Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _journal_volume ? _journal_year ? _journal_page_first ? _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Mike Ward' 'Zoe R. Bell' 'Dante Gatteschi' 'J. Maher' 'J. A. McCleverty' 'E. McInnes' 'Thomas W. Munhoven' 'Keira M. Stobie' 'Federico, Totti' _publ_contact_author_name 'Prof. Mike Ward' _publ_contact_author_address ; Prof. Mike Ward School of Chemistry University of Bristol Cantock's Close Bristol BS8 1TS ; _publ_contact_author_email 'mike.ward@bristol.ac.uk' _publ_section_title ; Mono- and dinuclear tris(pyrazolyl)borato-oxo-tungsten(V) complexes with phenolate ligands: syntheses and structures, and magnetic, electrochemical and UV/Vis/NIR spectroscopic properties ; #======================================================= data_complex5a _database_code_CSD 192528 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H66 B2 Cl6 N16 O6 W2' _chemical_formula_weight 1661.27 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' Cl Cl 0.1484 0.1585 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.275(4) _cell_length_b 17.034(7) _cell_length_c 17.117(5) _cell_angle_alpha 78.73(2) _cell_angle_beta 75.15(2) _cell_angle_gamma 70.36(2) _cell_volume 3234.5(18) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.706 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1644 _exptl_absorpt_coefficient_mu 3.863 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.29 _exptl_absorpt_correction_T_max 0.47 _exptl_absorpt_process_details ? _exptl_special_details ; There is disorder about the N=N bond of the ligand in one molecule which required use of heavy geometric restraints to give a sensible geometry. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34035 _diffrn_reflns_av_R_equivalents 0.0747 _diffrn_reflns_av_sigmaI/netI 0.1316 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 27.51 _reflns_number_total 14664 _reflns_number_gt 7829 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0698P)^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 14664 _refine_ls_number_parameters 806 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.1468 _refine_ls_R_factor_gt 0.0652 _refine_ls_wR_factor_ref 0.1632 _refine_ls_wR_factor_gt 0.1384 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.27249(4) 0.38192(3) 0.13202(2) 0.04303(14) Uani 1 1 d . . . Cl1 Cl 0.3701(3) 0.29052(18) 0.22599(17) 0.0640(8) Uani 1 1 d . . . O1 O 0.1492(5) 0.4507(4) 0.2039(4) 0.0368(15) Uani 1 1 d . . . O48 O 0.3837(5) 0.4471(4) 0.1079(4) 0.0414(16) Uani 1 1 d . . . O57 O 0.7013(7) 0.7241(5) 0.5580(5) 0.078(3) Uani 1 1 d . . . H57A H 0.6452 0.7561 0.5876 0.117 Uiso 1 1 calc R . . N11 N 0.1688(6) 0.3012(4) 0.1322(4) 0.0284(17) Uani 1 1 d . . . N12 N 0.1579(6) 0.2811(5) 0.0612(4) 0.0313(17) Uani 1 1 d . . . N21 N 0.2056(6) 0.4511(5) 0.0252(4) 0.040(2) Uani 1 1 d . . . N22 N 0.1870(6) 0.4121(5) -0.0297(4) 0.0381(19) Uani 1 1 d . . . N31 N 0.4015(6) 0.3044(4) 0.0328(4) 0.0319(17) Uani 1 1 d . . . N32 N 0.3570(6) 0.2829(4) -0.0236(4) 0.0312(17) Uani 1 1 d . . . N47 N 0.5622(6) 0.5954(4) 0.2893(5) 0.0338(18) Uani 1 1 d . . . N58 N 0.5235(7) 0.5881(5) 0.3663(5) 0.0394(19) Uani 1 1 d . . . C13 C 0.0884(8) 0.2318(6) 0.0785(6) 0.042(2) Uani 1 1 d . . . C14 C 0.0492(8) 0.2219(6) 0.1613(6) 0.041(2) Uani 1 1 d . . . H14A H -0.0045 0.1918 0.1904 0.049 Uiso 1 1 calc R . . C15 C 0.1019(8) 0.2639(6) 0.1951(6) 0.038(2) Uani 1 1 d . . . C16 C 0.0622(10) 0.1968(7) 0.0135(6) 0.058(3) Uani 1 1 d . . . H16A H 0.0697 0.2340 -0.0377 0.087 Uiso 1 1 calc R . . H16B H -0.0185 0.1928 0.0300 0.087 Uiso 1 1 calc R . . H16C H 0.1183 0.1408 0.0060 0.087 Uiso 1 1 calc R . . C17 C 0.0881(8) 0.2719(6) 0.2823(5) 0.045(3) Uani 1 1 d . . . H17A H 0.0643 0.3314 0.2896 0.067 Uiso 1 1 calc R . . H17B H 0.1634 0.2427 0.2993 0.067 Uiso 1 1 calc R . . H17C H 0.0274 0.2469 0.3154 0.067 Uiso 1 1 calc R . . C23 C 0.1413(8) 0.4690(7) -0.0895(6) 0.044(3) Uani 1 1 d . . . C24 C 0.1306(9) 0.5457(7) -0.0714(7) 0.056(3) Uani 1 1 d . . . H24A H 0.1011 0.5980 -0.1024 0.068 Uiso 1 1 calc R . . C25 C 0.1708(8) 0.5345(6) 0.0013(6) 0.041(2) Uani 1 1 d . . . C26 C 0.1173(9) 0.4478(7) -0.1615(6) 0.058(3) Uani 1 1 d . . . H26A H 0.0799 0.4029 -0.1449 0.087 Uiso 1 1 calc R . . H26B H 0.1918 0.4288 -0.2006 0.087 Uiso 1 1 calc R . . H26C H 0.0643 0.4975 -0.1869 0.087 Uiso 1 1 calc R . . C27 C 0.1805(10) 0.5980(6) 0.0456(7) 0.065(3) Uani 1 1 d . . . H27A H 0.1338 0.5944 0.1013 0.097 Uiso 1 1 calc R . . H27B H 0.1506 0.6543 0.0174 0.097 Uiso 1 1 calc R . . H27C H 0.2635 0.5872 0.0474 0.097 Uiso 1 1 calc R . . C33 C 0.4478(8) 0.2329(6) -0.0741(5) 0.036(2) Uani 1 1 d . . . C34 C 0.5504(8) 0.2244(6) -0.0498(5) 0.039(2) Uani 1 1 d . . . H34A H 0.6279 0.1932 -0.0737 0.047 Uiso 1 1 calc R . . C35 C 0.5206(7) 0.2692(5) 0.0152(5) 0.031(2) Uani 1 1 d . . . C36 C 0.4299(8) 0.1973(6) -0.1397(5) 0.044(3) Uani 1 1 d . . . H36A H 0.3697 0.1684 -0.1176 0.067 Uiso 1 1 calc R . . H36B H 0.5044 0.1573 -0.1629 0.067 Uiso 1 1 calc R . . H36C H 0.4036 0.2426 -0.1821 0.067 Uiso 1 1 calc R . . C37 C 0.5994(9) 0.2796(7) 0.0628(6) 0.051(3) Uani 1 1 d . . . H37A H 0.5839 0.3395 0.0652 0.077 Uiso 1 1 calc R . . H37B H 0.6821 0.2553 0.0365 0.077 Uiso 1 1 calc R . . H37C H 0.5842 0.2509 0.1181 0.077 Uiso 1 1 calc R . . C41 C 0.4219(8) 0.4827(5) 0.1549(5) 0.033(2) Uani 1 1 d . . . C42 C 0.5060(7) 0.5235(6) 0.1177(5) 0.035(2) Uani 1 1 d . . . H42A H 0.5339 0.5269 0.0604 0.043 Uiso 1 1 calc R . . C43 C 0.5492(8) 0.5596(5) 0.1648(5) 0.036(2) Uani 1 1 d . . . H43A H 0.6082 0.5861 0.1386 0.043 Uiso 1 1 calc R . . C44 C 0.5102(7) 0.5582(5) 0.2474(5) 0.033(2) Uani 1 1 d . . . C45 C 0.4224(9) 0.5195(7) 0.2845(6) 0.049(3) Uani 1 1 d . . . H45A H 0.3915 0.5188 0.3414 0.059 Uiso 1 1 calc R . . C46 C 0.3809(10) 0.4827(6) 0.2388(6) 0.050(3) Uani 1 1 d . . . H46A H 0.3221 0.4562 0.2652 0.060 Uiso 1 1 calc R . . C51 C 0.5749(8) 0.6231(6) 0.4109(6) 0.037(2) Uani 1 1 d . . . C52 C 0.6656(9) 0.6608(6) 0.3788(6) 0.048(3) Uani 1 1 d . . . H52A H 0.6996 0.6635 0.3222 0.058 Uiso 1 1 calc R . . C53 C 0.7043(9) 0.6933(7) 0.4293(7) 0.055(3) Uani 1 1 d . . . H53A H 0.7654 0.7187 0.4071 0.065 Uiso 1 1 calc R . . C54 C 0.6574(10) 0.6905(7) 0.5117(7) 0.056(3) Uani 1 1 d . . . C55 C 0.5685(9) 0.6512(6) 0.5459(6) 0.048(3) Uani 1 1 d . . . H55A H 0.5364 0.6472 0.6028 0.058 Uiso 1 1 calc R . . C56 C 0.5297(8) 0.6186(6) 0.4937(6) 0.045(3) Uani 1 1 d . . . H56A H 0.4697 0.5922 0.5157 0.054 Uiso 1 1 calc R . . B1 B 0.2245(9) 0.3152(7) -0.0214(7) 0.038(3) Uani 1 1 d . . . H1 H 0.2067 0.2965 -0.0674 0.046 Uiso 1 1 calc R . . C100 C 0.049(2) 0.1646(13) -0.2230(11) 0.157(9) Uani 1 1 d . . . H10A H 0.0371 0.1740 -0.2795 0.188 Uiso 1 1 calc R . . H10B H 0.0948 0.1048 -0.2124 0.188 Uiso 1 1 calc R . . Cl10 Cl -0.0784(7) 0.1796(5) -0.1627(4) 0.192(3) Uani 1 1 d . . . Cl11 Cl 0.1375(6) 0.2251(4) -0.2185(3) 0.165(3) Uani 1 1 d . . . C200 C 0.9745(12) 0.4470(9) 0.6389(11) 0.115(6) Uani 1 1 d . . . H20A H 1.0578 0.4355 0.6091 0.138 Uiso 1 1 calc R . . H20B H 0.9714 0.4542 0.6955 0.138 Uiso 1 1 calc R . . Cl20 Cl 0.9268(4) 0.3655(3) 0.6395(3) 0.1323(17) Uani 1 1 d . . . Cl21 Cl 0.8857(4) 0.5417(3) 0.5914(3) 0.1112(14) Uani 1 1 d . . . W2 W 0.73314(4) 0.12659(3) 0.38724(2) 0.04498(15) Uani 1 1 d . . . O148 O 0.8154(5) 0.1133(4) 0.2746(3) 0.0367(15) Uani 1 1 d . A . O157 O 0.6208(7) -0.0926(5) -0.2795(4) 0.072(2) Uani 1 1 d . . . H15A H 0.6528 -0.0688 -0.3226 0.108 Uiso 1 1 calc R . . N111 N 0.7482(6) 0.2572(5) 0.3615(4) 0.0321(17) Uani 1 1 d . A . N112 N 0.7792(6) 0.2880(4) 0.4188(4) 0.0310(17) Uani 1 1 d . . . N121 N 0.9071(6) 0.1044(4) 0.4144(4) 0.0303(17) Uani 1 1 d . A . N122 N 0.9250(6) 0.1553(4) 0.4588(4) 0.0291(17) Uani 1 1 d . . . N131 N 0.6678(6) 0.1540(5) 0.5110(4) 0.0363(18) Uani 1 1 d . A . N132 N 0.7203(6) 0.1964(4) 0.5451(4) 0.0316(17) Uani 1 1 d . . . C113 C 0.7753(8) 0.3691(6) 0.3919(6) 0.039(2) Uani 1 1 d . A . C114 C 0.7420(8) 0.3900(6) 0.3184(6) 0.041(2) Uani 1 1 d . . . H11A H 0.7315 0.4429 0.2857 0.049 Uiso 1 1 calc R A . C115 C 0.7265(8) 0.3189(6) 0.3011(5) 0.036(2) Uani 1 1 d . A . C116 C 0.8041(9) 0.4211(6) 0.4405(6) 0.054(3) Uani 1 1 d . . . H11E H 0.8885 0.3997 0.4415 0.081 Uiso 1 1 calc R A . H11F H 0.7577 0.4179 0.4962 0.081 Uiso 1 1 calc R . . H11G H 0.7848 0.4796 0.4154 0.081 Uiso 1 1 calc R . . C117 C 0.6904(9) 0.3097(7) 0.2267(6) 0.050(3) Uani 1 1 d . . . H11B H 0.6280 0.2825 0.2431 0.076 Uiso 1 1 calc R A . H11C H 0.7588 0.2754 0.1914 0.076 Uiso 1 1 calc R . . H11D H 0.6609 0.3653 0.1971 0.076 Uiso 1 1 calc R . . C123 C 1.0406(8) 0.1306(6) 0.4637(5) 0.032(2) Uani 1 1 d . A . C124 C 1.0964(8) 0.0609(6) 0.4235(5) 0.034(2) Uani 1 1 d . . . H12A H 1.1777 0.0295 0.4176 0.041 Uiso 1 1 calc R A . C125 C 1.0144(8) 0.0449(5) 0.3936(5) 0.031(2) Uani 1 1 d . A . C126 C 1.0906(8) 0.1788(6) 0.5020(6) 0.047(3) Uani 1 1 d . . . H12B H 1.0455 0.1862 0.5577 0.070 Uiso 1 1 calc R A . H12C H 1.0855 0.2340 0.4701 0.070 Uiso 1 1 calc R . . H12D H 1.1735 0.1479 0.5032 0.070 Uiso 1 1 calc R . . C127 C 1.0294(8) -0.0221(6) 0.3429(6) 0.042(2) Uani 1 1 d . . . H12E H 0.9628 -0.0452 0.3623 0.063 Uiso 1 1 calc R A . H12F H 1.1033 -0.0669 0.3475 0.063 Uiso 1 1 calc R . . H12G H 1.0320 0.0022 0.2859 0.063 Uiso 1 1 calc R . . C133 C 0.6672(9) 0.2015(6) 0.6240(6) 0.040(2) Uani 1 1 d . A . C134 C 0.5806(8) 0.1614(6) 0.6412(6) 0.045(3) Uani 1 1 d . . . H13D H 0.5293 0.1545 0.6923 0.054 Uiso 1 1 calc R A . C135 C 0.5833(8) 0.1338(6) 0.5705(6) 0.042(2) Uani 1 1 d . A . C136 C 0.7045(9) 0.2426(7) 0.6777(6) 0.050(3) Uani 1 1 d . . . H13A H 0.7033 0.2997 0.6526 0.075 Uiso 1 1 calc R A . H13B H 0.7847 0.2101 0.6850 0.075 Uiso 1 1 calc R . . H13C H 0.6500 0.2450 0.7308 0.075 Uiso 1 1 calc R . . C137 C 0.5044(9) 0.0883(7) 0.5587(6) 0.049(3) Uani 1 1 d . . . H13E H 0.4682 0.1173 0.5120 0.073 Uiso 1 1 calc R A . H13F H 0.4424 0.0873 0.6077 0.073 Uiso 1 1 calc R . . H13G H 0.5511 0.0307 0.5486 0.073 Uiso 1 1 calc R . . C141 C 0.7956(9) 0.0810(6) 0.2144(6) 0.041(2) Uani 1 1 d . . . C142 C 0.7133(14) 0.0430(14) 0.2246(10) 0.165(10) Uani 1 1 d . A . H14C H 0.6667 0.0354 0.2775 0.198 Uiso 1 1 calc R . . C143 C 0.6938(15) 0.0148(15) 0.1623(11) 0.191(13) Uani 1 1 d . . . H14D H 0.6348 -0.0127 0.1728 0.229 Uiso 1 1 calc R A . C144 C 0.7559(12) 0.0247(9) 0.0859(9) 0.094(6) Uani 1 1 d DU A . C145 C 0.8378(15) 0.0605(8) 0.0762(7) 0.089(5) Uani 1 1 d . . . H14B H 0.8830 0.0692 0.0230 0.106 Uiso 1 1 calc R A . C146 C 0.8614(15) 0.0858(9) 0.1387(7) 0.102(6) Uani 1 1 d . A . H14E H 0.9262 0.1075 0.1286 0.122 Uiso 1 1 calc R . . C151 C 0.6943(12) -0.0181(7) -0.0842(8) 0.078(5) Uani 1 1 d D . . C152 C 0.6255(16) -0.0716(8) -0.0727(6) 0.107(6) Uani 1 1 d . . . H15E H 0.5931 -0.0902 -0.0184 0.128 Uiso 1 1 calc R . . C153 C 0.6008(13) -0.0996(7) -0.1360(7) 0.084(5) Uani 1 1 d . . . H15D H 0.5566 -0.1382 -0.1252 0.100 Uiso 1 1 calc R . . C154 C 0.6426(10) -0.0695(7) -0.2135(6) 0.050(3) Uani 1 1 d . . . C155 C 0.7026(10) -0.0131(7) -0.2282(6) 0.055(3) Uani 1 1 d . . . H15B H 0.7272 0.0112 -0.2820 0.065 Uiso 1 1 calc R . . C156 C 0.7274(9) 0.0084(8) -0.1605(8) 0.068(4) Uani 1 1 d . . . H15C H 0.7730 0.0462 -0.1718 0.082 Uiso 1 1 calc R . . B2 B 0.8225(9) 0.2292(7) 0.4924(6) 0.036(3) Uani 1 1 d . A . H2 H 0.8491 0.2593 0.5250 0.043 Uiso 1 1 calc R . . Cl2 Cl 0.5587(3) 0.1712(2) 0.3563(2) 0.0557(15) Uani 0.530(12) 1 d P A 1 O2 O 0.7359(4) 0.0008(3) 0.4167(3) 0.0757(19) Uani 0.530(12) 1 d P A 1 Cl2' Cl 0.7359(4) 0.0008(3) 0.4167(3) 0.0757(19) Uani 0.470(12) 1 d P A 2 O2' O 0.5587(3) 0.1712(2) 0.3563(2) 0.0557(15) Uani 0.470(12) 1 d P A 2 N4 N 0.7373(9) 0.0150(6) -0.0316(6) 0.088(4) Uani 1 1 d D A . N5 N 0.7143(11) -0.0176(7) 0.0406(7) 0.146(7) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.0495(3) 0.0560(3) 0.0326(2) -0.00415(19) -0.00114(19) -0.0336(2) Cl1 0.0664(19) 0.0586(19) 0.0652(18) -0.0038(15) -0.0050(15) -0.0250(16) O1 0.017(3) 0.032(4) 0.053(4) 0.015(3) -0.001(3) -0.011(3) O48 0.043(4) 0.051(4) 0.037(3) -0.003(3) 0.002(3) -0.033(3) O57 0.090(6) 0.098(7) 0.073(5) -0.029(5) -0.003(5) -0.063(6) N11 0.029(4) 0.026(4) 0.032(4) -0.004(3) 0.001(3) -0.016(3) N12 0.028(4) 0.041(5) 0.027(4) 0.001(3) -0.005(3) -0.016(4) N21 0.033(5) 0.052(6) 0.036(4) -0.005(4) 0.002(4) -0.021(4) N22 0.024(4) 0.036(5) 0.041(5) 0.018(4) -0.001(3) -0.009(4) N31 0.037(5) 0.036(5) 0.027(4) -0.010(3) -0.005(3) -0.014(4) N32 0.034(4) 0.035(5) 0.021(4) 0.003(3) -0.002(3) -0.013(4) N47 0.027(4) 0.023(4) 0.049(5) -0.001(4) -0.008(4) -0.005(3) N58 0.037(5) 0.030(5) 0.051(5) -0.007(4) -0.007(4) -0.010(4) C13 0.038(6) 0.049(7) 0.044(6) 0.004(5) -0.009(5) -0.025(5) C14 0.034(5) 0.045(6) 0.044(6) 0.015(5) -0.012(5) -0.022(5) C15 0.032(5) 0.028(5) 0.046(6) 0.003(4) 0.000(4) -0.008(4) C16 0.063(7) 0.087(9) 0.043(6) -0.003(6) -0.015(5) -0.045(7) C17 0.042(6) 0.053(7) 0.037(5) 0.003(5) 0.002(5) -0.022(5) C23 0.029(5) 0.050(7) 0.046(6) 0.017(5) -0.002(5) -0.019(5) C24 0.033(6) 0.048(7) 0.071(8) 0.020(6) -0.006(6) -0.010(5) C25 0.025(5) 0.023(6) 0.056(6) 0.010(5) 0.003(5) 0.002(4) C26 0.049(7) 0.058(8) 0.066(7) 0.027(6) -0.028(6) -0.022(6) C27 0.062(8) 0.025(6) 0.083(8) 0.011(6) 0.005(6) -0.007(6) C33 0.042(6) 0.037(6) 0.030(5) 0.008(4) -0.011(4) -0.017(5) C34 0.030(5) 0.041(6) 0.042(5) -0.007(5) -0.001(4) -0.008(4) C35 0.025(5) 0.031(5) 0.037(5) 0.002(4) -0.008(4) -0.010(4) C36 0.044(6) 0.058(7) 0.028(5) -0.011(5) -0.001(4) -0.014(5) C37 0.051(7) 0.055(7) 0.055(6) -0.017(5) -0.008(5) -0.023(6) C41 0.035(5) 0.025(5) 0.039(5) 0.002(4) -0.002(4) -0.014(4) C42 0.028(5) 0.037(6) 0.035(5) 0.009(4) -0.005(4) -0.010(4) C43 0.034(5) 0.025(5) 0.046(6) 0.003(4) -0.007(4) -0.010(4) C44 0.027(5) 0.027(5) 0.045(5) 0.000(4) -0.005(4) -0.012(4) C45 0.054(7) 0.071(8) 0.029(5) -0.005(5) -0.001(5) -0.035(6) C46 0.068(7) 0.058(7) 0.037(6) 0.003(5) 0.001(5) -0.049(6) C51 0.030(5) 0.034(6) 0.047(6) -0.006(4) -0.009(4) -0.011(4) C52 0.051(7) 0.047(7) 0.051(6) -0.008(5) -0.001(5) -0.027(5) C53 0.051(7) 0.053(7) 0.066(7) 0.000(6) -0.013(6) -0.029(6) C54 0.064(7) 0.061(8) 0.056(7) -0.033(6) -0.003(6) -0.030(6) C55 0.047(6) 0.047(7) 0.050(6) -0.005(5) -0.001(5) -0.021(5) C56 0.033(5) 0.042(6) 0.065(7) -0.017(5) -0.005(5) -0.016(5) B1 0.022(6) 0.057(8) 0.036(6) 0.001(5) -0.009(5) -0.014(5) C100 0.24(3) 0.159(19) 0.139(17) -0.009(14) -0.052(17) -0.146(19) Cl10 0.219(7) 0.298(9) 0.146(5) -0.001(5) -0.070(5) -0.182(7) Cl11 0.269(7) 0.212(6) 0.098(3) 0.032(3) -0.066(4) -0.188(6) C200 0.064(10) 0.100(13) 0.178(17) -0.067(12) -0.021(10) 0.003(9) Cl20 0.132(4) 0.103(3) 0.185(5) -0.008(3) -0.048(4) -0.059(3) Cl21 0.082(3) 0.090(3) 0.129(3) -0.002(3) 0.009(2) -0.013(2) W2 0.0451(3) 0.0628(3) 0.0411(3) -0.0193(2) -0.0012(2) -0.0327(2) O148 0.039(4) 0.039(4) 0.038(4) -0.001(3) -0.016(3) -0.016(3) O157 0.094(6) 0.098(7) 0.044(4) -0.023(4) -0.005(4) -0.054(5) N111 0.036(4) 0.034(5) 0.030(4) 0.005(3) -0.016(3) -0.014(4) N112 0.028(4) 0.026(4) 0.043(4) -0.002(3) -0.011(3) -0.010(3) N121 0.034(4) 0.030(4) 0.034(4) -0.010(3) -0.015(3) -0.010(4) N122 0.027(4) 0.033(4) 0.030(4) -0.002(3) -0.009(3) -0.011(3) N131 0.032(4) 0.043(5) 0.040(4) -0.001(4) -0.013(4) -0.017(4) N132 0.023(4) 0.031(4) 0.038(4) -0.007(3) -0.012(3) 0.000(3) C113 0.026(5) 0.032(6) 0.055(6) -0.005(5) -0.008(5) -0.006(4) C114 0.045(6) 0.030(6) 0.052(6) 0.012(5) -0.026(5) -0.015(5) C115 0.033(5) 0.036(6) 0.042(5) 0.001(5) -0.016(4) -0.010(4) C116 0.051(7) 0.046(7) 0.073(8) -0.003(6) -0.019(6) -0.023(5) C117 0.060(7) 0.051(7) 0.047(6) 0.007(5) -0.025(5) -0.022(6) C123 0.033(5) 0.039(6) 0.029(5) 0.005(4) -0.011(4) -0.018(4) C124 0.030(5) 0.034(6) 0.033(5) 0.001(4) -0.008(4) -0.005(4) C125 0.043(6) 0.028(5) 0.026(4) 0.002(4) -0.011(4) -0.018(4) C126 0.042(6) 0.059(7) 0.052(6) -0.002(5) -0.017(5) -0.029(5) C127 0.038(6) 0.038(6) 0.047(6) -0.011(5) -0.009(5) -0.004(5) C133 0.049(6) 0.035(6) 0.039(6) -0.008(4) -0.010(5) -0.012(5) C134 0.037(6) 0.055(7) 0.038(6) 0.001(5) 0.003(5) -0.020(5) C135 0.033(6) 0.044(6) 0.048(6) 0.001(5) -0.010(5) -0.013(5) C136 0.045(6) 0.065(8) 0.040(6) -0.015(5) 0.002(5) -0.019(6) C137 0.049(6) 0.057(7) 0.046(6) 0.003(5) -0.008(5) -0.029(6) C141 0.053(6) 0.031(6) 0.043(6) -0.008(5) -0.015(5) -0.013(5) C142 0.120(14) 0.31(3) 0.141(15) -0.178(18) 0.066(12) -0.147(17) C143 0.117(15) 0.38(3) 0.158(17) -0.21(2) 0.033(13) -0.126(19) C144 0.107(11) 0.072(10) 0.121(12) -0.087(9) -0.073(10) 0.029(8) C145 0.178(16) 0.079(10) 0.040(7) -0.007(6) -0.022(8) -0.079(11) C146 0.175(16) 0.138(13) 0.043(7) -0.014(8) 0.007(8) -0.132(13) C151 0.138(13) 0.036(8) 0.059(8) -0.028(6) -0.058(9) 0.016(8) C152 0.25(2) 0.050(8) 0.025(6) 0.001(6) -0.022(9) -0.052(11) C153 0.153(14) 0.057(8) 0.055(7) -0.006(6) -0.006(8) -0.061(9) C154 0.067(7) 0.064(8) 0.033(5) -0.023(5) -0.002(5) -0.031(6) C155 0.065(8) 0.063(8) 0.041(6) -0.012(5) -0.003(5) -0.029(6) C156 0.038(6) 0.085(9) 0.094(10) -0.059(8) -0.025(7) 0.000(6) B2 0.036(6) 0.043(7) 0.033(6) -0.002(5) -0.010(5) -0.016(5) Cl2 0.049(3) 0.044(3) 0.059(3) -0.0007(18) -0.0073(19) 0.0001(19) O2 0.055(3) 0.061(3) 0.085(4) 0.029(2) -0.009(2) -0.009(2) Cl2' 0.055(3) 0.061(3) 0.085(4) 0.029(2) -0.009(2) -0.009(2) O2' 0.049(3) 0.044(3) 0.059(3) -0.0007(18) -0.0073(19) 0.0001(19) N4 0.098(9) 0.031(6) 0.097(9) -0.017(6) -0.004(7) 0.022(6) N5 0.155(14) 0.053(8) 0.163(14) -0.031(9) 0.088(12) -0.025(9) _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 W1 O1 1.896(6) . ? W1 O48 1.954(6) . ? W1 N21 2.164(8) . ? W1 N11 2.164(6) . ? W1 Cl1 2.281(3) . ? W1 N31 2.286(6) . ? O48 C41 1.345(10) . ? O57 C54 1.361(11) . ? N11 C15 1.366(10) . ? N11 N12 1.373(9) . ? N12 C13 1.333(11) . ? N12 B1 1.552(12) . ? N21 C25 1.349(11) . ? N21 N22 1.354(10) . ? N22 C23 1.358(11) . ? N22 B1 1.546(14) . ? N31 C35 1.358(10) . ? N31 N32 1.381(9) . ? N32 C33 1.368(11) . ? N32 B1 1.525(12) . ? N47 N58 1.278(9) . ? N47 C44 1.416(11) . ? N58 C51 1.419(11) . ? C13 C14 1.372(12) . ? C13 C16 1.506(13) . ? C14 C15 1.389(13) . ? C15 C17 1.486(12) . ? C23 C24 1.358(14) . ? C23 C26 1.472(14) . ? C24 C25 1.409(15) . ? C25 C27 1.488(14) . ? C33 C34 1.380(12) . ? C33 C36 1.468(12) . ? C34 C35 1.373(12) . ? C35 C37 1.486(12) . ? C41 C42 1.388(11) . ? C41 C46 1.394(12) . ? C42 C43 1.392(12) . ? C43 C44 1.371(12) . ? C44 C45 1.401(12) . ? C45 C46 1.369(13) . ? C51 C56 1.380(12) . ? C51 C52 1.407(12) . ? C52 C53 1.363(13) . ? C53 C54 1.377(14) . ? C54 C55 1.410(14) . ? C55 C56 1.388(13) . ? C100 Cl10 1.61(2) . ? C100 Cl11 1.750(16) . ? C200 Cl20 1.677(15) . ? C200 Cl21 1.792(16) . ? W2 O148 1.951(6) . ? W2 O2 2.094(5) . ? W2 N131 2.148(7) . ? W2 Cl2 2.184(4) . ? W2 N121 2.195(7) . ? W2 N111 2.242(7) . ? O148 C141 1.364(10) . ? O157 C154 1.378(11) . ? N111 C115 1.332(11) . ? N111 N112 1.382(9) . ? N112 C113 1.357(11) . ? N112 B2 1.538(12) . ? N121 N122 1.360(9) . ? N121 C125 1.375(11) . ? N122 C123 1.358(10) . ? N122 B2 1.531(12) . ? N131 C135 1.339(11) . ? N131 N132 1.397(10) . ? N132 C133 1.345(11) . ? N132 B2 1.547(12) . ? C113 C114 1.366(13) . ? C113 C116 1.500(13) . ? C114 C115 1.384(12) . ? C115 C117 1.502(12) . ? C123 C124 1.372(12) . ? C123 C126 1.496(12) . ? C124 C125 1.361(12) . ? C125 C127 1.501(11) . ? C133 C134 1.389(13) . ? C133 C136 1.494(13) . ? C134 C135 1.371(13) . ? C135 C137 1.497(13) . ? C141 C142 1.333(16) . ? C141 C146 1.344(14) . ? C142 C143 1.355(17) . ? C143 C144 1.35(2) . ? C144 C145 1.302(18) . ? C144 N5 1.4305(11) . ? C145 C146 1.354(16) . ? C151 C156 1.303(16) . ? C151 C152 1.394(19) . ? C151 N4 1.4307(11) . ? C152 C153 1.400(17) . ? C153 C154 1.359(14) . ? C154 C155 1.347(14) . ? C155 C156 1.411(14) . ? N4 N5 1.2541(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 W1 O48 98.3(2) . . ? O1 W1 N21 93.3(3) . . ? O48 W1 N21 88.2(3) . . ? O1 W1 N11 93.0(2) . . ? O48 W1 N11 167.2(2) . . ? N21 W1 N11 85.3(3) . . ? O1 W1 Cl1 98.60(19) . . ? O48 W1 Cl1 91.5(2) . . ? N21 W1 Cl1 168.0(2) . . ? N11 W1 Cl1 92.6(2) . . ? O1 W1 N31 171.4(3) . . ? O48 W1 N31 85.4(2) . . ? N21 W1 N31 79.1(3) . . ? N11 W1 N31 82.6(2) . . ? Cl1 W1 N31 89.0(2) . . ? C41 O48 W1 133.0(5) . . ? C15 N11 N12 107.4(7) . . ? C15 N11 W1 130.7(6) . . ? N12 N11 W1 121.8(5) . . ? C13 N12 N11 109.5(7) . . ? C13 N12 B1 131.2(8) . . ? N11 N12 B1 119.3(7) . . ? C25 N21 N22 107.8(8) . . ? C25 N21 W1 130.4(7) . . ? N22 N21 W1 121.7(6) . . ? N21 N22 C23 110.6(8) . . ? N21 N22 B1 120.1(7) . . ? C23 N22 B1 129.2(9) . . ? C35 N31 N32 106.8(6) . . ? C35 N31 W1 134.4(6) . . ? N32 N31 W1 118.8(5) . . ? C33 N32 N31 109.4(7) . . ? C33 N32 B1 131.0(8) . . ? N31 N32 B1 119.7(7) . . ? N58 N47 C44 113.1(7) . . ? N47 N58 C51 115.0(7) . . ? N12 C13 C14 108.0(8) . . ? N12 C13 C16 122.4(8) . . ? C14 C13 C16 129.6(9) . . ? C13 C14 C15 107.7(8) . . ? N11 C15 C14 107.3(8) . . ? N11 C15 C17 124.2(8) . . ? C14 C15 C17 128.5(8) . . ? C24 C23 N22 106.4(10) . . ? C24 C23 C26 128.7(10) . . ? N22 C23 C26 124.8(10) . . ? C23 C24 C25 108.3(10) . . ? N21 C25 C24 107.0(9) . . ? N21 C25 C27 123.4(10) . . ? C24 C25 C27 129.6(10) . . ? N32 C33 C34 106.8(8) . . ? N32 C33 C36 123.1(8) . . ? C34 C33 C36 130.1(9) . . ? C35 C34 C33 108.0(8) . . ? N31 C35 C34 109.1(8) . . ? N31 C35 C37 122.3(8) . . ? C34 C35 C37 128.6(8) . . ? O48 C41 C42 118.2(8) . . ? O48 C41 C46 124.3(8) . . ? C42 C41 C46 117.5(9) . . ? C41 C42 C43 119.7(8) . . ? C44 C43 C42 122.6(8) . . ? C43 C44 C45 117.6(8) . . ? C43 C44 N47 117.7(8) . . ? C45 C44 N47 124.7(8) . . ? C46 C45 C44 120.1(9) . . ? C45 C46 C41 122.4(9) . . ? C56 C51 C52 118.4(9) . . ? C56 C51 N58 115.2(8) . . ? C52 C51 N58 126.4(9) . . ? C53 C52 C51 119.6(9) . . ? C52 C53 C54 121.9(10) . . ? O57 C54 C53 118.3(10) . . ? O57 C54 C55 121.9(10) . . ? C53 C54 C55 119.8(9) . . ? C56 C55 C54 117.6(9) . . ? C51 C56 C55 122.6(9) . . ? N32 B1 N22 107.6(8) . . ? N32 B1 N12 109.2(8) . . ? N22 B1 N12 109.7(8) . . ? Cl10 C100 Cl11 118.3(11) . . ? Cl20 C200 Cl21 110.9(9) . . ? O148 W2 O2 94.0(2) . . ? O148 W2 N131 168.4(3) . . ? O2 W2 N131 93.9(2) . . ? O148 W2 Cl2 93.2(2) . . ? O2 W2 Cl2 95.04(17) . . ? N131 W2 Cl2 94.6(2) . . ? O148 W2 N121 86.8(2) . . ? O2 W2 N121 94.7(2) . . ? N131 W2 N121 84.1(3) . . ? Cl2 W2 N121 170.2(2) . . ? O148 W2 N111 86.7(2) . . ? O2 W2 N111 173.7(2) . . ? N131 W2 N111 84.6(3) . . ? Cl2 W2 N111 91.2(2) . . ? N121 W2 N111 79.0(3) . . ? C141 O148 W2 132.7(6) . . ? C115 N111 N112 107.3(7) . . ? C115 N111 W2 133.4(6) . . ? N112 N111 W2 119.1(5) . . ? C113 N112 N111 108.1(7) . . ? C113 N112 B2 131.2(8) . . ? N111 N112 B2 120.3(7) . . ? N122 N121 C125 106.3(6) . . ? N122 N121 W2 121.4(5) . . ? C125 N121 W2 132.3(5) . . ? C123 N122 N121 109.7(7) . . ? C123 N122 B2 129.9(7) . . ? N121 N122 B2 120.3(7) . . ? C135 N131 N132 106.5(7) . . ? C135 N131 W2 132.3(6) . . ? N132 N131 W2 121.0(5) . . ? C133 N132 N131 109.1(7) . . ? C133 N132 B2 130.7(8) . . ? N131 N132 B2 120.2(7) . . ? N112 C113 C114 108.5(8) . . ? N112 C113 C116 121.6(9) . . ? C114 C113 C116 129.9(9) . . ? C113 C114 C115 106.3(9) . . ? N111 C115 C114 109.7(8) . . ? N111 C115 C117 123.4(8) . . ? C114 C115 C117 126.9(9) . . ? N122 C123 C124 107.3(8) . . ? N122 C123 C126 122.6(8) . . ? C124 C123 C126 130.0(9) . . ? C125 C124 C123 107.7(8) . . ? C124 C125 N121 108.9(7) . . ? C124 C125 C127 129.4(9) . . ? N121 C125 C127 121.6(8) . . ? N132 C133 C134 107.4(8) . . ? N132 C133 C136 122.1(9) . . ? C134 C133 C136 130.5(9) . . ? C135 C134 C133 107.0(8) . . ? N131 C135 C134 109.9(9) . . ? N131 C135 C137 123.5(9) . . ? C134 C135 C137 126.5(9) . . ? C142 C141 C146 115.0(10) . . ? C142 C141 O148 124.5(10) . . ? C146 C141 O148 120.5(9) . . ? C141 C142 C143 122.4(15) . . ? C144 C143 C142 121.5(16) . . ? C145 C144 C143 116.0(11) . . ? C145 C144 N5 139.6(15) . . ? C143 C144 N5 104.0(14) . . ? C144 C145 C146 122.9(13) . . ? C141 C146 C145 121.8(12) . . ? C156 C151 C152 113.0(9) . . ? C156 C151 N4 112.0(12) . . ? C152 C151 N4 135.0(13) . . ? C151 C152 C153 124.3(11) . . ? C154 C153 C152 117.5(12) . . ? C155 C154 C153 120.8(10) . . ? C155 C154 O157 117.7(9) . . ? C153 C154 O157 121.4(10) . . ? C154 C155 C156 117.4(10) . . ? C151 C156 C155 126.8(12) . . ? N122 B2 N112 106.9(7) . . ? N122 B2 N132 109.3(8) . . ? N112 B2 N132 108.5(8) . . ? N5 N4 C151 110.9(10) . . ? N4 N5 C144 104.4(10) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.981 _refine_diff_density_min -1.892 _refine_diff_density_rms 0.161 #=END data_complex3 _database_code_CSD 192529 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H74 B2 Cl2 N12 O4 W2' _chemical_formula_weight 1331.4 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' Cl Cl 0.1484 0.1585 '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 11.819(3) _cell_length_b 20.631(5) _cell_length_c 25.873(10) _cell_angle_alpha 90.00 _cell_angle_beta 99.77(2) _cell_angle_gamma 90.00 _cell_volume 6218(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2656 _exptl_absorpt_coefficient_mu 3.829 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.23 _exptl_absorpt_correction_T_max 0.80 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20088 _diffrn_reflns_av_R_equivalents 0.0779 _diffrn_reflns_av_sigmaI/netI 0.1111 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 27.56 _reflns_number_total 7162 _reflns_number_gt 4316 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0621P)^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 7162 _refine_ls_number_parameters 303 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1194 _refine_ls_R_factor_gt 0.0596 _refine_ls_wR_factor_ref 0.1454 _refine_ls_wR_factor_gt 0.1281 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.68935(3) 0.609822(17) 0.901542(14) 0.02834(12) Uani 1 1 d . . . Cl1 Cl 0.8260(2) 0.60843(13) 0.84649(9) 0.0433(6) Uani 1 1 d . . . O1 O 0.6236(5) 0.6828(3) 0.8836(2) 0.0365(15) Uani 1 1 d . . . O41 O 0.5942(5) 0.5496(3) 0.8551(2) 0.0284(14) Uani 1 1 d . . . N11 N 0.5863(6) 0.5929(3) 0.9613(3) 0.0295(17) Uani 1 1 d . . . N12 N 0.6320(6) 0.5795(3) 1.0115(3) 0.0282(17) Uani 1 1 d . . . N21 N 0.8101(6) 0.6554(3) 0.9640(3) 0.0258(16) Uani 1 1 d . . . N22 N 0.8228(5) 0.6340(3) 1.0137(3) 0.0223(15) Uani 1 1 d . . . N31 N 0.7723(6) 0.5177(3) 0.9408(3) 0.0294(17) Uani 1 1 d . . . N32 N 0.8023(6) 0.5157(3) 0.9952(3) 0.0274(16) Uani 1 1 d . . . C13 C 0.5480(8) 0.5760(4) 1.0408(4) 0.037(2) Uani 1 1 d . . . C14 C 0.4453(8) 0.5892(4) 1.0074(4) 0.042(3) Uani 1 1 d . . . H14A H 0.3712 0.5910 1.0169 0.051 Uiso 1 1 calc R . . C15 C 0.4705(7) 0.5993(4) 0.9580(4) 0.033(2) Uani 1 1 d . . . C16 C 0.5679(10) 0.5639(5) 1.0980(4) 0.053(3) Uani 1 1 d . . . H16A H 0.6309 0.5328 1.1069 0.079 Uiso 1 1 calc R . . H16B H 0.4979 0.5461 1.1081 0.079 Uiso 1 1 calc R . . H16C H 0.5879 0.6046 1.1167 0.079 Uiso 1 1 calc R . . C17 C 0.3953(7) 0.6182(5) 0.9081(4) 0.046(3) Uani 1 1 d . . . H17A H 0.4193 0.5948 0.8788 0.068 Uiso 1 1 calc R . . H17B H 0.4017 0.6650 0.9026 0.068 Uiso 1 1 calc R . . H17C H 0.3155 0.6072 0.9100 0.068 Uiso 1 1 calc R . . C23 C 0.8896(7) 0.6768(5) 1.0463(3) 0.031(2) Uani 1 1 d . . . C24 C 0.9193(8) 0.7244(4) 1.0154(4) 0.034(2) Uani 1 1 d . . . H24A H 0.9662 0.7607 1.0269 0.041 Uiso 1 1 calc R . . C25 C 0.8698(7) 0.7113(4) 0.9640(3) 0.029(2) Uani 1 1 d . . . C26 C 0.9216(9) 0.6647(5) 1.1037(4) 0.044(2) Uani 1 1 d . . . H26A H 0.9679 0.7010 1.1201 0.065 Uiso 1 1 calc R . . H26B H 0.9661 0.6245 1.1095 0.065 Uiso 1 1 calc R . . H26C H 0.8518 0.6608 1.1192 0.065 Uiso 1 1 calc R . . C27 C 0.8767(8) 0.7499(4) 0.9169(4) 0.039(2) Uani 1 1 d . . . H27A H 0.8010 0.7513 0.8945 0.059 Uiso 1 1 calc R . . H27B H 0.9323 0.7301 0.8976 0.059 Uiso 1 1 calc R . . H27C H 0.9013 0.7941 0.9273 0.059 Uiso 1 1 calc R . . C33 C 0.8625(7) 0.4605(4) 1.0087(4) 0.031(2) Uani 1 1 d . . . C34 C 0.8663(8) 0.4267(5) 0.9649(4) 0.037(2) Uani 1 1 d . . . H34A H 0.9008 0.3854 0.9631 0.044 Uiso 1 1 calc R . . C35 C 0.8114(7) 0.4625(4) 0.9227(4) 0.029(2) Uani 1 1 d . . . C36 C 0.9092(8) 0.4458(5) 1.0656(4) 0.045(3) Uani 1 1 d . . . H36A H 0.9356 0.4007 1.0688 0.068 Uiso 1 1 calc R . . H36B H 0.8486 0.4522 1.0866 0.068 Uiso 1 1 calc R . . H36C H 0.9736 0.4748 1.0781 0.068 Uiso 1 1 calc R . . C37 C 0.7965(9) 0.4456(5) 0.8665(4) 0.047(3) Uani 1 1 d . . . H37A H 0.8090 0.4842 0.8461 0.070 Uiso 1 1 calc R . . H37B H 0.7184 0.4293 0.8548 0.070 Uiso 1 1 calc R . . H37C H 0.8520 0.4120 0.8612 0.070 Uiso 1 1 calc R . . C41 C 0.5495(7) 0.5508(4) 0.8030(3) 0.028(2) Uani 1 1 d . . . C42 C 0.5239(9) 0.6083(5) 0.7767(4) 0.046(3) Uani 1 1 d . . . H42A H 0.5387 0.6483 0.7949 0.056 Uiso 1 1 calc R . . C43 C 0.5245(7) 0.4932(4) 0.7765(3) 0.030(2) Uani 1 1 d . . . H43A H 0.5407 0.4532 0.7945 0.036 Uiso 1 1 calc R . . C100 C 0.0000 0.5197(18) 0.7500 0.144(12) Uani 1 2 d S . . H10A H -0.0238 0.5492 0.7764 0.173 Uiso 0.50 1 calc PR . . H10B H 0.0238 0.5492 0.7236 0.173 Uiso 0.50 1 calc PR . . C101 C 0.105(3) 0.502(3) 0.7761(10) 0.36(3) Uani 1 1 d . . . H10C H 0.0839 0.4832 0.8083 0.434 Uiso 1 1 calc R . . H10D H 0.1211 0.4642 0.7551 0.434 Uiso 1 1 calc R . . C102 C 0.1982(19) 0.520(2) 0.7921(11) 0.28(2) Uani 1 1 d . . . H10E H 0.2372 0.5302 0.7626 0.423 Uiso 1 1 calc R . . H10F H 0.2404 0.4853 0.8133 0.423 Uiso 1 1 calc R . . H10G H 0.1952 0.5584 0.8138 0.423 Uiso 1 1 calc R . . C200 C 0.225(2) 0.7441(14) 0.9708(9) 0.196(11) Uiso 1 1 d . . . H20A H 0.1453 0.7336 0.9746 0.236 Uiso 1 1 calc R . . H20B H 0.2603 0.7012 0.9669 0.236 Uiso 1 1 calc R . . C201 C 0.199(3) 0.767(2) 0.9040(18) 0.37(3) Uiso 1 1 d . . . H20C H 0.2711 0.7910 0.9020 0.447 Uiso 1 1 calc R . . H20D H 0.1414 0.8016 0.9049 0.447 Uiso 1 1 calc R . . C202 C 0.160(4) 0.740(2) 0.835(2) 0.44(3) Uiso 1 1 d . . . H20E H 0.0959 0.7667 0.8170 0.664 Uiso 1 1 calc R . . H20F H 0.1365 0.6946 0.8338 0.664 Uiso 1 1 calc R . . H20G H 0.2260 0.7453 0.8169 0.664 Uiso 1 1 calc R . . B1 B 0.7640(8) 0.5713(5) 1.0270(4) 0.030(2) Uani 1 1 d . . . H1 H 0.7848 0.5618 1.0653 0.036 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 W1 0.02564(18) 0.0293(2) 0.02753(19) -0.00015(19) -0.00294(12) -0.00160(19) Cl1 0.0417(13) 0.0507(15) 0.0384(13) -0.0006(13) 0.0096(10) -0.0036(13) O1 0.031(3) 0.028(4) 0.046(4) -0.009(3) -0.005(3) -0.001(3) O41 0.031(3) 0.031(3) 0.021(3) 0.005(3) -0.005(2) 0.003(3) N11 0.024(4) 0.026(4) 0.035(4) -0.001(3) -0.002(3) -0.004(3) N12 0.026(4) 0.025(4) 0.036(4) -0.007(3) 0.009(3) -0.004(3) N21 0.027(4) 0.024(4) 0.025(4) 0.000(3) 0.002(3) 0.004(3) N22 0.018(3) 0.023(4) 0.022(4) -0.003(3) -0.006(3) 0.002(3) N31 0.027(4) 0.032(4) 0.029(4) -0.005(3) 0.004(3) -0.003(3) N32 0.029(4) 0.023(4) 0.027(4) 0.002(3) -0.005(3) -0.001(3) C13 0.041(6) 0.025(5) 0.048(6) -0.001(4) 0.015(5) -0.005(4) C14 0.029(5) 0.035(6) 0.067(7) -0.006(5) 0.020(5) -0.008(4) C15 0.020(4) 0.036(6) 0.045(6) -0.002(4) 0.008(4) 0.000(4) C16 0.076(8) 0.037(6) 0.050(7) -0.001(5) 0.026(6) -0.006(6) C17 0.021(5) 0.059(7) 0.054(6) -0.014(5) -0.005(4) 0.011(5) C23 0.019(4) 0.032(5) 0.039(5) -0.011(4) -0.007(4) 0.004(4) C24 0.033(5) 0.027(5) 0.041(6) -0.001(4) 0.002(4) -0.005(4) C25 0.020(4) 0.030(5) 0.037(5) -0.004(4) 0.005(4) 0.000(4) C26 0.051(6) 0.045(6) 0.032(5) -0.008(5) -0.003(4) 0.000(5) C27 0.038(6) 0.031(6) 0.048(6) 0.001(5) 0.004(5) 0.001(4) C33 0.016(4) 0.027(5) 0.045(6) 0.015(4) -0.005(4) 0.001(4) C34 0.032(5) 0.032(6) 0.049(6) -0.004(5) 0.013(4) 0.005(4) C35 0.019(4) 0.027(5) 0.040(5) -0.002(4) 0.003(4) 0.003(4) C36 0.036(5) 0.041(6) 0.054(7) 0.010(5) -0.004(5) 0.002(5) C37 0.049(6) 0.046(7) 0.042(6) -0.015(5) 0.002(5) 0.007(5) C41 0.018(4) 0.037(6) 0.026(5) 0.003(4) -0.001(3) 0.003(4) C42 0.058(7) 0.032(5) 0.041(6) 0.000(5) -0.015(5) 0.001(5) C43 0.024(5) 0.030(5) 0.035(5) 0.008(4) 0.002(4) -0.007(4) C100 0.08(2) 0.25(4) 0.11(3) 0.000 0.037(17) 0.000 C101 0.21(4) 0.81(11) 0.07(2) 0.07(3) 0.03(2) -0.03(6) C102 0.071(15) 0.67(8) 0.11(2) 0.02(3) 0.023(15) -0.02(3) B1 0.027(5) 0.030(6) 0.031(6) 0.001(5) 0.000(4) -0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 O1 1.721(6) . ? W1 O41 1.948(6) . ? W1 N11 2.153(7) . ? W1 N21 2.179(7) . ? W1 N31 2.295(7) . ? W1 Cl1 2.328(2) . ? O41 C41 1.360(9) . ? N11 N12 1.347(10) . ? N11 C15 1.363(10) . ? N12 C13 1.350(11) . ? N12 B1 1.553(12) . ? N21 N22 1.345(9) . ? N21 C25 1.352(11) . ? N22 C23 1.375(10) . ? N22 B1 1.533(12) . ? N31 C35 1.342(10) . ? N31 N32 1.392(9) . ? N32 C33 1.358(10) . ? N32 B1 1.524(12) . ? C13 C14 1.393(13) . ? C13 C16 1.479(14) . ? C14 C15 1.376(13) . ? C15 C17 1.490(13) . ? C23 C24 1.350(13) . ? C23 C26 1.488(12) . ? C24 C25 1.386(12) . ? C25 C27 1.469(12) . ? C33 C34 1.339(13) . ? C33 C36 1.511(12) . ? C34 C35 1.384(12) . ? C35 C37 1.478(12) . ? C41 C42 1.376(12) . ? C41 C43 1.379(12) . ? C42 C42 1.402(18) 2_656 ? C43 C43 1.396(16) 2_656 ? C100 C101 1.36(4) 2_556 ? C100 C101 1.36(4) . ? C101 C102 1.17(4) . ? C200 C200 1.55(4) 7_567 ? C200 C201 1.77(4) . ? C201 C202 1.86(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 W1 O41 101.8(3) . . ? O1 W1 N11 92.9(3) . . ? O41 W1 N11 90.2(2) . . ? O1 W1 N21 91.8(3) . . ? O41 W1 N21 165.9(2) . . ? N11 W1 N21 85.2(3) . . ? O1 W1 N31 169.4(3) . . ? O41 W1 N31 84.4(2) . . ? N11 W1 N31 78.4(3) . . ? N21 W1 N31 81.6(2) . . ? O1 W1 Cl1 100.1(2) . . ? O41 W1 Cl1 90.13(18) . . ? N11 W1 Cl1 166.7(2) . . ? N21 W1 Cl1 91.36(19) . . ? N31 W1 Cl1 88.37(19) . . ? C41 O41 W1 133.3(5) . . ? N12 N11 C15 108.4(7) . . ? N12 N11 W1 122.8(5) . . ? C15 N11 W1 128.6(6) . . ? N11 N12 C13 109.8(7) . . ? N11 N12 B1 119.5(7) . . ? C13 N12 B1 130.7(8) . . ? N22 N21 C25 107.9(7) . . ? N22 N21 W1 121.3(5) . . ? C25 N21 W1 130.2(6) . . ? N21 N22 C23 109.6(7) . . ? N21 N22 B1 120.7(7) . . ? C23 N22 B1 129.7(7) . . ? C35 N31 N32 106.5(7) . . ? C35 N31 W1 134.1(6) . . ? N32 N31 W1 119.1(5) . . ? C33 N32 N31 108.5(7) . . ? C33 N32 B1 133.0(8) . . ? N31 N32 B1 118.5(7) . . ? N12 C13 C14 106.7(9) . . ? N12 C13 C16 124.3(9) . . ? C14 C13 C16 128.9(9) . . ? C15 C14 C13 107.6(8) . . ? N11 C15 C14 107.5(8) . . ? N11 C15 C17 121.7(8) . . ? C14 C15 C17 130.7(8) . . ? C24 C23 N22 106.4(8) . . ? C24 C23 C26 131.7(8) . . ? N22 C23 C26 121.8(8) . . ? C23 C24 C25 108.5(8) . . ? N21 C25 C24 107.5(8) . . ? N21 C25 C27 124.3(8) . . ? C24 C25 C27 128.1(8) . . ? C34 C33 N32 108.0(8) . . ? C34 C33 C36 131.3(9) . . ? N32 C33 C36 120.6(8) . . ? C33 C34 C35 108.1(8) . . ? N31 C35 C34 108.8(8) . . ? N31 C35 C37 123.5(8) . . ? C34 C35 C37 127.7(8) . . ? O41 C41 C42 121.4(8) . . ? O41 C41 C43 119.4(8) . . ? C42 C41 C43 119.1(8) . . ? C41 C42 C42 120.4(5) . 2_656 ? C41 C43 C43 120.5(5) . 2_656 ? C101 C100 C101 149(6) 2_556 . ? C102 C101 C100 145(6) . . ? C200 C200 C201 153(4) 7_567 . ? C200 C201 C202 147(4) . . ? N32 B1 N22 109.0(7) . . ? N32 B1 N12 108.6(7) . . ? N22 B1 N12 108.9(7) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.490 _refine_diff_density_min -2.260 _refine_diff_density_rms 0.174 #=END data_complex5 _database_code_CSD 192530 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H72 B2 Cl2 N14 O6 W2' _chemical_formula_weight 1425.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3744(16) _cell_length_b 10.610(2) _cell_length_c 14.654(4) _cell_angle_alpha 97.81(2) _cell_angle_beta 95.395(17) _cell_angle_gamma 97.33(2) _cell_volume 1423.0(6) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.663 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 710 _exptl_absorpt_coefficient_mu 4.192 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.27 _exptl_absorpt_correction_T_max 0.80 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14958 _diffrn_reflns_av_R_equivalents 0.0477 _diffrn_reflns_av_sigmaI/netI 0.0790 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 27.54 _reflns_number_total 6450 _reflns_number_gt 4048 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0740P)^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 6450 _refine_ls_number_parameters 359 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0963 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_ref 0.1361 _refine_ls_wR_factor_gt 0.1198 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.982 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.17297(4) 0.51304(3) 0.25882(2) 0.05251(15) Uani 1 1 d . . . Cl1A Cl 0.1722(5) 0.7098(4) 0.3264(3) 0.0387(11) Uani 0.50 1 d P A 1 Cl1B Cl 0.4019(6) 0.5234(6) 0.2901(4) 0.0455(13) Uani 0.50 1 d P A 2 O1A O 0.3672(18) 0.4964(16) 0.2713(12) 0.049(6) Uiso 0.50 1 d P A 1 O1B O 0.1395(14) 0.6739(13) 0.3298(10) 0.039(4) Uiso 0.50 1 d P A 2 O48 O 0.1679(5) 0.5685(5) 0.1369(3) 0.0435(12) Uani 1 1 d . A . O53 O 0.3270(7) 0.0932(6) 0.5024(5) 0.0710(18) Uani 1 1 d . . . N11 N -0.1402(6) 0.3598(5) 0.2504(4) 0.0329(13) Uani 1 1 d . . . N12 N -0.0670(6) 0.4705(5) 0.2307(4) 0.0359(14) Uani 1 1 d . A . N21 N 0.0394(6) 0.3124(5) 0.3728(4) 0.0356(13) Uani 1 1 d . . . N22 N 0.1362(6) 0.4236(5) 0.3791(4) 0.0348(13) Uani 1 1 d . A . N31 N 0.0486(6) 0.2216(5) 0.2067(4) 0.0366(14) Uani 1 1 d . . . N32 N 0.1451(6) 0.3178(6) 0.1828(4) 0.0383(15) Uani 1 1 d . A . N47 N 0.4421(6) 0.9690(5) -0.0200(4) 0.0374(14) Uani 1 1 d . . . C13 C -0.1661(8) 0.5414(7) 0.2027(5) 0.0387(17) Uani 1 1 d . . . C14 C -0.3027(8) 0.4759(8) 0.2055(6) 0.052(2) Uani 1 1 d . A . H14A H -0.3925 0.5045 0.1896 0.062 Uiso 1 1 calc R . . C15 C -0.2831(8) 0.3609(7) 0.2360(5) 0.0430(18) Uani 1 1 d . A . C16 C -0.1290(9) 0.6689(8) 0.1716(7) 0.058(2) Uani 1 1 d . A . H16A H -0.0602 0.7250 0.2191 0.087 Uiso 1 1 calc R . . H16B H -0.2172 0.7083 0.1619 0.087 Uiso 1 1 calc R . . H16C H -0.0854 0.6569 0.1134 0.087 Uiso 1 1 calc R . . C17 C -0.3931(8) 0.2533(7) 0.2513(6) 0.052(2) Uani 1 1 d . . . H17A H -0.3615 0.2209 0.3082 0.078 Uiso 1 1 calc R A . H17B H -0.4036 0.1839 0.1986 0.078 Uiso 1 1 calc R . . H17C H -0.4863 0.2845 0.2571 0.078 Uiso 1 1 calc R . . C23 C 0.1926(8) 0.4546(7) 0.4685(5) 0.0376(16) Uani 1 1 d . . . C24 C 0.1298(8) 0.3654(7) 0.5185(5) 0.0404(17) Uani 1 1 d . A . H24A H 0.1490 0.3655 0.5834 0.049 Uiso 1 1 calc R . . C25 C 0.0351(8) 0.2773(6) 0.4582(5) 0.0355(16) Uani 1 1 d . A . C26 C 0.3048(9) 0.5674(7) 0.5030(5) 0.0484(19) Uani 1 1 d . A . H26A H 0.2675 0.6461 0.4899 0.073 Uiso 1 1 calc R . . H26B H 0.3917 0.5583 0.4718 0.073 Uiso 1 1 calc R . . H26C H 0.3291 0.5724 0.5700 0.073 Uiso 1 1 calc R . . C27 C -0.0544(9) 0.1560(7) 0.4738(6) 0.051(2) Uani 1 1 d . . . H27A H -0.1557 0.1565 0.4505 0.077 Uiso 1 1 calc R A . H27B H -0.0469 0.1506 0.5403 0.077 Uiso 1 1 calc R . . H27C H -0.0188 0.0816 0.4409 0.077 Uiso 1 1 calc R . . C33 C 0.2118(8) 0.2612(7) 0.1130(5) 0.0398(17) Uani 1 1 d . . . C34 C 0.1575(9) 0.1325(8) 0.0940(5) 0.049(2) Uani 1 1 d . A . H34A H 0.1852 0.0709 0.0481 0.059 Uiso 1 1 calc R . . C35 C 0.0560(9) 0.1097(7) 0.1536(5) 0.0463(19) Uani 1 1 d . A . C36 C 0.3223(9) 0.3346(9) 0.0671(6) 0.056(2) Uani 1 1 d . A . H36A H 0.3996 0.3806 0.1140 0.084 Uiso 1 1 calc R . . H36B H 0.2773 0.3964 0.0342 0.084 Uiso 1 1 calc R . . H36C H 0.3631 0.2752 0.0229 0.084 Uiso 1 1 calc R . . C37 C -0.0340(11) -0.0143(7) 0.1631(6) 0.066(3) Uani 1 1 d . . . H37A H -0.0179 -0.0314 0.2270 0.099 Uiso 1 1 calc R A . H37B H -0.0064 -0.0846 0.1208 0.099 Uiso 1 1 calc R . . H37C H -0.1366 -0.0080 0.1476 0.099 Uiso 1 1 calc R . . C41 C 0.2377(7) 0.6688(6) 0.1027(5) 0.0343(16) Uani 1 1 d . . . C42 C 0.3613(9) 0.7456(8) 0.1493(6) 0.062(3) Uani 1 1 d . A . H42A H 0.3983 0.7295 0.2086 0.074 Uiso 1 1 calc R . . C43 C 0.4312(9) 0.8447(8) 0.1112(5) 0.055(2) Uani 1 1 d . . . H43A H 0.5158 0.8961 0.1439 0.066 Uiso 1 1 calc R A . C44 C 0.3780(8) 0.8688(6) 0.0257(5) 0.0369(16) Uani 1 1 d . A . C45 C 0.2555(8) 0.7941(7) -0.0210(5) 0.0414(18) Uani 1 1 d . . . H45A H 0.2184 0.8115 -0.0798 0.050 Uiso 1 1 calc R A . C46 C 0.1849(8) 0.6929(7) 0.0170(5) 0.0400(17) Uani 1 1 d . A . H46A H 0.1010 0.6410 -0.0162 0.048 Uiso 1 1 calc R . . C51 C 0.2981(13) 0.0545(12) 0.3433(8) 0.091(4) Uani 1 1 d . . . H51A H 0.3310 0.0872 0.2882 0.137 Uiso 1 1 calc R . . H51B H 0.1956 0.0628 0.3456 0.137 Uiso 1 1 calc R . . H51C H 0.3109 -0.0362 0.3402 0.137 Uiso 1 1 calc R . . C52 C 0.3816(10) 0.1274(10) 0.4250(6) 0.062(2) Uani 1 1 d . . . H52A H 0.4836 0.1117 0.4261 0.075 Uiso 1 1 calc R . . H52B H 0.3795 0.2203 0.4241 0.075 Uiso 1 1 calc R . . C54 C 0.3967(11) 0.1671(10) 0.5847(7) 0.074(3) Uani 1 1 d . . . H54A H 0.5004 0.1565 0.5925 0.089 Uiso 1 1 calc R . . H54B H 0.3894 0.2593 0.5842 0.089 Uiso 1 1 calc R . . C55 C 0.3261(10) 0.1221(9) 0.6563(7) 0.071(3) Uani 1 1 d . . . H55A H 0.3533 0.1837 0.7134 0.107 Uiso 1 1 calc R . . H55B H 0.3544 0.0388 0.6661 0.107 Uiso 1 1 calc R . . H55C H 0.2212 0.1124 0.6397 0.107 Uiso 1 1 calc R . . B1 B -0.0531(9) 0.2558(7) 0.2807(5) 0.0360(19) Uani 1 1 d . A . H1 H -0.1200 0.1776 0.2884 0.043 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 W1 0.0619(2) 0.0467(2) 0.04009(19) 0.02289(14) -0.01343(14) -0.02925(15) Cl1A 0.045(2) 0.028(2) 0.038(2) 0.0031(16) 0.0049(17) -0.0091(19) Cl1B 0.040(3) 0.056(3) 0.038(3) 0.007(2) 0.000(2) 0.001(2) O48 0.048(3) 0.044(3) 0.036(3) 0.017(2) 0.001(2) -0.012(2) O53 0.066(4) 0.066(4) 0.075(5) 0.016(3) -0.008(4) -0.007(3) N11 0.037(3) 0.030(3) 0.029(3) 0.010(2) 0.001(2) -0.009(2) N12 0.039(3) 0.029(3) 0.036(3) 0.016(2) -0.007(3) -0.012(3) N21 0.043(3) 0.026(3) 0.036(3) 0.012(2) -0.001(3) -0.005(2) N22 0.038(3) 0.033(3) 0.031(3) 0.011(2) -0.003(3) -0.005(2) N31 0.052(4) 0.027(3) 0.029(3) 0.007(2) 0.003(3) -0.004(3) N32 0.038(3) 0.042(3) 0.031(3) 0.015(3) -0.008(3) -0.009(3) N47 0.043(3) 0.035(3) 0.036(3) 0.014(3) 0.012(3) -0.003(2) C13 0.044(4) 0.035(4) 0.037(4) 0.012(3) 0.003(3) 0.001(3) C14 0.040(4) 0.049(5) 0.064(5) 0.019(4) -0.011(4) -0.004(4) C15 0.039(4) 0.042(4) 0.046(4) 0.017(3) -0.002(3) -0.012(3) C16 0.054(5) 0.045(5) 0.079(6) 0.032(4) -0.003(5) 0.002(4) C17 0.046(4) 0.045(5) 0.060(5) 0.017(4) -0.005(4) -0.017(4) C23 0.040(4) 0.040(4) 0.032(4) 0.005(3) -0.001(3) 0.007(3) C24 0.053(5) 0.040(4) 0.029(4) 0.009(3) 0.000(3) 0.012(4) C25 0.047(4) 0.029(4) 0.034(4) 0.012(3) 0.006(3) 0.008(3) C26 0.053(5) 0.049(5) 0.040(4) 0.008(4) -0.004(4) 0.000(4) C27 0.072(6) 0.040(4) 0.045(5) 0.022(4) 0.013(4) 0.001(4) C33 0.046(4) 0.046(4) 0.028(4) 0.005(3) 0.010(3) 0.010(3) C34 0.069(6) 0.044(5) 0.036(4) 0.006(4) 0.005(4) 0.013(4) C35 0.069(5) 0.027(4) 0.043(4) 0.012(3) -0.007(4) 0.006(4) C36 0.054(5) 0.070(6) 0.040(5) 0.001(4) 0.011(4) -0.005(4) C37 0.108(8) 0.028(4) 0.058(5) 0.004(4) 0.006(5) -0.003(5) C41 0.039(4) 0.030(4) 0.033(4) 0.010(3) 0.004(3) -0.003(3) C42 0.062(5) 0.065(6) 0.050(5) 0.032(4) -0.015(4) -0.029(4) C43 0.058(5) 0.058(5) 0.040(4) 0.024(4) -0.010(4) -0.028(4) C44 0.044(4) 0.033(4) 0.034(4) 0.009(3) 0.008(3) 0.000(3) C45 0.045(4) 0.046(4) 0.032(4) 0.016(3) 0.003(3) -0.007(3) C46 0.042(4) 0.041(4) 0.035(4) 0.011(3) 0.004(3) -0.004(3) C51 0.102(9) 0.094(9) 0.083(8) 0.022(7) 0.019(7) 0.018(7) C52 0.061(6) 0.075(6) 0.055(6) 0.012(5) 0.020(5) 0.017(5) C54 0.059(6) 0.072(7) 0.081(7) -0.001(6) -0.026(5) 0.007(5) C55 0.057(5) 0.069(6) 0.077(7) 0.027(5) -0.031(5) -0.020(5) B1 0.044(5) 0.027(4) 0.034(4) 0.010(3) 0.001(4) -0.009(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 W1 O1A 1.846(17) . ? W1 O1B 1.952(14) . ? W1 O48 1.954(5) . ? W1 Cl1B 2.138(6) . ? W1 N22 2.147(5) . ? W1 Cl1A 2.187(4) . ? W1 N32 2.187(6) . ? W1 N12 2.225(5) . ? O48 C41 1.357(7) . ? O53 C52 1.360(10) . ? O53 C54 1.401(11) . ? N11 C15 1.339(9) . ? N11 N12 1.364(7) . ? N11 B1 1.541(10) . ? N12 C13 1.337(9) . ? N21 C25 1.356(8) . ? N21 N22 1.381(7) . ? N21 B1 1.537(9) . ? N22 C23 1.347(8) . ? N31 C35 1.342(9) . ? N31 N32 1.380(7) . ? N31 B1 1.546(10) . ? N32 C33 1.359(9) . ? N47 N47 1.244(11) 2_675 ? N47 C44 1.430(8) . ? C13 C14 1.384(10) . ? C13 C16 1.495(10) . ? C14 C15 1.383(10) . ? C15 C17 1.493(9) . ? C23 C24 1.381(9) . ? C23 C26 1.486(10) . ? C24 C25 1.364(10) . ? C25 C27 1.501(9) . ? C33 C34 1.376(11) . ? C33 C36 1.483(10) . ? C34 C35 1.371(11) . ? C35 C37 1.501(10) . ? C41 C46 1.375(9) . ? C41 C42 1.390(10) . ? C42 C43 1.379(9) . ? C43 C44 1.373(10) . ? C44 C45 1.374(10) . ? C45 C46 1.397(9) . ? C51 C52 1.437(14) . ? C54 C55 1.398(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1A W1 O1B 110.7(6) . . ? O1A W1 O48 96.5(6) . . ? O1B W1 O48 97.9(4) . . ? O1A W1 Cl1B 9.9(6) . . ? O1B W1 Cl1B 100.9(4) . . ? O48 W1 Cl1B 99.2(2) . . ? O1A W1 N22 92.2(6) . . ? O1B W1 N22 87.7(4) . . ? O48 W1 N22 167.26(19) . . ? Cl1B W1 N22 91.0(2) . . ? O1A W1 Cl1A 102.7(5) . . ? O1B W1 Cl1A 11.3(4) . . ? O48 W1 Cl1A 91.29(19) . . ? Cl1B W1 Cl1A 93.0(2) . . ? N22 W1 Cl1A 95.87(19) . . ? O1A W1 N32 84.6(5) . . ? O1B W1 N32 163.7(4) . . ? O48 W1 N32 85.6(2) . . ? Cl1B W1 N32 94.3(2) . . ? N22 W1 N32 86.0(2) . . ? Cl1A W1 N32 172.44(19) . . ? O1A W1 N12 163.0(5) . . ? O1B W1 N12 85.4(4) . . ? O48 W1 N12 86.2(2) . . ? Cl1B W1 N12 171.0(2) . . ? N22 W1 N12 82.8(2) . . ? Cl1A W1 N12 94.1(2) . . ? N32 W1 N12 78.8(2) . . ? C41 O48 W1 134.4(4) . . ? C52 O53 C54 113.4(8) . . ? C15 N11 N12 110.3(5) . . ? C15 N11 B1 130.9(5) . . ? N12 N11 B1 118.8(5) . . ? C13 N12 N11 107.0(5) . . ? C13 N12 W1 131.6(4) . . ? N11 N12 W1 121.0(4) . . ? C25 N21 N22 109.2(5) . . ? C25 N21 B1 130.1(5) . . ? N22 N21 B1 120.4(5) . . ? C23 N22 N21 106.8(5) . . ? C23 N22 W1 132.1(4) . . ? N21 N22 W1 121.0(4) . . ? C35 N31 N32 109.8(6) . . ? C35 N31 B1 130.6(6) . . ? N32 N31 B1 119.4(5) . . ? C33 N32 N31 106.1(6) . . ? C33 N32 W1 133.0(5) . . ? N31 N32 W1 120.8(4) . . ? N47 N47 C44 115.7(7) 2_675 . ? N12 C13 C14 109.0(6) . . ? N12 C13 C16 123.5(6) . . ? C14 C13 C16 127.5(7) . . ? C15 C14 C13 106.7(7) . . ? N11 C15 C14 106.9(6) . . ? N11 C15 C17 123.5(7) . . ? C14 C15 C17 129.6(7) . . ? N22 C23 C24 108.8(6) . . ? N22 C23 C26 123.2(6) . . ? C24 C23 C26 128.0(7) . . ? C25 C24 C23 107.8(6) . . ? N21 C25 C24 107.4(6) . . ? N21 C25 C27 122.2(6) . . ? C24 C25 C27 130.3(6) . . ? N32 C33 C34 109.1(6) . . ? N32 C33 C36 122.3(7) . . ? C34 C33 C36 128.6(7) . . ? C35 C34 C33 107.3(7) . . ? N31 C35 C34 107.7(6) . . ? N31 C35 C37 123.1(7) . . ? C34 C35 C37 129.2(8) . . ? O48 C41 C46 118.0(6) . . ? O48 C41 C42 123.0(6) . . ? C46 C41 C42 119.0(6) . . ? C43 C42 C41 121.2(7) . . ? C44 C43 C42 119.7(7) . . ? C43 C44 C45 119.7(6) . . ? C43 C44 N47 124.2(6) . . ? C45 C44 N47 116.1(6) . . ? C44 C45 C46 120.9(7) . . ? C41 C46 C45 119.5(7) . . ? O53 C52 C51 110.3(9) . . ? C55 C54 O53 106.1(8) . . ? N21 B1 N11 107.9(6) . . ? N21 B1 N31 108.8(6) . . ? N11 B1 N31 108.9(5) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 4.027 _refine_diff_density_min -3.483 _refine_diff_density_rms 0.152 #=END data_complex1 _database_code_CSD 192531 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H27 B Cl N6 O2 W' _chemical_formula_weight 625.60 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' Cl Cl 0.1484 0.1585 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.429(4) _cell_length_b 11.283(4) _cell_length_c 11.437(5) _cell_angle_alpha 86.39(3) _cell_angle_beta 76.986(19) _cell_angle_gamma 66.99(2) _cell_volume 1206.5(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.722 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 614 _exptl_absorpt_coefficient_mu 4.928 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.09 _exptl_absorpt_correction_T_max 0.60 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8793 _diffrn_reflns_av_R_equivalents 0.1370 _diffrn_reflns_av_sigmaI/netI 0.1062 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 23.00 _reflns_number_total 3355 _reflns_number_gt 2903 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0638P)^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 3355 _refine_ls_number_parameters 297 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0565 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1316 _refine_ls_wR_factor_gt 0.1251 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.102 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.20878(4) 0.16401(3) 0.30096(3) 0.0520(2) Uani 1 1 d . . . O41 O 0.2890(7) 0.0592(6) 0.1527(5) 0.0545(16) Uani 1 1 d . A . N11 N 0.4857(7) 0.1816(6) 0.3530(6) 0.0426(16) Uani 1 1 d . . . N12 N 0.4323(8) 0.0956(6) 0.3243(6) 0.0457(17) Uani 1 1 d . A . N21 N 0.2557(8) 0.3444(6) 0.4693(6) 0.0431(17) Uani 1 1 d . . . N22 N 0.1645(7) 0.2880(6) 0.4564(5) 0.0386(16) Uani 1 1 d . A . N31 N 0.3429(7) 0.3768(6) 0.2498(6) 0.0430(17) Uani 1 1 d . . . N32 N 0.2775(8) 0.3119(7) 0.1995(6) 0.0473(18) Uani 1 1 d . A . C13 C 0.5384(9) -0.0224(7) 0.3154(7) 0.046(2) Uani 1 1 d . . . C14 C 0.6581(9) -0.0108(9) 0.3406(8) 0.055(2) Uani 1 1 d . A . H14A H 0.7453 -0.0776 0.3420 0.066 Uiso 1 1 calc R . . C15 C 0.6228(9) 0.1177(8) 0.3629(8) 0.050(2) Uani 1 1 d . A . C16 C 0.5203(10) -0.1383(8) 0.2827(8) 0.058(3) Uani 1 1 d . A . H16A H 0.4424 -0.1483 0.3396 0.087 Uiso 1 1 calc R . . H16B H 0.6063 -0.2126 0.2833 0.087 Uiso 1 1 calc R . . H16C H 0.5005 -0.1294 0.2039 0.087 Uiso 1 1 calc R . . C17 C 0.7096(10) 0.1851(10) 0.3903(10) 0.070(3) Uani 1 1 d . . . H17A H 0.6673 0.2268 0.4681 0.105 Uiso 1 1 calc R A . H17B H 0.7133 0.2484 0.3309 0.105 Uiso 1 1 calc R . . H17C H 0.8047 0.1238 0.3897 0.105 Uiso 1 1 calc R . . C23 C 0.0576(8) 0.3182(7) 0.5566(7) 0.041(2) Uani 1 1 d . . . C24 C 0.0860(9) 0.3942(8) 0.6321(7) 0.046(2) Uani 1 1 d . A . H24A H 0.0313 0.4281 0.7075 0.055 Uiso 1 1 calc R . . C25 C 0.2080(9) 0.4092(7) 0.5751(7) 0.047(2) Uani 1 1 d . A . C26 C -0.0600(10) 0.2742(9) 0.5777(8) 0.054(2) Uani 1 1 d . A . H26A H -0.1213 0.3153 0.5233 0.081 Uiso 1 1 calc R . . H26B H -0.1136 0.2958 0.6589 0.081 Uiso 1 1 calc R . . H26C H -0.0224 0.1825 0.5649 0.081 Uiso 1 1 calc R . . C27 C 0.2883(11) 0.4764(9) 0.6184(9) 0.061(3) Uani 1 1 d . . . H27A H 0.3035 0.5374 0.5603 0.091 Uiso 1 1 calc R A . H27B H 0.3787 0.4141 0.6291 0.091 Uiso 1 1 calc R . . H27C H 0.2340 0.5206 0.6935 0.091 Uiso 1 1 calc R . . C33 C 0.2553(11) 0.3729(8) 0.0933(7) 0.054(2) Uani 1 1 d . . . C34 C 0.3017(10) 0.4746(9) 0.0818(8) 0.059(3) Uani 1 1 d . A . H34A H 0.2941 0.5336 0.0206 0.071 Uiso 1 1 calc R . . C35 C 0.3610(10) 0.4703(7) 0.1790(8) 0.048(2) Uani 1 1 d . A . C36 C 0.1855(14) 0.3286(10) 0.0122(9) 0.075(3) Uani 1 1 d . A . H36A H 0.2095 0.3562 -0.0680 0.113 Uiso 1 1 calc R . . H36B H 0.0838 0.3652 0.0409 0.113 Uiso 1 1 calc R . . H36C H 0.2189 0.2364 0.0121 0.113 Uiso 1 1 calc R . . C37 C 0.4252(11) 0.5611(9) 0.2099(9) 0.063(3) Uani 1 1 d . . . H37A H 0.3856 0.5900 0.2922 0.094 Uiso 1 1 calc R A . H37B H 0.4038 0.6340 0.1589 0.094 Uiso 1 1 calc R . . H37C H 0.5269 0.5167 0.1981 0.094 Uiso 1 1 calc R . . C41 C 0.2500(10) -0.0230(8) 0.1005(7) 0.046(2) Uani 1 1 d . . . C42 C 0.1220(12) -0.0397(11) 0.1440(9) 0.072(3) Uani 1 1 d . A . H42A H 0.0590 0.0059 0.2125 0.086 Uiso 1 1 calc R . . C43 C 0.0887(13) -0.1235(10) 0.0854(10) 0.076(3) Uani 1 1 d . . . H43A H 0.0031 -0.1342 0.1142 0.091 Uiso 1 1 calc R A . C44 C 0.1839(12) -0.1923(8) -0.0172(8) 0.061(3) Uani 1 1 d . A . H44A H 0.1601 -0.2462 -0.0587 0.074 Uiso 1 1 calc R . . C45 C 0.3123(11) -0.1803(9) -0.0567(8) 0.057(2) Uani 1 1 d . . . H45A H 0.3781 -0.2298 -0.1221 0.068 Uiso 1 1 calc R A . C46 C 0.3434(10) -0.0946(8) 0.0007(7) 0.050(2) Uani 1 1 d . A . H46A H 0.4293 -0.0847 -0.0284 0.060 Uiso 1 1 calc R . . B1 B 0.3892(11) 0.3289(9) 0.3690(9) 0.043(2) Uani 1 1 d . A . H1A H 0.454(10) 0.369(8) 0.392(7) 0.052 Uiso 1 1 d . . . Cl1 Cl -0.0004(8) 0.2687(7) 0.2539(7) 0.054(3) Uiso 0.488(13) 1 d P A 1 O1 O 0.1869(18) 0.0445(17) 0.4033(13) 0.056(4) Uiso 0.488(13) 1 d P A 1 Cl1' Cl 0.1608(7) 0.0085(6) 0.4078(5) 0.0596(19) Uiso 0.512(13) 1 d P A 2 O1' O 0.0108(14) 0.2590(13) 0.2773(13) 0.029(4) Uiso 0.512(13) 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.0565(3) 0.0561(3) 0.0475(3) -0.01293(17) 0.00594(18) -0.0334(2) O41 0.053(4) 0.052(4) 0.054(3) -0.013(3) 0.004(3) -0.022(3) N11 0.036(4) 0.030(3) 0.058(4) 0.000(3) -0.005(3) -0.012(3) N12 0.048(4) 0.035(4) 0.049(4) -0.002(3) 0.001(3) -0.018(3) N21 0.045(4) 0.035(4) 0.053(4) -0.003(3) -0.011(3) -0.018(3) N22 0.033(4) 0.041(4) 0.043(4) 0.002(3) -0.007(3) -0.016(3) N31 0.035(4) 0.033(4) 0.051(4) 0.005(3) 0.000(3) -0.008(3) N32 0.050(4) 0.040(4) 0.048(4) -0.010(3) -0.005(3) -0.016(3) C13 0.042(5) 0.033(4) 0.056(5) 0.002(4) -0.011(4) -0.006(4) C14 0.029(5) 0.056(6) 0.072(6) 0.011(4) -0.012(4) -0.007(4) C15 0.035(5) 0.044(5) 0.067(6) 0.004(4) -0.015(4) -0.011(4) C16 0.051(6) 0.039(5) 0.068(6) -0.003(4) -0.011(4) -0.002(4) C17 0.036(5) 0.072(7) 0.107(8) -0.001(6) -0.029(5) -0.019(5) C23 0.035(4) 0.036(4) 0.044(4) -0.008(3) -0.008(4) -0.003(4) C24 0.048(5) 0.039(4) 0.041(4) -0.003(4) -0.008(4) -0.007(4) C25 0.049(5) 0.037(4) 0.050(5) -0.005(4) -0.014(4) -0.008(4) C26 0.045(5) 0.060(6) 0.049(5) -0.009(4) -0.004(4) -0.013(4) C27 0.068(7) 0.047(5) 0.070(6) -0.008(4) -0.025(5) -0.018(5) C33 0.066(6) 0.046(5) 0.041(5) -0.001(4) -0.006(4) -0.015(5) C34 0.051(6) 0.058(6) 0.048(5) 0.013(4) -0.001(4) -0.007(5) C35 0.046(5) 0.029(4) 0.060(5) 0.004(4) 0.001(4) -0.014(4) C36 0.105(9) 0.068(7) 0.057(6) 0.011(5) -0.032(6) -0.031(6) C37 0.054(6) 0.059(6) 0.075(6) 0.008(5) -0.007(5) -0.027(5) C41 0.053(6) 0.041(5) 0.041(4) 0.000(4) -0.008(4) -0.016(4) C42 0.065(7) 0.081(7) 0.069(6) -0.030(5) 0.014(5) -0.039(6) C43 0.078(8) 0.075(7) 0.085(7) -0.021(6) -0.006(6) -0.043(6) C44 0.085(8) 0.038(5) 0.061(6) -0.008(4) -0.030(5) -0.015(5) C45 0.053(6) 0.057(6) 0.049(5) -0.009(4) -0.006(4) -0.011(5) C46 0.051(5) 0.051(5) 0.039(4) -0.004(4) -0.005(4) -0.011(4) B1 0.038(5) 0.041(5) 0.055(6) 0.001(4) -0.010(4) -0.018(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 O1 1.779(18) . ? W1 O41 1.954(6) . ? W1 O1' 1.992(14) . ? W1 N22 2.183(6) . ? W1 Cl1 2.209(8) . ? W1 N12 2.225(7) . ? W1 N32 2.227(8) . ? W1 Cl1' 2.228(8) . ? O41 C41 1.362(11) . ? N11 C15 1.354(10) . ? N11 N12 1.380(10) . ? N11 B1 1.568(11) . ? N12 C13 1.350(10) . ? N21 C25 1.343(10) . ? N21 N22 1.371(10) . ? N21 B1 1.549(13) . ? N22 C23 1.360(10) . ? N31 C35 1.335(11) . ? N31 N32 1.398(10) . ? N31 B1 1.544(12) . ? N32 C33 1.379(10) . ? C13 C14 1.397(13) . ? C13 C16 1.473(13) . ? C14 C15 1.375(12) . ? C15 C17 1.481(14) . ? C23 C24 1.405(12) . ? C23 C26 1.463(13) . ? C24 C25 1.361(13) . ? C25 C27 1.500(14) . ? C33 C34 1.398(15) . ? C33 C36 1.512(15) . ? C34 C35 1.378(13) . ? C35 C37 1.521(14) . ? C41 C46 1.380(11) . ? C41 C42 1.397(14) . ? C42 C43 1.380(15) . ? C43 C44 1.398(15) . ? C44 C45 1.370(15) . ? C45 C46 1.375(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 W1 O41 99.1(5) . . ? O1 W1 O1' 101.8(7) . . ? O41 W1 O1' 98.7(4) . . ? O1 W1 N22 87.7(6) . . ? O41 W1 N22 166.9(3) . . ? O1' W1 N22 90.7(4) . . ? O1 W1 Cl1 106.2(6) . . ? O41 W1 Cl1 93.6(3) . . ? O1' W1 Cl1 6.2(5) . . ? N22 W1 Cl1 95.2(2) . . ? O1 W1 N12 87.4(6) . . ? O41 W1 N12 86.0(3) . . ? O1' W1 N12 168.8(4) . . ? N22 W1 N12 83.2(2) . . ? Cl1 W1 N12 166.3(3) . . ? O1 W1 N32 165.2(6) . . ? O41 W1 N32 87.0(3) . . ? O1' W1 N32 90.4(4) . . ? N22 W1 N32 83.8(2) . . ? Cl1 W1 N32 86.7(3) . . ? N12 W1 N32 79.6(3) . . ? O1 W1 Cl1' 9.9(6) . . ? O41 W1 Cl1' 93.2(2) . . ? O1' W1 Cl1' 95.1(4) . . ? N22 W1 Cl1' 95.0(2) . . ? Cl1 W1 Cl1' 98.9(3) . . ? N12 W1 Cl1' 94.8(2) . . ? N32 W1 Cl1' 174.3(2) . . ? C41 O41 W1 133.7(6) . . ? C15 N11 N12 109.7(6) . . ? C15 N11 B1 130.1(7) . . ? N12 N11 B1 120.1(7) . . ? C13 N12 N11 107.0(7) . . ? C13 N12 W1 132.5(6) . . ? N11 N12 W1 120.5(5) . . ? C25 N21 N22 109.6(7) . . ? C25 N21 B1 129.9(8) . . ? N22 N21 B1 120.5(6) . . ? C23 N22 N21 107.7(6) . . ? C23 N22 W1 130.6(6) . . ? N21 N22 W1 121.6(5) . . ? C35 N31 N32 111.1(7) . . ? C35 N31 B1 130.4(8) . . ? N32 N31 B1 118.4(7) . . ? C33 N32 N31 104.5(8) . . ? C33 N32 W1 133.7(7) . . ? N31 N32 W1 121.3(5) . . ? N12 C13 C14 108.6(8) . . ? N12 C13 C16 122.0(8) . . ? C14 C13 C16 129.4(7) . . ? C15 C14 C13 107.2(7) . . ? N11 C15 C14 107.4(8) . . ? N11 C15 C17 122.1(7) . . ? C14 C15 C17 130.4(8) . . ? N22 C23 C24 107.0(8) . . ? N22 C23 C26 124.3(7) . . ? C24 C23 C26 128.7(8) . . ? C25 C24 C23 107.7(7) . . ? N21 C25 C24 108.0(8) . . ? N21 C25 C27 122.5(9) . . ? C24 C25 C27 129.4(8) . . ? N32 C33 C34 109.6(8) . . ? N32 C33 C36 120.1(9) . . ? C34 C33 C36 130.3(8) . . ? C35 C34 C33 106.5(8) . . ? N31 C35 C34 108.1(8) . . ? N31 C35 C37 124.0(8) . . ? C34 C35 C37 127.6(8) . . ? O41 C41 C46 117.9(9) . . ? O41 C41 C42 123.4(8) . . ? C46 C41 C42 118.7(9) . . ? C43 C42 C41 120.2(9) . . ? C42 C43 C44 119.7(12) . . ? C45 C44 C43 120.1(10) . . ? C44 C45 C46 119.7(9) . . ? C45 C46 C41 121.5(10) . . ? N31 B1 N21 109.5(7) . . ? N31 B1 N11 108.3(7) . . ? N21 B1 N11 107.6(7) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.327 _refine_diff_density_min -2.615 _refine_diff_density_rms 0.162 #=END data_complex2 _database_code_CSD 192532 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H29 B Cl N6 O3 W' _chemical_formula_weight 655.62 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' Cl Cl 0.1484 0.1585 '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 trinclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.872(2) _cell_length_b 10.929(5) _cell_length_c 12.296(4) _cell_angle_alpha 68.91(3) _cell_angle_beta 82.24(2) _cell_angle_gamma 65.41(3) _cell_volume 1239.4(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.757 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 646 _exptl_absorpt_coefficient_mu 4.804 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.09 _exptl_absorpt_correction_T_max 0.63 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13028 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_sigmaI/netI 0.0346 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 27.54 _reflns_number_total 5633 _reflns_number_gt 4795 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0414P)^2^+0.6837P] 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 5633 _refine_ls_number_parameters 335 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0416 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_ref 0.0792 _refine_ls_wR_factor_gt 0.0758 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W -0.166013(18) 0.767022(18) 0.687148(15) 0.03896(8) Uani 1 1 d . . . N11 N -0.0895(3) 0.5468(4) 0.6807(3) 0.0325(7) Uani 1 1 d . A . N12 N -0.1757(3) 0.4972(3) 0.6546(3) 0.0304(7) Uani 1 1 d . . . N21 N -0.3255(3) 0.6946(3) 0.7874(3) 0.0295(7) Uani 1 1 d . A . N22 N -0.3843(3) 0.6333(3) 0.7424(3) 0.0277(7) Uani 1 1 d . . . N31 N -0.2847(3) 0.8198(4) 0.5374(3) 0.0317(7) Uani 1 1 d . A . N32 N -0.3419(3) 0.7311(4) 0.5301(3) 0.0314(7) Uani 1 1 d . . . C12 C 0.0350(4) 0.4398(5) 0.6959(4) 0.0391(10) Uani 1 1 d . . . C13 C -0.1054(4) 0.3620(5) 0.6566(4) 0.0378(9) Uani 1 1 d . A . C14 C 0.0281(5) 0.3243(5) 0.6796(4) 0.0432(10) Uani 1 1 d . A . H14A H 0.0997 0.2379 0.6836 0.052 Uiso 1 1 calc R . . C16 C -0.1726(5) 0.2745(5) 0.6399(5) 0.0503(12) Uani 1 1 d . . . H16A H -0.2227 0.3243 0.5675 0.075 Uiso 1 1 calc R A . H16B H -0.2331 0.2592 0.7030 0.075 Uiso 1 1 calc R . . H16C H -0.1051 0.1840 0.6386 0.075 Uiso 1 1 calc R . . C17 C 0.1560(5) 0.4543(5) 0.7277(5) 0.0539(13) Uani 1 1 d . A . H17A H 0.1378 0.4793 0.7972 0.081 Uiso 1 1 calc R . . H17B H 0.1743 0.5276 0.6651 0.081 Uiso 1 1 calc R . . H17C H 0.2331 0.3651 0.7411 0.081 Uiso 1 1 calc R . . C23 C -0.4876(4) 0.6153(4) 0.8104(3) 0.0296(8) Uani 1 1 d . A . C24 C -0.4918(4) 0.6632(4) 0.9003(3) 0.0314(8) Uani 1 1 d . . . H24A H -0.5524 0.6626 0.9614 0.038 Uiso 1 1 calc R A . C25 C -0.3923(4) 0.7116(4) 0.8844(3) 0.0316(8) Uani 1 1 d . A . C26 C -0.5735(5) 0.5499(5) 0.7867(4) 0.0419(10) Uani 1 1 d . . . H26A H -0.6055 0.5971 0.7072 0.063 Uiso 1 1 calc R A . H26B H -0.6492 0.5606 0.8379 0.063 Uiso 1 1 calc R . . H26C H -0.5207 0.4502 0.7997 0.063 Uiso 1 1 calc R . . C27 C -0.3558(5) 0.7751(5) 0.9579(4) 0.0447(11) Uani 1 1 d . . . H27A H -0.2598 0.7303 0.9725 0.067 Uiso 1 1 calc R A . H27B H -0.4020 0.7601 1.0307 0.067 Uiso 1 1 calc R . . H27C H -0.3819 0.8758 0.9178 0.067 Uiso 1 1 calc R . . C33 C -0.4093(4) 0.7891(5) 0.4278(4) 0.0361(9) Uani 1 1 d . A . C34 C -0.3971(4) 0.9175(5) 0.3674(4) 0.0383(10) Uani 1 1 d . . . H34A H -0.4339 0.9804 0.2943 0.046 Uiso 1 1 calc R A . C35 C -0.3197(4) 0.9338(4) 0.4372(3) 0.0330(9) Uani 1 1 d . A . C36 C -0.4843(5) 0.7190(6) 0.3949(4) 0.0494(12) Uani 1 1 d . . . H36A H -0.4250 0.6220 0.4032 0.074 Uiso 1 1 calc R A . H36B H -0.5156 0.7701 0.3155 0.074 Uiso 1 1 calc R . . H36C H -0.5603 0.7201 0.4450 0.074 Uiso 1 1 calc R . . C37 C -0.2762(5) 1.0536(5) 0.4127(4) 0.0398(10) Uani 1 1 d . . . H37A H -0.1791 1.0170 0.4143 0.060 Uiso 1 1 calc R A . H37B H -0.3116 1.0984 0.4709 0.060 Uiso 1 1 calc R . . H37C H -0.3097 1.1224 0.3372 0.060 Uiso 1 1 calc R . . C41 C 0.0100(4) 0.7275(4) 0.8804(3) 0.0297(8) Uani 1 1 d . . . C42 C 0.0209(6) 0.8572(6) 0.8292(5) 0.0646(18) Uani 1 1 d . A . H42A H -0.0228 0.9186 0.7581 0.077 Uiso 1 1 calc R . . C43 C 0.0958(6) 0.8986(5) 0.8818(4) 0.0557(14) Uani 1 1 d . . . H43A H 0.1020 0.9866 0.8459 0.067 Uiso 1 1 calc R A . C44 C 0.1602(4) 0.8088(4) 0.9864(4) 0.0328(9) Uani 1 1 d . A . C45 C 0.1500(5) 0.6788(5) 1.0378(4) 0.0382(10) Uani 1 1 d . . . H45A H 0.1937 0.6173 1.1088 0.046 Uiso 1 1 calc R A . C46 C 0.0757(4) 0.6386(4) 0.9852(4) 0.0343(9) Uani 1 1 d . A . H46A H 0.0700 0.5503 1.0211 0.041 Uiso 1 1 calc R . . C47 C 0.2491(6) 0.9706(6) 0.9949(5) 0.0572(14) Uani 1 1 d . A . H47A H 0.3038 0.9795 1.0444 0.086 Uiso 1 1 calc R . . H47B H 0.1608 1.0467 0.9850 0.086 Uiso 1 1 calc R . . H47C H 0.2907 0.9757 0.9203 0.086 Uiso 1 1 calc R . . B1 B -0.3275(5) 0.5935(5) 0.6328(4) 0.0307(9) Uani 1 1 d . A . H1A H -0.374(5) 0.531(5) 0.614(4) 0.046 Uiso 1 1 d . . . O41 O -0.0645(3) 0.6836(3) 0.8336(2) 0.0351(6) Uani 1 1 d . A . O47 O 0.2372(3) 0.8385(3) 1.0462(3) 0.0435(7) Uani 1 1 d . . . Cl1 Cl 0.0049(4) 0.8110(4) 0.5855(3) 0.0397(9) Uani 0.522(8) 1 d P A 1 O1 O -0.2742(13) 0.9410(13) 0.6963(11) 0.037(2) Uani 0.522(8) 1 d P A 1 Cl1' Cl -0.2691(5) 0.9762(5) 0.7102(4) 0.0349(9) Uani 0.478(8) 1 d P A 2 O1' O -0.0317(12) 0.7920(12) 0.5846(10) 0.040(2) Uani 0.478(8) 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.05116(12) 0.03457(11) 0.03759(10) 0.00426(7) -0.01609(8) -0.03189(9) N11 0.0310(17) 0.0330(18) 0.0402(18) -0.0115(15) -0.0026(14) -0.0187(15) N12 0.0342(17) 0.0277(16) 0.0355(17) -0.0101(14) -0.0018(14) -0.0177(14) N21 0.0355(17) 0.0303(17) 0.0298(16) -0.0044(14) -0.0048(14) -0.0230(14) N22 0.0312(16) 0.0268(16) 0.0314(16) -0.0060(13) -0.0025(13) -0.0195(13) N31 0.0352(18) 0.0326(17) 0.0315(17) -0.0066(14) -0.0021(14) -0.0204(15) N32 0.0335(17) 0.0349(18) 0.0329(17) -0.0100(14) -0.0028(14) -0.0205(15) C12 0.033(2) 0.035(2) 0.048(2) -0.0088(19) -0.0031(19) -0.0147(18) C13 0.045(2) 0.033(2) 0.041(2) -0.0132(19) 0.0035(19) -0.0213(19) C14 0.040(2) 0.033(2) 0.056(3) -0.017(2) 0.004(2) -0.0127(19) C16 0.062(3) 0.037(2) 0.066(3) -0.024(2) 0.001(3) -0.027(2) C17 0.032(2) 0.046(3) 0.085(4) -0.023(3) -0.007(2) -0.014(2) C23 0.0288(19) 0.0268(19) 0.036(2) -0.0055(16) -0.0027(16) -0.0166(16) C24 0.037(2) 0.028(2) 0.0319(19) -0.0130(16) 0.0075(16) -0.0152(17) C25 0.041(2) 0.028(2) 0.0300(19) -0.0063(16) -0.0023(17) -0.0196(17) C26 0.047(2) 0.048(3) 0.045(2) -0.011(2) 0.000(2) -0.035(2) C27 0.061(3) 0.055(3) 0.040(2) -0.020(2) 0.008(2) -0.043(2) C33 0.036(2) 0.044(2) 0.033(2) -0.0141(19) -0.0034(17) -0.0177(19) C34 0.039(2) 0.044(2) 0.0282(19) -0.0050(18) -0.0031(17) -0.019(2) C35 0.033(2) 0.031(2) 0.0305(19) -0.0037(16) 0.0013(16) -0.0142(17) C36 0.056(3) 0.068(3) 0.041(2) -0.020(2) -0.009(2) -0.036(3) C37 0.046(2) 0.036(2) 0.035(2) -0.0003(18) -0.0030(19) -0.022(2) C41 0.033(2) 0.0282(19) 0.0339(19) -0.0064(16) -0.0035(16) -0.0202(16) C42 0.104(4) 0.047(3) 0.052(3) 0.020(2) -0.042(3) -0.058(3) C43 0.082(4) 0.043(3) 0.054(3) 0.005(2) -0.020(3) -0.048(3) C44 0.035(2) 0.037(2) 0.039(2) -0.0166(18) 0.0000(17) -0.0228(18) C45 0.047(2) 0.036(2) 0.034(2) -0.0066(18) -0.0092(19) -0.0206(19) C46 0.043(2) 0.0259(19) 0.036(2) -0.0026(17) -0.0055(18) -0.0207(18) C47 0.066(3) 0.059(3) 0.077(4) -0.031(3) 0.000(3) -0.046(3) B1 0.031(2) 0.032(2) 0.037(2) -0.0110(19) 0.0002(18) -0.0192(19) O41 0.0435(16) 0.0313(14) 0.0356(14) 0.0008(12) -0.0126(12) -0.0258(13) O47 0.0509(18) 0.0495(19) 0.0484(18) -0.0214(15) -0.0041(15) -0.0316(15) Cl1 0.0394(17) 0.0478(16) 0.0401(13) -0.0079(11) 0.0063(11) -0.0326(12) O1 0.041(4) 0.030(6) 0.044(5) -0.008(4) -0.007(3) -0.020(4) Cl1' 0.0396(14) 0.0272(19) 0.0420(16) -0.0099(13) -0.0051(11) -0.0170(13) O1' 0.044(6) 0.042(5) 0.045(4) -0.005(3) 0.006(4) -0.035(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 O1 1.808(12) . ? W1 O1' 1.839(12) . ? W1 O41 1.952(3) . ? W1 N31 2.155(3) . ? W1 Cl1' 2.193(5) . ? W1 Cl1 2.221(4) . ? W1 N11 2.223(4) . ? W1 N21 2.240(3) . ? N11 C12 1.352(5) . ? N11 N12 1.380(4) . ? N12 C13 1.344(5) . ? N12 B1 1.541(6) . ? N21 C25 1.341(5) . ? N21 N22 1.372(4) . ? N22 C23 1.346(5) . ? N22 B1 1.537(6) . ? N31 C35 1.357(5) . ? N31 N32 1.384(4) . ? N32 C33 1.345(5) . ? N32 B1 1.540(6) . ? C12 C14 1.380(6) . ? C12 C17 1.505(6) . ? C13 C14 1.373(6) . ? C13 C16 1.502(6) . ? C23 C24 1.372(6) . ? C23 C26 1.499(5) . ? C24 C25 1.353(5) . ? C25 C27 1.495(6) . ? C33 C34 1.384(6) . ? C33 C36 1.499(6) . ? C34 C35 1.380(6) . ? C35 C37 1.491(6) . ? C41 O41 1.365(4) . ? C41 C46 1.373(5) . ? C41 C42 1.378(6) . ? C42 C43 1.394(6) . ? C43 C44 1.368(6) . ? C44 C45 1.377(6) . ? C44 O47 1.383(5) . ? C45 C46 1.381(6) . ? C47 O47 1.406(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 O1 W1 O1' 106.6(5) . . ? O1 W1 O41 99.5(4) . . ? O1' W1 O41 99.3(4) . . ? O1 W1 N31 87.9(4) . . ? O1' W1 N31 86.9(4) . . ? O41 W1 N31 168.45(11) . . ? O1 W1 Cl1' 9.1(4) . . ? O1' W1 Cl1' 102.5(4) . . ? O41 W1 Cl1' 92.37(16) . . ? N31 W1 Cl1' 95.81(16) . . ? O1 W1 Cl1 101.3(4) . . ? O1' W1 Cl1 10.2(4) . . ? O41 W1 Cl1 91.79(13) . . ? N31 W1 Cl1 95.43(13) . . ? Cl1' W1 Cl1 96.04(17) . . ? O1 W1 N11 163.5(4) . . ? O1' W1 N11 87.0(4) . . ? O41 W1 N11 87.31(12) . . ? N31 W1 N11 83.28(13) . . ? Cl1' W1 N11 170.48(16) . . ? Cl1 W1 N11 93.48(14) . . ? O1 W1 N21 86.1(4) . . ? O1' W1 N21 164.1(4) . . ? O41 W1 N21 87.79(12) . . ? N31 W1 N21 83.89(12) . . ? Cl1' W1 N21 91.37(16) . . ? Cl1 W1 N21 172.59(14) . . ? N11 W1 N21 79.11(13) . . ? C12 N11 N12 106.4(3) . . ? C12 N11 W1 132.8(3) . . ? N12 N11 W1 120.8(2) . . ? C13 N12 N11 109.2(3) . . ? C13 N12 B1 130.8(3) . . ? N11 N12 B1 119.9(3) . . ? C25 N21 N22 107.1(3) . . ? C25 N21 W1 132.6(3) . . ? N22 N21 W1 119.9(2) . . ? C23 N22 N21 109.0(3) . . ? C23 N22 B1 130.5(3) . . ? N21 N22 B1 120.5(3) . . ? C35 N31 N32 106.4(3) . . ? C35 N31 W1 131.8(3) . . ? N32 N31 W1 121.8(2) . . ? C33 N32 N31 109.4(3) . . ? C33 N32 B1 130.2(3) . . ? N31 N32 B1 120.3(3) . . ? N11 C12 C14 109.6(4) . . ? N11 C12 C17 121.7(4) . . ? C14 C12 C17 128.8(4) . . ? N12 C13 C14 108.4(4) . . ? N12 C13 C16 122.1(4) . . ? C14 C13 C16 129.5(4) . . ? C13 C14 C12 106.4(4) . . ? N22 C23 C24 106.9(3) . . ? N22 C23 C26 123.1(4) . . ? C24 C23 C26 130.0(4) . . ? C25 C24 C23 108.0(4) . . ? N21 C25 C24 109.0(3) . . ? N21 C25 C27 122.3(4) . . ? C24 C25 C27 128.7(4) . . ? N32 C33 C34 108.2(4) . . ? N32 C33 C36 122.1(4) . . ? C34 C33 C36 129.7(4) . . ? C35 C34 C33 106.5(4) . . ? N31 C35 C34 109.5(4) . . ? N31 C35 C37 122.2(4) . . ? C34 C35 C37 128.2(4) . . ? O41 C41 C46 118.2(3) . . ? O41 C41 C42 123.6(4) . . ? C46 C41 C42 118.2(4) . . ? C41 C42 C43 121.5(4) . . ? C44 C43 C42 119.6(4) . . ? C43 C44 C45 119.3(4) . . ? C43 C44 O47 124.5(4) . . ? C45 C44 O47 116.2(4) . . ? C44 C45 C46 120.8(4) . . ? C41 C46 C45 120.7(4) . . ? N22 B1 N32 108.6(3) . . ? N22 B1 N12 108.1(3) . . ? N32 B1 N12 108.2(3) . . ? C41 O41 W1 132.8(2) . . ? C44 O47 C47 117.0(4) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.247 _refine_diff_density_min -1.743 _refine_diff_density_rms 0.114 #=END data_WtpOCl2 _database_code_CSD 192533 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H22 B Cl2 N6 O W' _chemical_formula_weight 567.95 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' Cl Cl 0.1484 0.1585 '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)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 8.008(2) _cell_length_b 13.970(4) _cell_length_c 8.963(2) _cell_angle_alpha 90.00(2) _cell_angle_beta 100.19(2) _cell_angle_gamma 90.000(18) _cell_volume 986.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.911 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 550 _exptl_absorpt_coefficient_mu 6.140 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.05 _exptl_absorpt_correction_T_max 0.70 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6421 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_sigmaI/netI 0.0421 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 27.52 _reflns_number_total 2358 _reflns_number_gt 1915 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0354P)^2^+9.8856P] 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 2358 _refine_ls_number_parameters 135 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0712 _refine_ls_R_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.1250 _refine_ls_wR_factor_gt 0.1181 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.116 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.05892(7) 0.2500 0.30264(5) 0.04421(19) Uani 1 2 d S . . N11 N 0.1699(7) 0.1470(5) 0.1630(6) 0.0296(13) Uani 1 1 d . A . N12 N 0.1562(7) 0.1602(4) 0.0085(6) 0.0266(12) Uani 1 1 d . . . N21 N -0.1491(9) 0.2500 0.1075(10) 0.040(2) Uani 1 2 d S A . N22 N -0.1184(10) 0.2500 -0.0391(9) 0.0291(18) Uani 1 2 d S . . C13 C 0.2263(9) 0.0853(6) -0.0523(9) 0.0336(17) Uani 1 1 d . A . C14 C 0.2865(10) 0.0225(6) 0.0645(10) 0.0401(19) Uani 1 1 d . . . H14A H 0.3421 -0.0367 0.0553 0.048 Uiso 1 1 calc R A . C15 C 0.2511(10) 0.0614(6) 0.1955(9) 0.0365(18) Uani 1 1 d . A . C16 C 0.2946(13) 0.0235(8) 0.3535(11) 0.059(3) Uani 1 1 d . . . H16A H 0.3576 0.0722 0.4193 0.089 Uiso 1 1 calc R A . H16B H 0.3646 -0.0341 0.3541 0.089 Uiso 1 1 calc R . . H16C H 0.1901 0.0074 0.3907 0.089 Uiso 1 1 calc R . . C17 C 0.2304(12) 0.0771(7) -0.2171(9) 0.051(2) Uani 1 1 d . . . H17A H 0.1148 0.0826 -0.2748 0.076 Uiso 1 1 calc R A . H17B H 0.2782 0.0150 -0.2378 0.076 Uiso 1 1 calc R . . H17C H 0.3008 0.1285 -0.2474 0.076 Uiso 1 1 calc R . . C23 C -0.2646(13) 0.2500 -0.1379(13) 0.034(2) Uani 1 2 d S A . C24 C -0.3960(13) 0.2500 -0.0566(14) 0.041(3) Uani 1 2 d S . . H24A H -0.5143 0.2500 -0.0957 0.049 Uiso 1 2 calc SR A . C25 C -0.3172(14) 0.2500 0.0962(13) 0.034(2) Uani 1 2 d S A . C26 C -0.4076(15) 0.2500 0.2306(15) 0.049(3) Uani 1 2 d S . . H26A H -0.3494 0.2936 0.3085 0.074 Uiso 0.50 1 calc PR A . H26B H -0.4069 0.1851 0.2723 0.074 Uiso 0.50 1 calc PR . . H26C H -0.5250 0.2712 0.1981 0.074 Uiso 0.50 1 calc PR . . C27 C -0.2726(17) 0.2500 -0.3057(14) 0.050(3) Uani 1 2 d S . . H27A H -0.3902 0.2596 -0.3564 0.075 Uiso 0.50 1 calc PR A . H27B H -0.2312 0.1885 -0.3372 0.075 Uiso 0.50 1 calc PR . . H27C H -0.2017 0.3019 -0.3336 0.075 Uiso 0.50 1 calc PR . . B1 B 0.0661(15) 0.2500 -0.0667(13) 0.030(2) Uani 1 2 d S . . H1 H 0.067(14) 0.2500 -0.183(13) 0.036 Uiso 1 2 d S . . Cl1 Cl 0.2949(5) 0.2500 0.4756(5) 0.0646(10) Uiso 1 2 d S A . Cl2 Cl -0.0605(9) 0.1307(6) 0.4141(9) 0.032(2) Uiso 0.50 1 d P A 1 O1 O -0.066(3) 0.1394(16) 0.396(2) 0.039(7) Uiso 0.50 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.0493(3) 0.0621(4) 0.0239(2) 0.000 0.01397(19) 0.000 N11 0.027(3) 0.040(4) 0.023(3) 0.003(3) 0.008(2) 0.002(3) N12 0.026(3) 0.031(3) 0.023(3) 0.000(2) 0.006(2) 0.000(2) N21 0.003(3) 0.079(8) 0.035(5) 0.000 -0.003(3) 0.000 N22 0.027(4) 0.034(5) 0.025(4) 0.000 0.001(3) 0.000 C13 0.032(4) 0.030(4) 0.039(4) -0.008(3) 0.007(3) 0.001(3) C14 0.041(4) 0.031(4) 0.049(5) 0.000(4) 0.009(4) 0.012(4) C15 0.033(4) 0.035(4) 0.042(4) 0.008(4) 0.008(3) 0.012(3) C16 0.066(6) 0.061(7) 0.053(6) 0.027(5) 0.016(5) 0.028(5) C17 0.061(6) 0.057(6) 0.035(4) -0.018(4) 0.009(4) 0.011(5) C23 0.029(5) 0.027(6) 0.042(6) 0.000 -0.006(4) 0.000 C24 0.017(5) 0.058(8) 0.046(7) 0.000 0.000(4) 0.000 C25 0.037(6) 0.028(6) 0.035(6) 0.000 -0.002(5) 0.000 C26 0.028(6) 0.073(10) 0.048(7) 0.000 0.012(5) 0.000 C27 0.044(7) 0.063(9) 0.039(7) 0.000 -0.006(5) 0.000 B1 0.027(6) 0.042(7) 0.021(5) 0.000 0.005(4) 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 W1 O1 2.10(2) 4_565 ? W1 O1 2.10(2) . ? W1 N21 2.192(8) . ? W1 N11 2.195(6) . ? W1 N11 2.195(6) 4_565 ? W1 Cl1 2.222(4) . ? W1 Cl2 2.243(8) . ? W1 Cl2 2.243(8) 4_565 ? N11 C15 1.368(10) . ? N11 N12 1.382(8) . ? N12 C13 1.347(9) . ? N12 B1 1.542(9) . ? N21 C25 1.332(13) . ? N21 N22 1.379(12) . ? N22 C23 1.337(13) . ? N22 B1 1.541(14) . ? C13 C14 1.385(11) . ? C13 C17 1.488(11) . ? C14 C15 1.368(11) . ? C15 C16 1.494(11) . ? C23 C24 1.382(16) . ? C23 C27 1.495(17) . ? C24 C25 1.403(16) . ? C25 C26 1.511(16) . ? B1 N12 1.542(9) 4_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 W1 O1 95.0(13) 4_565 . ? O1 W1 N21 88.3(6) 4_565 . ? O1 W1 N21 88.3(6) . . ? O1 W1 N11 169.0(6) 4_565 . ? O1 W1 N11 90.9(7) . . ? N21 W1 N11 82.7(2) . . ? O1 W1 N11 90.9(7) 4_565 4_565 ? O1 W1 N11 169.0(6) . 4_565 ? N21 W1 N11 82.7(2) . 4_565 ? N11 W1 N11 81.9(3) . 4_565 ? O1 W1 Cl1 97.4(6) 4_565 . ? O1 W1 Cl1 97.4(6) . . ? N21 W1 Cl1 171.6(2) . . ? N11 W1 Cl1 91.02(17) . . ? N11 W1 Cl1 91.02(17) 4_565 . ? O1 W1 Cl2 95.6(5) 4_565 . ? O1 W1 Cl2 3.6(7) . . ? N21 W1 Cl2 91.8(2) . . ? N11 W1 Cl2 90.8(3) . . ? N11 W1 Cl2 171.3(2) 4_565 . ? Cl1 W1 Cl2 93.8(2) . . ? O1 W1 Cl2 3.6(7) 4_565 4_565 ? O1 W1 Cl2 95.6(5) . 4_565 ? N21 W1 Cl2 91.8(2) . 4_565 ? N11 W1 Cl2 171.3(2) . 4_565 ? N11 W1 Cl2 90.8(3) 4_565 4_565 ? Cl1 W1 Cl2 93.8(2) . 4_565 ? Cl2 W1 Cl2 96.0(4) . 4_565 ? C15 N11 N12 106.3(6) . . ? C15 N11 W1 132.6(5) . . ? N12 N11 W1 121.1(5) . . ? C13 N12 N11 109.7(6) . . ? C13 N12 B1 130.6(7) . . ? N11 N12 B1 119.6(6) . . ? C25 N21 N22 106.0(8) . . ? C25 N21 W1 132.5(8) . . ? N22 N21 W1 121.5(6) . . ? C23 N22 N21 110.4(9) . . ? C23 N22 B1 130.3(9) . . ? N21 N22 B1 119.4(8) . . ? N12 C13 C14 107.5(7) . . ? N12 C13 C17 123.0(7) . . ? C14 C13 C17 129.5(7) . . ? C15 C14 C13 107.5(7) . . ? C14 C15 N11 109.1(7) . . ? C14 C15 C16 128.6(8) . . ? N11 C15 C16 122.3(8) . . ? N22 C23 C24 108.1(10) . . ? N22 C23 C27 122.9(10) . . ? C24 C23 C27 129.0(10) . . ? C23 C24 C25 105.2(9) . . ? N21 C25 C24 110.4(10) . . ? N21 C25 C26 124.0(10) . . ? C24 C25 C26 125.6(10) . . ? N22 B1 N12 108.5(6) . . ? N22 B1 N12 108.5(6) . 4_565 ? N12 B1 N12 108.9(8) . 4_565 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.899 _refine_diff_density_min -3.269 _refine_diff_density_rms 0.193 #=END