(8) . . ? B8 B9 B11 59.4(8) . . ? B5 B9 B11 108.5(10) . . ? B4 B9 B11 109.3(9) . . ? C1 B10 B6 58.5(7) . . ? C1 B10 B9 106.7(8) . . ? B6 B10 B9 109.3(10) . . ? C1 B10 B5 59.5(6) . . ? B6 B10 B5 108.5(9) . . ? B9 B10 B5 60.6(7) . . ? C1 B10 B11 106.3(9) . . ? B6 B10 B11 60.7(8) . . ? B9 B10 B11 60.8(8) . . ? B5 B10 B11 109.4(9) . . ? B8 B11 B10 106.5(9) . . ? B8 B11 B7 61.0(8) . . ? B10 B11 B7 107.0(9) . . ? B8 B11 B6 107.6(9) . . ? B10 B11 B6 58.8(8) . . ? B7 B11 B6 59.9(8) . . ? B8 B11 B9 59.6(8) . . ? B10 B11 B9 59.0(8) . . ? B7 B11 B9 108.3(9) . . ? B6 B11 B9 106.4(9) . . ? O2 C2 W 176.7(11) . . ? O3 C3 W 176.4(11) . . ? O4 C4 W 174.7(10) . . ? C21 P C11 103.5(4) . . ? C21 P C31 102.5(4) . . ? C11 P C31 103.8(5) . . ? C21 P W 117.2(3) . . ? C11 P W 115.9(3) . . ? C31 P W 112.3(3) . . ? C16 C11 C12 118.1(9) . . ? C16 C11 P 123.0(8) . . ? C12 C11 P 118.9(8) . . ? C13 C12 C11 119.6(11) . . ? C14 C13 C12 121.0(12) . . ? C13 C14 C15 120.0(11) . . ? C14 C15 C16 120.0(12) . . ? C11 C16 C15 121.3(11) . . ? C26 C21 C22 115.7(9) . . ? C26 C21 P 123.1(7) . . ? C22 C21 P 121.1(8) . . ? C23 C22 C21 121.8(11) . . ? C24 C23 C22 119.9(11) . . ? C23 C24 C25 119.6(10) . . ? C26 C25 C24 119.9(10) . . ? C25 C26 C21 123.1(10) . . ? C32 C31 C36 118.3(9) . . ? C32 C31 P 120.8(8) . . ? C36 C31 P 120.1(8) . . ? C33 C32 C31 120.3(11) . . ? C32 C33 C34 120.8(12) . . ? C33 C34 C35 119.4(12) . . ? C36 C35 C34 119.6(12) . . ? C35 C36 C31 121.4(12) . . ? C5 N B3 177.5(12) . . ? N C5 C6 179.5(13) . . ? C7 C6 C9 117.3(16) . . ? C7 C6 C8 107.9(17) . . ? C9 C6 C8 108.4(16) . . ? C7 C6 C5 107.2(11) . . ? C9 C6 C5 107.6(12) . . ? C8 C6 C5 108.3(12) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.94 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.918 _refine_diff_density_min -1.024 _refine_diff_density_rms 0.153