# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2003 data_global _publ_contact_author_email MIKE.WARD@BRISTOL.AC.UK _publ_contact_author_name 'Prof Michael Ward' _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name M.Ward Z.R.Bell R.H.Laye data_blinda _database_code_CSD 199480 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H30 B Mo N6 O3' _chemical_formula_weight 593.32 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.848(2) _cell_length_b 9.7316(14) _cell_length_c 21.776(5) _cell_angle_alpha 90.00 _cell_angle_beta 106.361(17) _cell_angle_gamma 90.00 _cell_volume 2612.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(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 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.509 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1220 _exptl_absorpt_coefficient_mu 0.544 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.83 _exptl_absorpt_correction_T_max 0.86 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 29837 _diffrn_reflns_av_R_equivalents 0.0656 _diffrn_reflns_av_sigmaI/netI 0.0518 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5998 _reflns_number_gt 4674 _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^)+(0.0462P)^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 5998 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0550 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.0887 _refine_ls_wR_factor_gt 0.0831 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.986 _refine_ls_shift/su_max 0.004 _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 Mo1 Mo -0.200752(18) 0.11209(2) 0.123642(11) 0.01527(7) Uani 1 1 d . . . O1 O -0.09944(14) 0.22523(19) 0.12945(9) 0.0210(4) Uani 1 1 d . . . O41 O -0.20193(15) 0.07879(19) 0.21073(9) 0.0185(4) Uani 1 1 d . . . O51 O -0.32215(14) 0.23936(18) 0.11568(8) 0.0180(4) Uani 1 1 d . . . N11 N -0.21160(18) 0.0922(2) 0.02137(11) 0.0194(5) Uani 1 1 d . . . N12 N -0.18992(17) -0.0327(2) -0.00210(10) 0.0187(5) Uani 1 1 d . . . N21 N -0.09671(17) -0.0666(2) 0.13840(11) 0.0184(5) Uani 1 1 d . . . N22 N -0.11238(17) -0.1746(2) 0.09607(10) 0.0178(5) Uani 1 1 d . . . N31 N -0.33396(18) -0.0574(2) 0.08729(10) 0.0174(5) Uani 1 1 d . . . N32 N -0.31435(17) -0.1584(2) 0.04703(10) 0.0175(5) Uani 1 1 d . . . C13 C -0.1689(2) -0.0137(3) -0.05866(13) 0.0232(6) Uani 1 1 d . . . C14 C -0.1782(2) 0.1245(3) -0.07236(14) 0.0255(6) Uani 1 1 d . . . H14A H -0.1683 0.1679 -0.1094 0.031 Uiso 1 1 calc R . . C15 C -0.2044(2) 0.1881(3) -0.02197(13) 0.0216(6) Uani 1 1 d . . . C16 C -0.1387(3) -0.1296(3) -0.09534(15) 0.0324(7) Uani 1 1 d . . . H16A H -0.1977 -0.1970 -0.1061 0.049 Uiso 1 1 calc R . . H16B H -0.0724 -0.1737 -0.0692 0.049 Uiso 1 1 calc R . . H16C H -0.1262 -0.0941 -0.1348 0.049 Uiso 1 1 calc R . . C17 C -0.2225(3) 0.3369(3) -0.01283(14) 0.0277(7) Uani 1 1 d . . . H17A H -0.2777 0.3476 0.0100 0.042 Uiso 1 1 calc R . . H17B H -0.2473 0.3820 -0.0547 0.042 Uiso 1 1 calc R . . H17C H -0.1545 0.3791 0.0122 0.042 Uiso 1 1 calc R . . C23 C -0.0383(2) -0.2725(3) 0.11971(13) 0.0195(6) Uani 1 1 d . . . C24 C 0.0271(2) -0.2281(3) 0.17807(13) 0.0200(6) Uani 1 1 d . . . H24A H 0.0869 -0.2757 0.2055 0.024 Uiso 1 1 calc R . . C25 C -0.0117(2) -0.1006(3) 0.18867(13) 0.0195(6) Uani 1 1 d . . . C26 C -0.0319(2) -0.4045(3) 0.08580(15) 0.0288(7) Uani 1 1 d . . . H26A H -0.0413 -0.3861 0.0403 0.043 Uiso 1 1 calc R . . H26B H -0.0892 -0.4667 0.0904 0.043 Uiso 1 1 calc R . . H26C H 0.0391 -0.4472 0.1045 0.043 Uiso 1 1 calc R . . C27 C 0.0297(2) -0.0101(3) 0.24535(13) 0.0251(6) Uani 1 1 d . . . H27A H 0.0328 0.0850 0.2311 0.038 Uiso 1 1 calc R . . H27B H 0.1026 -0.0400 0.2695 0.038 Uiso 1 1 calc R . . H27C H -0.0189 -0.0155 0.2728 0.038 Uiso 1 1 calc R . . C33 C -0.4066(2) -0.2295(3) 0.02015(13) 0.0191(6) Uani 1 1 d . . . C34 C -0.4862(2) -0.1769(3) 0.04366(13) 0.0212(6) Uani 1 1 d . . . H34A H -0.5594 -0.2071 0.0338 0.025 Uiso 1 1 calc R . . C35 C -0.4395(2) -0.0702(3) 0.08496(13) 0.0180(6) Uani 1 1 d . . . C36 C -0.4137(2) -0.3414(3) -0.02780(14) 0.0254(6) Uani 1 1 d . . . H36A H -0.3596 -0.4122 -0.0096 0.038 Uiso 1 1 calc R . . H36B H -0.3997 -0.3032 -0.0664 0.038 Uiso 1 1 calc R . . H36C H -0.4864 -0.3820 -0.0389 0.038 Uiso 1 1 calc R . . C37 C -0.4967(2) 0.0167(3) 0.12193(14) 0.0222(6) Uani 1 1 d . . . H37A H -0.4762 0.1132 0.1195 0.033 Uiso 1 1 calc R . . H37B H -0.4759 -0.0129 0.1668 0.033 Uiso 1 1 calc R . . H37C H -0.5752 0.0069 0.1038 0.033 Uiso 1 1 calc R . . C41 C -0.2748(2) 0.0783(3) 0.24474(12) 0.0177(6) Uani 1 1 d . . . C42 C -0.3363(2) 0.1954(3) 0.24991(12) 0.0172(6) Uani 1 1 d . . . C43 C -0.4069(2) 0.1835(3) 0.28836(13) 0.0228(6) Uani 1 1 d . . . H43A H -0.4494 0.2607 0.2929 0.027 Uiso 1 1 calc R . . C44 C -0.4166(2) 0.0628(3) 0.31988(14) 0.0273(7) Uani 1 1 d . . . H44A H -0.4658 0.0575 0.3452 0.033 Uiso 1 1 calc R . . C45 C -0.3545(3) -0.0501(3) 0.31437(15) 0.0283(7) Uani 1 1 d . . . H45A H -0.3607 -0.1331 0.3360 0.034 Uiso 1 1 calc R . . C46 C -0.2834(2) -0.0420(3) 0.27735(13) 0.0231(6) Uani 1 1 d . . . H46A H -0.2400 -0.1193 0.2741 0.028 Uiso 1 1 calc R . . C51 C -0.3160(2) 0.3469(3) 0.15744(13) 0.0177(6) Uani 1 1 d . . . C52 C -0.3235(2) 0.3300(3) 0.22018(13) 0.0183(6) Uani 1 1 d . . . C53 C -0.3205(2) 0.4481(3) 0.25722(14) 0.0228(6) Uani 1 1 d . . . H53A H -0.3251 0.4387 0.2998 0.027 Uiso 1 1 calc R . . C54 C -0.3109(2) 0.5782(3) 0.23385(14) 0.0254(7) Uani 1 1 d . . . H54A H -0.3092 0.6564 0.2602 0.031 Uiso 1 1 calc R . . C55 C -0.3038(2) 0.5942(3) 0.17215(14) 0.0239(6) Uani 1 1 d . . . H55A H -0.2969 0.6832 0.1558 0.029 Uiso 1 1 calc R . . C56 C -0.3069(2) 0.4795(3) 0.13447(13) 0.0211(6) Uani 1 1 d . . . H56A H -0.3027 0.4908 0.0919 0.025 Uiso 1 1 calc R . . B1 B -0.2038(2) -0.1658(3) 0.03295(15) 0.0194(6) Uani 1 1 d . . . H1A H -0.205(2) -0.254(3) 0.0022(13) 0.023 Uiso 1 1 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 Mo1 0.01373(11) 0.01797(12) 0.01365(12) -0.00061(10) 0.00311(8) 0.00028(10) O1 0.0173(10) 0.0235(11) 0.0217(10) -0.0032(8) 0.0049(8) -0.0022(8) O41 0.0164(9) 0.0242(11) 0.0153(9) 0.0006(7) 0.0051(8) 0.0019(8) O51 0.0155(9) 0.0188(10) 0.0183(10) 0.0010(8) 0.0027(8) 0.0026(8) N11 0.0178(11) 0.0237(13) 0.0162(12) -0.0008(9) 0.0041(9) -0.0010(9) N12 0.0163(11) 0.0248(13) 0.0145(12) -0.0013(9) 0.0034(9) 0.0011(10) N21 0.0150(11) 0.0222(12) 0.0174(12) -0.0026(9) 0.0036(9) 0.0014(9) N22 0.0163(11) 0.0206(12) 0.0162(12) -0.0028(9) 0.0043(9) 0.0017(9) N31 0.0178(11) 0.0204(11) 0.0143(11) -0.0005(9) 0.0051(9) 0.0005(9) N32 0.0171(11) 0.0187(11) 0.0147(11) 0.0001(9) 0.0012(9) 0.0013(9) C13 0.0184(14) 0.0348(17) 0.0165(14) -0.0042(12) 0.0048(11) -0.0040(12) C14 0.0269(15) 0.0322(17) 0.0184(14) 0.0006(12) 0.0079(12) -0.0083(13) C15 0.0203(14) 0.0256(16) 0.0177(14) 0.0013(12) 0.0032(11) -0.0068(12) C16 0.0379(18) 0.039(2) 0.0254(17) -0.0044(14) 0.0176(14) -0.0034(15) C17 0.0351(17) 0.0247(16) 0.0231(16) 0.0002(12) 0.0077(13) -0.0075(14) C23 0.0185(13) 0.0187(14) 0.0221(15) 0.0020(11) 0.0071(11) -0.0002(11) C24 0.0167(13) 0.0213(15) 0.0210(15) 0.0031(11) 0.0036(11) 0.0025(11) C25 0.0137(12) 0.0260(15) 0.0190(14) 0.0003(12) 0.0048(11) 0.0008(11) C26 0.0259(15) 0.0230(16) 0.0341(17) -0.0036(13) 0.0031(13) 0.0045(13) C27 0.0184(14) 0.0318(17) 0.0204(15) -0.0042(12) -0.0024(12) 0.0039(12) C33 0.0182(13) 0.0187(14) 0.0174(14) 0.0031(11) 0.0003(11) -0.0009(11) C34 0.0160(13) 0.0243(15) 0.0202(15) 0.0031(12) 0.0000(11) -0.0027(12) C35 0.0161(13) 0.0189(14) 0.0166(14) 0.0053(11) 0.0010(11) 0.0003(11) C36 0.0217(14) 0.0271(16) 0.0231(16) -0.0036(12) -0.0005(12) -0.0008(12) C37 0.0172(13) 0.0257(15) 0.0247(15) 0.0003(12) 0.0074(12) 0.0003(12) C41 0.0167(13) 0.0211(15) 0.0132(13) -0.0016(10) 0.0008(11) -0.0030(11) C42 0.0175(13) 0.0198(14) 0.0127(13) 0.0001(10) 0.0015(10) 0.0001(11) C43 0.0211(14) 0.0272(16) 0.0200(15) -0.0018(12) 0.0059(12) 0.0024(12) C44 0.0233(15) 0.0363(17) 0.0246(16) 0.0061(13) 0.0106(13) -0.0041(13) C45 0.0325(17) 0.0254(16) 0.0274(16) 0.0086(13) 0.0092(14) -0.0012(13) C46 0.0264(15) 0.0190(15) 0.0226(15) 0.0003(12) 0.0047(12) -0.0005(12) C51 0.0121(12) 0.0216(14) 0.0173(14) -0.0005(11) 0.0006(10) 0.0017(10) C52 0.0147(13) 0.0194(14) 0.0198(14) 0.0003(11) 0.0031(11) 0.0014(11) C53 0.0206(14) 0.0263(15) 0.0203(15) 0.0008(12) 0.0035(12) 0.0042(12) C54 0.0265(15) 0.0215(16) 0.0268(16) -0.0030(12) 0.0052(13) 0.0015(12) C55 0.0237(14) 0.0167(15) 0.0280(16) 0.0041(12) 0.0022(12) 0.0008(12) C56 0.0183(14) 0.0252(15) 0.0183(14) 0.0048(11) 0.0025(11) 0.0006(12) B1 0.0183(15) 0.0215(16) 0.0176(16) -0.0021(13) 0.0037(13) 0.0007(13) _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 Mo1 O1 1.6822(18) . ? Mo1 O41 1.9281(18) . ? Mo1 O51 1.9608(18) . ? Mo1 N21 2.162(2) . ? Mo1 N11 2.200(2) . ? Mo1 N31 2.348(2) . ? O41 C41 1.347(3) . ? O51 C51 1.374(3) . ? N11 C15 1.349(3) . ? N11 N12 1.377(3) . ? N12 C13 1.346(3) . ? N12 B1 1.540(4) . ? N21 C25 1.352(3) . ? N21 N22 1.375(3) . ? N22 C23 1.343(3) . ? N22 B1 1.538(4) . ? N31 C35 1.349(3) . ? N31 N32 1.386(3) . ? N32 C33 1.355(3) . ? N32 B1 1.537(4) . ? C13 C14 1.375(4) . ? C13 C16 1.495(4) . ? C14 C15 1.382(4) . ? C15 C17 1.489(4) . ? C23 C24 1.381(4) . ? C23 C26 1.496(4) . ? C24 C25 1.380(4) . ? C25 C27 1.488(4) . ? C33 C34 1.366(4) . ? C33 C36 1.494(4) . ? C34 C35 1.393(4) . ? C35 C37 1.495(4) . ? C41 C46 1.390(4) . ? C41 C42 1.410(4) . ? C42 C43 1.401(4) . ? C42 C52 1.491(4) . ? C43 C44 1.384(4) . ? C44 C45 1.383(4) . ? C45 C46 1.380(4) . ? C51 C56 1.401(4) . ? C51 C52 1.406(4) . ? C52 C53 1.398(4) . ? C53 C54 1.383(4) . ? C54 C55 1.381(4) . ? C55 C56 1.379(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mo1 O41 104.85(8) . . ? O1 Mo1 O51 99.94(8) . . ? O41 Mo1 O51 88.09(8) . . ? O1 Mo1 N21 94.73(9) . . ? O41 Mo1 N21 83.94(8) . . ? O51 Mo1 N21 164.70(8) . . ? O1 Mo1 N11 87.75(9) . . ? O41 Mo1 N11 164.76(8) . . ? O51 Mo1 N11 98.28(8) . . ? N21 Mo1 N11 86.55(8) . . ? O1 Mo1 N31 163.79(8) . . ? O41 Mo1 N31 90.38(8) . . ? O51 Mo1 N31 85.86(8) . . ? N21 Mo1 N31 81.17(8) . . ? N11 Mo1 N31 76.38(8) . . ? C41 O41 Mo1 137.76(17) . . ? C51 O51 Mo1 121.78(15) . . ? C15 N11 N12 106.9(2) . . ? C15 N11 Mo1 130.54(19) . . ? N12 N11 Mo1 119.45(16) . . ? C13 N12 N11 109.4(2) . . ? C13 N12 B1 130.6(2) . . ? N11 N12 B1 119.7(2) . . ? C25 N21 N22 106.7(2) . . ? C25 N21 Mo1 129.95(18) . . ? N22 N21 Mo1 123.21(16) . . ? C23 N22 N21 109.3(2) . . ? C23 N22 B1 131.5(2) . . ? N21 N22 B1 119.2(2) . . ? C35 N31 N32 105.7(2) . . ? C35 N31 Mo1 135.04(18) . . ? N32 N31 Mo1 117.78(15) . . ? C33 N32 N31 110.0(2) . . ? C33 N32 B1 129.4(2) . . ? N31 N32 B1 120.2(2) . . ? N12 C13 C14 107.8(2) . . ? N12 C13 C16 122.3(3) . . ? C14 C13 C16 129.9(3) . . ? C13 C14 C15 106.9(3) . . ? N11 C15 C14 109.0(3) . . ? N11 C15 C17 122.4(2) . . ? C14 C15 C17 128.6(3) . . ? N22 C23 C24 108.2(2) . . ? N22 C23 C26 123.5(3) . . ? C24 C23 C26 128.3(3) . . ? C25 C24 C23 106.3(2) . . ? N21 C25 C24 109.4(2) . . ? N21 C25 C27 123.1(2) . . ? C24 C25 C27 127.5(3) . . ? N32 C33 C34 107.7(2) . . ? N32 C33 C36 123.2(2) . . ? C34 C33 C36 129.1(3) . . ? C33 C34 C35 106.8(2) . . ? N31 C35 C34 109.8(2) . . ? N31 C35 C37 124.6(2) . . ? C34 C35 C37 125.6(2) . . ? O41 C41 C46 116.8(2) . . ? O41 C41 C42 122.2(2) . . ? C46 C41 C42 120.9(2) . . ? C43 C42 C41 116.9(2) . . ? C43 C42 C52 120.1(2) . . ? C41 C42 C52 122.9(2) . . ? C44 C43 C42 122.0(3) . . ? C45 C44 C43 119.7(3) . . ? C46 C45 C44 119.9(3) . . ? C45 C46 C41 120.5(3) . . ? O51 C51 C56 117.4(2) . . ? O51 C51 C52 123.1(2) . . ? C56 C51 C52 119.4(2) . . ? C53 C52 C51 117.7(3) . . ? C53 C52 C42 117.4(2) . . ? C51 C52 C42 124.8(2) . . ? C54 C53 C52 122.1(3) . . ? C55 C54 C53 119.9(3) . . ? C56 C55 C54 119.3(3) . . ? C55 C56 C51 121.6(3) . . ? N32 B1 N22 109.9(2) . . ? N32 B1 N12 107.6(2) . . ? N22 B1 N12 108.9(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.752 _refine_diff_density_min -0.430 _refine_diff_density_rms 0.087 #=END data_kilns _database_code_CSD 199481 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H30 B N6 O3 W' _chemical_formula_weight 681.23 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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.410(3) _cell_length_b 10.0634(18) _cell_length_c 17.134(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.629(11) _cell_angle_gamma 90.00 _cell_volume 2558.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(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 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.768 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1348 _exptl_absorpt_coefficient_mu 4.557 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.39 _exptl_absorpt_correction_T_max 0.24 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 17426 _diffrn_reflns_av_R_equivalents 0.0624 _diffrn_reflns_av_sigmaI/netI 0.0722 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5852 _reflns_number_gt 4651 _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^)+(0.0574P)^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 5852 _refine_ls_number_parameters 347 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0612 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.1088 _refine_ls_wR_factor_gt 0.1014 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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 0.776205(14) -0.08103(2) 0.405035(14) 0.01043(9) Uani 1 1 d . . . O1 O 0.7975(3) -0.1819(4) 0.3316(3) 0.0151(9) Uani 1 1 d . . . O41 O 0.7147(3) 0.0731(4) 0.3467(3) 0.0143(9) Uani 1 1 d . . . O51 O 0.8875(3) 0.0260(4) 0.4332(2) 0.0124(8) Uani 1 1 d . . . N11 N 0.8206(3) -0.2354(5) 0.4928(3) 0.0118(10) Uani 1 1 d . . . N12 N 0.7669(3) -0.2855(5) 0.5400(3) 0.0114(10) Uiso 1 1 d . . . N21 N 0.6417(3) -0.1604(5) 0.3882(3) 0.0129(10) Uani 1 1 d . . . N22 N 0.6137(3) -0.2211(5) 0.4489(3) 0.0133(10) Uani 1 1 d . . . N31 N 0.7461(3) 0.0060(5) 0.5237(3) 0.0108(10) Uani 1 1 d . . . N32 N 0.6958(3) -0.0726(5) 0.5617(3) 0.0144(10) Uani 1 1 d . . . C13 C 0.8109(4) -0.3850(6) 0.5867(4) 0.0116(12) Uani 1 1 d . . . C14 C 0.8919(4) -0.4045(6) 0.5676(4) 0.0154(13) Uani 1 1 d . . . H14A H 0.9354 -0.4680 0.5896 0.018 Uiso 1 1 calc R . . C15 C 0.8952(4) -0.3121(6) 0.5103(3) 0.0104(11) Uani 1 1 d . . . C16 C 0.7732(5) -0.4557(6) 0.6469(4) 0.0201(14) Uani 1 1 d . . . H16A H 0.7156 -0.4929 0.6199 0.030 Uiso 1 1 calc R . . H16B H 0.7663 -0.3940 0.6876 0.030 Uiso 1 1 calc R . . H16C H 0.8135 -0.5256 0.6720 0.030 Uiso 1 1 calc R . . C17 C 0.9685(4) -0.2914(6) 0.4689(4) 0.0156(13) Uani 1 1 d . . . H17A H 0.9855 -0.1994 0.4724 0.023 Uiso 1 1 calc R . . H17B H 0.9470 -0.3168 0.4130 0.023 Uiso 1 1 calc R . . H17C H 1.0197 -0.3448 0.4949 0.023 Uiso 1 1 calc R . . C23 C 0.5284(4) -0.2615(6) 0.4199(4) 0.0149(12) Uani 1 1 d . . . C24 C 0.5007(4) -0.2316(6) 0.3380(4) 0.0177(13) Uani 1 1 d . . . H24A H 0.4451 -0.2511 0.3022 0.021 Uiso 1 1 calc R . . C25 C 0.5724(4) -0.1668(6) 0.3203(4) 0.0149(12) Uani 1 1 d . . . C26 C 0.4743(4) -0.3219(7) 0.4713(4) 0.0242(15) Uani 1 1 d . . . H26A H 0.5129 -0.3753 0.5130 0.036 Uiso 1 1 calc R . . H26B H 0.4277 -0.3766 0.4383 0.036 Uiso 1 1 calc R . . H26C H 0.4477 -0.2527 0.4958 0.036 Uiso 1 1 calc R . . C27 C 0.5765(4) -0.1064(6) 0.2416(4) 0.0170(13) Uani 1 1 d . . . H27A H 0.6363 -0.1162 0.2354 0.026 Uiso 1 1 calc R . . H27B H 0.5616 -0.0138 0.2412 0.026 Uiso 1 1 calc R . . H27C H 0.5344 -0.1506 0.1977 0.026 Uiso 1 1 calc R . . C33 C 0.6799(4) -0.0067(6) 0.6255(4) 0.0141(12) Uani 1 1 d . . . C34 C 0.7217(4) 0.1166(6) 0.6299(4) 0.0140(12) Uani 1 1 d . . . H34A H 0.7220 0.1833 0.6676 0.017 Uiso 1 1 calc R . . C35 C 0.7631(4) 0.1204(6) 0.5668(4) 0.0125(12) Uani 1 1 d . . . C36 C 0.6281(5) -0.0662(6) 0.6786(4) 0.0208(14) Uani 1 1 d . . . H36A H 0.5727 -0.1027 0.6457 0.031 Uiso 1 1 calc R . . H36B H 0.6150 0.0012 0.7134 0.031 Uiso 1 1 calc R . . H36C H 0.6631 -0.1353 0.7109 0.031 Uiso 1 1 calc R . . C37 C 0.8190(4) 0.2309(6) 0.5488(4) 0.0155(12) Uani 1 1 d . . . H37A H 0.8496 0.2015 0.5100 0.023 Uiso 1 1 calc R . . H37B H 0.8624 0.2575 0.5977 0.023 Uiso 1 1 calc R . . H37C H 0.7809 0.3049 0.5270 0.023 Uiso 1 1 calc R . . C41 C 0.7272(4) 0.2068(6) 0.3578(4) 0.0134(12) Uani 1 1 d . . . C42 C 0.8053(4) 0.2711(6) 0.3507(4) 0.0150(12) Uani 1 1 d . . . C43 C 0.8103(4) 0.4082(6) 0.3592(4) 0.0172(13) Uani 1 1 d . . . H43A H 0.8616 0.4520 0.3539 0.021 Uiso 1 1 calc R . . C44 C 0.7406(4) 0.4825(7) 0.3757(4) 0.0204(14) Uani 1 1 d . . . H44A H 0.7459 0.5741 0.3826 0.024 Uiso 1 1 calc R . . C45 C 0.6625(4) 0.4168(6) 0.3815(4) 0.0195(13) Uani 1 1 d . . . H45A H 0.6151 0.4640 0.3922 0.023 Uiso 1 1 calc R . . C46 C 0.6569(4) 0.2800(6) 0.3711(4) 0.0166(13) Uani 1 1 d . . . H46A H 0.6043 0.2365 0.3731 0.020 Uiso 1 1 calc R . . C51 C 0.9220(4) 0.0860(6) 0.3759(4) 0.0138(12) Uani 1 1 d . . . C52 C 0.8842(4) 0.1987(6) 0.3337(4) 0.0123(12) Uani 1 1 d . . . C53 C 0.9268(4) 0.2556(6) 0.2795(4) 0.0171(12) Uani 1 1 d . . . H53A H 0.9016 0.3306 0.2504 0.021 Uiso 1 1 calc R . . C54 C 1.0058(4) 0.2034(6) 0.2679(4) 0.0173(13) Uani 1 1 d . . . H54A H 1.0321 0.2419 0.2305 0.021 Uiso 1 1 calc R . . C55 C 1.0451(4) 0.0939(6) 0.3121(4) 0.0187(13) Uani 1 1 d . . . H55A H 1.0992 0.0603 0.3062 0.022 Uiso 1 1 calc R . . C56 C 1.0034(4) 0.0346(6) 0.3652(4) 0.0178(13) Uani 1 1 d . . . H56A H 1.0292 -0.0402 0.3943 0.021 Uiso 1 1 calc R . . B1 B 0.6765(4) -0.2181(7) 0.5364(4) 0.0152(14) Uani 1 1 d . . . H1A H 0.650(4) -0.276(6) 0.576(4) 0.018 Uiso 1 1 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 0.00741(13) 0.01025(13) 0.01651(14) -0.00005(10) 0.00818(9) -0.00063(9) O1 0.013(2) 0.013(2) 0.021(2) -0.0013(17) 0.0077(18) -0.0004(17) O41 0.010(2) 0.014(2) 0.020(2) 0.0030(18) 0.0057(17) -0.0012(17) O51 0.0073(19) 0.015(2) 0.019(2) 0.0012(17) 0.0100(17) 0.0017(16) N11 0.011(2) 0.011(2) 0.016(2) 0.002(2) 0.009(2) 0.000(2) N21 0.008(2) 0.013(3) 0.021(3) 0.000(2) 0.010(2) -0.0027(19) N22 0.010(2) 0.014(3) 0.019(3) -0.001(2) 0.009(2) -0.0004(19) N31 0.011(2) 0.007(2) 0.018(3) 0.0018(19) 0.010(2) -0.0013(19) N32 0.015(2) 0.012(3) 0.021(3) 0.002(2) 0.013(2) -0.004(2) C13 0.010(3) 0.010(3) 0.018(3) -0.002(2) 0.010(2) -0.004(2) C14 0.008(3) 0.009(3) 0.033(4) 0.003(3) 0.012(3) 0.006(2) C15 0.009(3) 0.009(3) 0.016(3) -0.001(2) 0.009(2) -0.001(2) C16 0.024(3) 0.019(3) 0.022(3) 0.008(3) 0.014(3) 0.005(3) C17 0.010(3) 0.018(3) 0.024(3) 0.001(2) 0.013(3) 0.001(2) C23 0.008(3) 0.013(3) 0.027(3) 0.001(3) 0.010(2) -0.002(2) C24 0.011(3) 0.014(3) 0.026(3) -0.005(3) 0.004(3) -0.002(2) C25 0.014(3) 0.013(3) 0.019(3) -0.005(2) 0.006(3) 0.000(2) C26 0.014(3) 0.029(4) 0.033(4) 0.009(3) 0.013(3) -0.003(3) C27 0.016(3) 0.019(3) 0.017(3) -0.001(2) 0.007(3) 0.000(2) C33 0.011(3) 0.012(3) 0.022(3) 0.000(2) 0.011(2) 0.001(2) C34 0.010(3) 0.015(3) 0.021(3) -0.002(2) 0.011(2) 0.000(2) C35 0.009(3) 0.010(3) 0.020(3) 0.002(2) 0.004(2) 0.005(2) C36 0.025(3) 0.020(3) 0.027(3) -0.001(3) 0.023(3) 0.000(3) C37 0.013(3) 0.015(3) 0.020(3) 0.000(2) 0.006(2) -0.001(2) C41 0.012(3) 0.012(3) 0.019(3) 0.003(2) 0.009(2) 0.003(2) C42 0.010(3) 0.012(3) 0.021(3) -0.003(2) 0.000(2) 0.001(2) C43 0.019(3) 0.011(3) 0.022(3) 0.002(2) 0.006(3) 0.001(2) C44 0.020(3) 0.013(3) 0.026(3) -0.004(3) 0.004(3) 0.005(3) C45 0.013(3) 0.023(3) 0.023(3) 0.000(3) 0.006(3) 0.002(3) C46 0.009(3) 0.024(3) 0.016(3) 0.005(3) 0.002(2) 0.000(2) C51 0.011(3) 0.012(3) 0.020(3) -0.003(2) 0.008(2) -0.002(2) C52 0.009(3) 0.012(3) 0.020(3) -0.001(2) 0.010(2) -0.002(2) C53 0.020(3) 0.013(3) 0.022(3) -0.001(3) 0.012(3) -0.002(3) C54 0.017(3) 0.019(3) 0.021(3) 0.001(2) 0.013(3) -0.002(2) C55 0.014(3) 0.018(3) 0.027(3) -0.004(3) 0.011(3) -0.001(3) C56 0.017(3) 0.013(3) 0.027(3) 0.000(3) 0.013(3) 0.003(2) B1 0.011(3) 0.012(3) 0.023(4) -0.001(3) 0.005(3) -0.001(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 O1 1.716(4) . ? W1 O41 1.948(4) . ? W1 O51 1.972(4) . ? W1 N11 2.142(5) . ? W1 N21 2.168(5) . ? W1 N31 2.372(5) . ? O41 C41 1.365(7) . ? O51 C51 1.375(7) . ? N11 C15 1.351(7) . ? N11 N12 1.396(6) . ? N12 C13 1.346(7) . ? N12 B1 1.536(8) . ? N21 C25 1.353(8) . ? N21 N22 1.371(6) . ? N22 C23 1.336(7) . ? N22 B1 1.551(9) . ? N31 C35 1.355(8) . ? N31 N32 1.386(6) . ? N32 C33 1.357(8) . ? N32 B1 1.533(8) . ? C13 C14 1.387(7) . ? C13 C16 1.493(8) . ? C14 C15 1.363(8) . ? C15 C17 1.500(7) . ? C23 C24 1.386(9) . ? C23 C26 1.495(8) . ? C24 C25 1.385(8) . ? C25 C27 1.496(8) . ? C33 C34 1.390(8) . ? C33 C36 1.488(8) . ? C34 C35 1.398(8) . ? C35 C37 1.488(8) . ? C41 C46 1.380(8) . ? C41 C42 1.401(8) . ? C42 C43 1.387(8) . ? C42 C52 1.510(8) . ? C43 C44 1.399(8) . ? C44 C45 1.400(9) . ? C45 C46 1.388(9) . ? C51 C52 1.386(8) . ? C51 C56 1.413(8) . ? C52 C53 1.397(8) . ? C53 C54 1.389(8) . ? C54 C55 1.381(9) . ? C55 C56 1.384(9) . ? 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 104.90(19) . . ? O1 W1 O51 100.20(17) . . ? O41 W1 O51 87.78(17) . . ? O1 W1 N11 89.91(19) . . ? O41 W1 N11 163.17(17) . . ? O51 W1 N11 97.60(17) . . ? O1 W1 N21 92.86(19) . . ? O41 W1 N21 84.82(18) . . ? O51 W1 N21 166.29(17) . . ? N11 W1 N21 86.50(18) . . ? O1 W1 N31 165.34(18) . . ? O41 W1 N31 88.04(17) . . ? O51 W1 N31 86.94(16) . . ? N11 W1 N31 76.39(17) . . ? N21 W1 N31 81.30(17) . . ? C41 O41 W1 133.0(4) . . ? C51 O51 W1 122.9(4) . . ? C15 N11 N12 105.5(4) . . ? C15 N11 W1 131.4(4) . . ? N12 N11 W1 122.8(3) . . ? C13 N12 N11 109.4(4) . . ? C13 N12 B1 131.1(5) . . ? N11 N12 B1 119.3(5) . . ? C25 N21 N22 107.1(4) . . ? C25 N21 W1 129.6(4) . . ? N22 N21 W1 123.3(4) . . ? C23 N22 N21 109.4(5) . . ? C23 N22 B1 131.3(5) . . ? N21 N22 B1 118.8(5) . . ? C35 N31 N32 106.3(5) . . ? C35 N31 W1 136.6(4) . . ? N32 N31 W1 117.1(3) . . ? C33 N32 N31 110.2(5) . . ? C33 N32 B1 129.1(5) . . ? N31 N32 B1 120.2(5) . . ? N12 C13 C14 107.7(5) . . ? N12 C13 C16 122.6(5) . . ? C14 C13 C16 129.7(6) . . ? C15 C14 C13 106.6(5) . . ? N11 C15 C14 110.7(5) . . ? N11 C15 C17 121.4(5) . . ? C14 C15 C17 127.9(5) . . ? N22 C23 C24 108.3(5) . . ? N22 C23 C26 123.6(6) . . ? C24 C23 C26 128.0(5) . . ? C25 C24 C23 106.1(5) . . ? N21 C25 C24 109.0(5) . . ? N21 C25 C27 122.7(5) . . ? C24 C25 C27 128.3(6) . . ? N32 C33 C34 107.4(5) . . ? N32 C33 C36 122.6(5) . . ? C34 C33 C36 130.0(6) . . ? C33 C34 C35 106.5(5) . . ? N31 C35 C34 109.7(5) . . ? N31 C35 C37 124.0(5) . . ? C34 C35 C37 126.3(5) . . ? O41 C41 C46 117.5(5) . . ? O41 C41 C42 122.4(5) . . ? C46 C41 C42 120.0(5) . . ? C43 C42 C41 118.4(5) . . ? C43 C42 C52 118.4(5) . . ? C41 C42 C52 123.2(5) . . ? C42 C43 C44 121.9(6) . . ? C43 C44 C45 118.9(6) . . ? C46 C45 C44 119.0(6) . . ? C41 C46 C45 121.8(6) . . ? O51 C51 C52 122.8(5) . . ? O51 C51 C56 117.3(5) . . ? C52 C51 C56 119.7(5) . . ? C51 C52 C53 118.4(5) . . ? C51 C52 C42 122.8(5) . . ? C53 C52 C42 118.4(5) . . ? C54 C53 C52 121.8(6) . . ? C55 C54 C53 119.7(6) . . ? C54 C55 C56 119.5(6) . . ? C55 C56 C51 120.9(6) . . ? N32 B1 N12 107.8(5) . . ? N32 B1 N22 108.4(5) . . ? N12 B1 N22 110.7(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.809 _refine_diff_density_min -2.785 _refine_diff_density_rms 0.210 #=END data_engls _database_code_CSD 199482 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H14 Cl2 N2 O Ru0.50' _chemical_formula_weight 383.74 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' Ru Ru -1.2594 0.8363 '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' _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 13.467(5) _cell_length_b 15.593(6) _cell_length_c 15.861(6) _cell_angle_alpha 90.00 _cell_angle_beta 98.310(7) _cell_angle_gamma 90.00 _cell_volume 3296(2) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 0.838 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.66 _exptl_absorpt_correction_T_max 0.76 _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 17252 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3779 _reflns_number_gt 3137 _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^)+(0.0578P)^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 3779 _refine_ls_number_parameters 214 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.0983 _refine_ls_wR_factor_gt 0.0955 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 Ru1 Ru 0.0000 -0.360780(18) -0.2500 0.02156(10) Uani 1 2 d S . . O31 O 0.10903(13) -0.26556(11) -0.23727(11) 0.0273(4) Uani 1 1 d . . . N11 N -0.10756(15) -0.44974(13) -0.28199(13) 0.0242(4) Uani 1 1 d . . . N21 N -0.00625(16) -0.36398(13) -0.37903(13) 0.0246(4) Uani 1 1 d . . . C12 C -0.13362(19) -0.46613(16) -0.36682(16) 0.0265(5) Uani 1 1 d . . . C13 C -0.2076(2) -0.52632(18) -0.39542(19) 0.0354(6) Uani 1 1 d . . . H13A H -0.2240 -0.5377 -0.4546 0.043 Uiso 1 1 calc R . . C14 C -0.2570(2) -0.56931(19) -0.3378(2) 0.0410(7) Uani 1 1 d . . . H14A H -0.3075 -0.6103 -0.3567 0.049 Uiso 1 1 calc R . . C15 C -0.2316(2) -0.5516(2) -0.2519(2) 0.0407(7) Uani 1 1 d . . . H15A H -0.2646 -0.5801 -0.2109 0.049 Uiso 1 1 calc R . . C16 C -0.1581(2) -0.49229(18) -0.22701(18) 0.0338(6) Uani 1 1 d . . . H16A H -0.1416 -0.4804 -0.1679 0.041 Uiso 1 1 calc R . . C22 C -0.07707(19) -0.41611(17) -0.42230(16) 0.0266(5) Uani 1 1 d . . . C23 C -0.0934(2) -0.4185(2) -0.51040(17) 0.0374(7) Uani 1 1 d . . . H23A H -0.1439 -0.4547 -0.5395 0.045 Uiso 1 1 calc R . . C24 C -0.0360(3) -0.3680(2) -0.55555(19) 0.0458(8) Uani 1 1 d . . . H24A H -0.0459 -0.3693 -0.6161 0.055 Uiso 1 1 calc R . . C25 C 0.0363(2) -0.3154(2) -0.5118(2) 0.0429(8) Uani 1 1 d . . . H25A H 0.0767 -0.2802 -0.5419 0.051 Uiso 1 1 calc R . . C26 C 0.0491(2) -0.31440(18) -0.42455(18) 0.0335(6) Uani 1 1 d . . . H26A H 0.0986 -0.2776 -0.3950 0.040 Uiso 1 1 calc R . . C31 C 0.09849(18) -0.20149(16) -0.18312(17) 0.0268(5) Uani 1 1 d . . . C32 C 0.0315(2) -0.13314(17) -0.20729(19) 0.0319(6) Uani 1 1 d . . . C33 C 0.0279(2) -0.06438(19) -0.1512(2) 0.0422(7) Uani 1 1 d . . . H33A H -0.0156 -0.0174 -0.1678 0.051 Uiso 1 1 calc R . . C34 C 0.0864(2) -0.0634(2) -0.0718(2) 0.0485(8) Uani 1 1 d . . . H34A H 0.0825 -0.0165 -0.0342 0.058 Uiso 1 1 calc R . . C35 C 0.1505(2) -0.1309(2) -0.0474(2) 0.0423(7) Uani 1 1 d . . . H35A H 0.1897 -0.1310 0.0074 0.051 Uiso 1 1 calc R . . C36 C 0.1576(2) -0.19855(18) -0.10307(18) 0.0329(6) Uani 1 1 d . . . H36A H 0.2035 -0.2438 -0.0864 0.039 Uiso 1 1 calc R . . C100 C -0.1757(3) -0.7995(4) -0.2703(3) 0.0843(15) Uani 1 1 d . . . Cl1 Cl -0.11515(13) -0.84530(11) -0.17751(12) 0.0747(6) Uani 0.658(3) 1 d P A 1 Cl1' Cl -0.0964(3) -0.7415(3) -0.2532(3) 0.1071(19) Uani 0.342(3) 1 d P A 2 Cl2 Cl -0.17813(11) -0.85101(8) -0.36986(10) 0.0919(4) Uani 1 1 d . A . 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 Ru1 0.02089(15) 0.02388(16) 0.01954(16) 0.000 0.00166(10) 0.000 O31 0.0211(9) 0.0271(9) 0.0334(10) -0.0021(8) 0.0025(7) -0.0017(7) N11 0.0250(11) 0.0234(10) 0.0238(11) 0.0009(8) 0.0021(9) 0.0010(9) N21 0.0248(11) 0.0262(10) 0.0228(10) 0.0013(9) 0.0035(8) 0.0026(9) C12 0.0241(13) 0.0272(13) 0.0269(13) -0.0011(10) -0.0011(10) 0.0043(10) C13 0.0329(15) 0.0355(15) 0.0353(15) -0.0076(12) -0.0038(12) 0.0002(12) C14 0.0330(16) 0.0327(15) 0.056(2) -0.0037(14) 0.0017(14) -0.0085(13) C15 0.0407(17) 0.0372(16) 0.0449(18) 0.0065(14) 0.0082(14) -0.0091(13) C16 0.0356(15) 0.0349(15) 0.0314(15) 0.0042(12) 0.0060(12) -0.0035(12) C22 0.0248(12) 0.0307(13) 0.0236(13) -0.0022(11) 0.0005(10) 0.0057(11) C23 0.0385(16) 0.0471(17) 0.0252(14) -0.0038(13) -0.0003(12) 0.0007(14) C24 0.0522(19) 0.065(2) 0.0197(14) 0.0007(14) 0.0040(13) 0.0035(17) C25 0.0474(19) 0.0500(19) 0.0337(16) 0.0106(14) 0.0140(14) -0.0011(15) C26 0.0348(15) 0.0375(15) 0.0291(14) 0.0043(12) 0.0077(12) -0.0014(12) C31 0.0204(12) 0.0263(13) 0.0341(14) -0.0002(11) 0.0048(11) -0.0054(10) C32 0.0219(12) 0.0292(14) 0.0436(17) -0.0030(12) 0.0013(12) -0.0038(11) C33 0.0285(15) 0.0339(15) 0.063(2) -0.0128(15) 0.0003(14) -0.0001(12) C34 0.0382(17) 0.0476(19) 0.059(2) -0.0269(16) 0.0041(15) -0.0056(15) C35 0.0353(16) 0.0508(19) 0.0388(17) -0.0102(14) -0.0011(13) -0.0110(15) C36 0.0274(14) 0.0317(14) 0.0383(16) -0.0003(12) 0.0001(12) -0.0047(11) C100 0.049(2) 0.135(5) 0.071(3) 0.007(3) 0.015(2) 0.004(3) Cl1 0.0639(10) 0.0792(12) 0.0775(12) -0.0061(9) -0.0011(8) 0.0184(8) Cl1' 0.054(2) 0.121(3) 0.144(4) -0.083(3) 0.006(2) -0.0009(19) Cl2 0.0916(9) 0.0908(9) 0.1060(10) -0.0127(7) 0.0574(8) -0.0218(7) _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 Ru1 N11 2.017(2) . ? Ru1 N11 2.017(2) 6 ? Ru1 N21 2.037(2) 6 ? Ru1 N21 2.037(2) . ? Ru1 O31 2.0774(18) . ? Ru1 O31 2.0774(18) 6 ? O31 C31 1.338(3) . ? N11 C16 1.355(3) . ? N11 C12 1.365(3) . ? N21 C26 1.353(3) . ? N21 C22 1.361(3) . ? C12 C13 1.396(4) . ? C12 C22 1.469(4) . ? C13 C14 1.379(4) . ? C14 C15 1.383(4) . ? C15 C16 1.371(4) . ? C22 C23 1.383(4) . ? C23 C24 1.375(4) . ? C24 C25 1.381(5) . ? C25 C26 1.369(4) . ? C31 C36 1.398(4) . ? C31 C32 1.413(4) . ? C32 C33 1.399(4) . ? C32 C32 1.490(6) 6 ? C33 C34 1.386(5) . ? C34 C35 1.379(5) . ? C35 C36 1.388(4) . ? C100 Cl1' 1.396(6) . ? C100 Cl1 1.731(5) . ? C100 Cl2 1.767(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 N11 Ru1 N11 93.09(12) . 6 ? N11 Ru1 N21 99.20(8) . 6 ? N11 Ru1 N21 78.84(8) 6 6 ? N11 Ru1 N21 78.84(8) . . ? N11 Ru1 N21 99.20(8) 6 . ? N21 Ru1 N21 177.19(11) 6 . ? N11 Ru1 O31 171.08(7) . . ? N11 Ru1 O31 89.73(8) 6 . ? N21 Ru1 O31 89.65(8) 6 . ? N21 Ru1 O31 92.36(8) . . ? N11 Ru1 O31 89.73(8) . 6 ? N11 Ru1 O31 171.08(7) 6 6 ? N21 Ru1 O31 92.36(8) 6 6 ? N21 Ru1 O31 89.65(8) . 6 ? O31 Ru1 O31 88.76(10) . 6 ? C31 O31 Ru1 117.19(15) . . ? C16 N11 C12 117.5(2) . . ? C16 N11 Ru1 125.74(18) . . ? C12 N11 Ru1 116.74(17) . . ? C26 N21 C22 118.2(2) . . ? C26 N21 Ru1 125.18(18) . . ? C22 N21 Ru1 116.46(17) . . ? N11 C12 C13 121.1(2) . . ? N11 C12 C22 114.2(2) . . ? C13 C12 C22 124.7(2) . . ? C14 C13 C12 120.1(3) . . ? C13 C14 C15 118.7(3) . . ? C16 C15 C14 119.0(3) . . ? N11 C16 C15 123.6(3) . . ? N21 C22 C23 121.5(2) . . ? N21 C22 C12 113.7(2) . . ? C23 C22 C12 124.8(2) . . ? C24 C23 C22 119.4(3) . . ? C23 C24 C25 119.1(3) . . ? C26 C25 C24 119.5(3) . . ? N21 C26 C25 122.2(3) . . ? O31 C31 C36 120.5(2) . . ? O31 C31 C32 120.8(2) . . ? C36 C31 C32 118.6(2) . . ? C33 C32 C31 119.0(3) . . ? C33 C32 C32 120.7(2) . 6 ? C31 C32 C32 120.2(2) . 6 ? C34 C33 C32 121.3(3) . . ? C35 C34 C33 119.8(3) . . ? C34 C35 C36 120.0(3) . . ? C35 C36 C31 121.3(3) . . ? Cl1' C100 Cl1 81.3(3) . . ? Cl1' C100 Cl2 112.5(3) . . ? Cl1 C100 Cl2 121.2(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.000 _refine_diff_density_min -0.638 _refine_diff_density_rms 0.080 #=END data_jollys _database_code_CSD 199483 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H24 O6 W' _chemical_formula_weight 736.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 16.8678(12) _cell_length_b 17.776(2) _cell_length_c 19.036(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5707.8(10) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.714 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2896 _exptl_absorpt_coefficient_mu 4.096 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.31 _exptl_absorpt_correction_T_max 0.82 _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 23560 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_sigmaI/netI 0.0234 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 22.48 _reflns_number_total 3727 _reflns_number_gt 2597 _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^)+(0.0239P)^2^+4.7811P] 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 3727 _refine_ls_number_parameters 389 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0396 _refine_ls_R_factor_gt 0.0207 _refine_ls_wR_factor_ref 0.0515 _refine_ls_wR_factor_gt 0.0445 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _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 0.2500 0.2500 0.379300(12) 0.02518(9) Uani 1 2 d S . . O11 O 0.23153(15) 0.18115(16) 0.30429(15) 0.0284(8) Uani 1 1 d . . . O12 O 0.35052(17) 0.20267(17) 0.38937(15) 0.0285(8) Uani 1 1 d . . . O13 O 0.20476(17) 0.17838(17) 0.44150(14) 0.0305(8) Uani 1 1 d . . . C111 C 0.2777(2) 0.1675(2) 0.2456(2) 0.0268(12) Uani 1 1 d . . . C112 C 0.3256(3) 0.1045(2) 0.2467(2) 0.0353(12) Uani 1 1 d . . . H11A H 0.3265 0.0727 0.2868 0.042 Uiso 1 1 calc R . . C113 C 0.3720(3) 0.0882(3) 0.1893(3) 0.0411(13) Uani 1 1 d . . . H11B H 0.4055 0.0453 0.1897 0.049 Uiso 1 1 calc R . . C114 C 0.3697(3) 0.1345(3) 0.1313(3) 0.0433(14) Uani 1 1 d . . . H11C H 0.4014 0.1231 0.0914 0.052 Uiso 1 1 calc R . . C115 C 0.3216(3) 0.1974(3) 0.1306(2) 0.0367(13) Uani 1 1 d . . . H11D H 0.3201 0.2283 0.0899 0.044 Uiso 1 1 calc R . . C116 C 0.2752(2) 0.2161(2) 0.1885(2) 0.0284(12) Uani 1 1 d . . . C121 C 0.3989(3) 0.1899(3) 0.4465(2) 0.0299(12) Uani 1 1 d . . . C122 C 0.4045(3) 0.1167(3) 0.4711(3) 0.0456(14) Uani 1 1 d . . . H12A H 0.3731 0.0780 0.4506 0.055 Uiso 1 1 calc R . . C123 C 0.4558(3) 0.1004(3) 0.5254(3) 0.0595(17) Uani 1 1 d . . . H12B H 0.4591 0.0506 0.5433 0.071 Uiso 1 1 calc R . . C124 C 0.5020(3) 0.1563(4) 0.5535(3) 0.0586(17) Uani 1 1 d . . . H12C H 0.5387 0.1446 0.5898 0.070 Uiso 1 1 calc R . . C125 C 0.4961(3) 0.2287(3) 0.5298(3) 0.0451(16) Uani 1 1 d . . . H12D H 0.5282 0.2666 0.5505 0.054 Uiso 1 1 calc R . . C126 C 0.4437(2) 0.2483(3) 0.4758(2) 0.0320(11) Uani 1 1 d . . . C131 C 0.1344(3) 0.1387(3) 0.4348(2) 0.0318(12) Uani 1 1 d . . . C132 C 0.1377(3) 0.0646(3) 0.4148(2) 0.0392(13) Uani 1 1 d . . . H13A H 0.1876 0.0426 0.4040 0.047 Uiso 1 1 calc R . . C133 C 0.0703(3) 0.0219(3) 0.4101(3) 0.0489(15) Uani 1 1 d . . . H13B H 0.0733 -0.0293 0.3959 0.059 Uiso 1 1 calc R . . C134 C -0.0013(3) 0.0538(3) 0.4260(3) 0.0452(14) Uani 1 1 d . . . H13C H -0.0482 0.0243 0.4236 0.054 Uiso 1 1 calc R . . C135 C -0.0058(3) 0.1280(3) 0.4454(2) 0.0396(13) Uani 1 1 d . . . H13D H -0.0563 0.1492 0.4552 0.047 Uiso 1 1 calc R . . C136 C 0.0618(3) 0.1735(3) 0.4512(2) 0.0296(12) Uani 1 1 d . . . W2 W 0.7500 0.2500 0.150658(12) 0.02204(9) Uani 1 2 d S . . O21 O 0.80813(16) 0.19272(16) 0.21732(14) 0.0253(7) Uani 1 1 d . . . O22 O 0.66657(16) 0.17874(16) 0.16145(15) 0.0262(7) Uani 1 1 d . . . O23 O 0.79510(16) 0.19269(16) 0.07701(15) 0.0255(7) Uani 1 1 d . . . C211 C 0.8865(3) 0.1766(3) 0.2284(2) 0.0259(11) Uani 1 1 d . . . C212 C 0.9390(3) 0.2328(2) 0.2502(2) 0.0289(12) Uani 1 1 d . . . C213 C 1.0187(3) 0.2114(3) 0.2604(2) 0.0369(13) Uani 1 1 d . . . H21A H 1.0565 0.2485 0.2735 0.044 Uiso 1 1 calc R . . C214 C 1.0426(3) 0.1385(3) 0.2520(3) 0.0460(14) Uani 1 1 d . . . H21B H 1.0967 0.1257 0.2589 0.055 Uiso 1 1 calc R . . C215 C 0.9888(3) 0.0834(3) 0.2334(3) 0.0409(14) Uani 1 1 d . . . H21C H 1.0056 0.0326 0.2289 0.049 Uiso 1 1 calc R . . C216 C 0.9104(3) 0.1021(3) 0.2213(2) 0.0305(12) Uani 1 1 d . . . H21D H 0.8732 0.0645 0.2082 0.037 Uiso 1 1 calc R . . C221 C 0.6377(3) 0.1476(3) 0.2233(2) 0.0300(12) Uani 1 1 d . . . C222 C 0.6623(3) 0.0763(3) 0.2407(3) 0.0374(13) Uani 1 1 d . . . H22A H 0.6966 0.0494 0.2101 0.045 Uiso 1 1 calc R . . C223 C 0.6373(3) 0.0442(3) 0.3022(3) 0.0488(15) Uani 1 1 d . . . H22B H 0.6541 -0.0051 0.3143 0.059 Uiso 1 1 calc R . . C224 C 0.5876(3) 0.0834(3) 0.3468(3) 0.0502(16) Uani 1 1 d . . . H22C H 0.5706 0.0614 0.3897 0.060 Uiso 1 1 calc R . . C225 C 0.5626(3) 0.1551(3) 0.3284(3) 0.0422(14) Uani 1 1 d . . . H22D H 0.5277 0.1813 0.3589 0.051 Uiso 1 1 calc R . . C226 C 0.5872(3) 0.1898(3) 0.2662(2) 0.0306(12) Uani 1 1 d . . . C231 C 0.7667(2) 0.1626(3) 0.0154(2) 0.0304(12) Uani 1 1 d . . . C232 C 0.7612(3) 0.0847(3) 0.0119(2) 0.0370(12) Uani 1 1 d . . . H23A H 0.7772 0.0546 0.0506 0.044 Uiso 1 1 calc R . . C233 C 0.7322(3) 0.0518(3) -0.0484(3) 0.0496(15) Uani 1 1 d . . . H23B H 0.7276 -0.0013 -0.0509 0.060 Uiso 1 1 calc R . . C234 C 0.7099(3) 0.0949(3) -0.1048(3) 0.0471(15) Uani 1 1 d . . . H23C H 0.6898 0.0716 -0.1461 0.057 Uiso 1 1 calc R . . C235 C 0.7167(3) 0.1725(3) -0.1012(3) 0.0387(14) Uani 1 1 d . . . H23D H 0.7016 0.2021 -0.1406 0.046 Uiso 1 1 calc R . . C236 C 0.7453(3) 0.2083(2) -0.0408(2) 0.0284(10) Uani 1 1 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 0.02079(15) 0.03794(17) 0.01680(16) 0.000 0.000 0.00280(16) O11 0.026(2) 0.0385(18) 0.0207(18) 0.0030(14) 0.0019(13) -0.0009(14) O12 0.0223(18) 0.040(2) 0.0230(19) -0.0012(15) 0.0014(14) 0.0047(16) O13 0.0227(18) 0.049(2) 0.0197(19) 0.0076(15) 0.0024(14) 0.0085(17) C111 0.030(3) 0.029(3) 0.021(3) -0.003(2) -0.001(2) -0.005(2) C112 0.052(3) 0.031(3) 0.023(3) 0.002(2) 0.000(2) -0.001(3) C113 0.058(4) 0.028(3) 0.037(4) -0.002(2) 0.007(3) 0.012(3) C114 0.054(4) 0.049(4) 0.027(3) -0.007(3) 0.013(3) 0.004(3) C115 0.052(4) 0.039(3) 0.019(3) 0.001(2) 0.002(2) 0.002(3) C116 0.030(3) 0.033(2) 0.022(3) -0.004(2) -0.002(2) -0.0020(19) C121 0.018(3) 0.044(3) 0.028(3) 0.009(2) 0.006(2) 0.008(3) C122 0.037(3) 0.048(4) 0.052(4) 0.013(3) 0.001(3) -0.003(3) C123 0.055(4) 0.061(4) 0.063(4) 0.039(3) -0.001(3) 0.004(3) C124 0.042(4) 0.083(5) 0.051(4) 0.026(4) -0.014(3) 0.006(3) C125 0.035(3) 0.067(5) 0.033(4) 0.006(3) -0.008(3) 0.005(3) C126 0.025(3) 0.052(3) 0.019(3) -0.001(3) 0.0046(18) 0.001(3) C131 0.030(3) 0.044(3) 0.021(3) 0.010(2) 0.000(2) 0.001(3) C132 0.044(4) 0.044(3) 0.030(3) 0.012(3) 0.011(2) 0.016(3) C133 0.060(4) 0.037(3) 0.049(4) 0.002(3) 0.018(3) 0.001(3) C134 0.055(4) 0.045(4) 0.036(3) 0.000(3) 0.007(3) -0.013(3) C135 0.030(3) 0.059(4) 0.030(3) 0.002(3) 0.003(2) -0.001(3) C136 0.030(3) 0.044(3) 0.014(3) 0.006(2) 0.003(2) 0.004(3) W2 0.01803(14) 0.03131(15) 0.01678(16) 0.000 0.000 -0.00186(16) O21 0.0194(18) 0.0348(19) 0.0216(19) 0.0010(14) -0.0005(13) -0.0047(15) O22 0.0235(18) 0.0320(18) 0.023(2) -0.0059(15) -0.0020(13) -0.0041(15) O23 0.0226(17) 0.0337(18) 0.0203(19) 0.0020(15) 0.0023(14) 0.0022(15) C211 0.026(3) 0.038(3) 0.015(3) 0.007(2) 0.001(2) 0.000(2) C212 0.028(3) 0.039(4) 0.020(3) 0.006(2) -0.002(2) -0.005(2) C213 0.023(3) 0.055(4) 0.032(3) 0.001(3) -0.002(2) -0.003(3) C214 0.026(3) 0.068(4) 0.043(4) 0.013(3) 0.000(2) 0.005(3) C215 0.036(3) 0.044(3) 0.043(4) 0.010(3) 0.012(2) 0.010(3) C216 0.030(3) 0.040(3) 0.021(3) 0.004(2) 0.007(2) 0.001(2) C221 0.024(3) 0.034(3) 0.032(3) 0.002(2) -0.005(2) -0.013(2) C222 0.032(3) 0.033(3) 0.047(4) -0.004(3) -0.006(2) -0.006(3) C223 0.055(4) 0.032(3) 0.060(4) 0.005(3) -0.012(3) -0.014(3) C224 0.059(4) 0.052(4) 0.040(4) 0.012(3) 0.004(3) -0.026(3) C225 0.038(3) 0.050(4) 0.039(4) 0.003(3) 0.011(3) -0.012(3) C226 0.023(3) 0.038(3) 0.031(3) -0.002(2) 0.002(2) -0.008(2) C231 0.023(3) 0.050(3) 0.018(3) -0.006(2) 0.004(2) -0.001(2) C232 0.038(3) 0.041(3) 0.032(3) -0.003(2) 0.007(2) -0.002(3) C233 0.051(4) 0.048(3) 0.049(4) -0.019(3) 0.009(3) -0.010(3) C234 0.038(3) 0.068(5) 0.035(4) -0.021(3) 0.003(3) -0.010(3) C235 0.031(3) 0.062(4) 0.023(3) -0.007(3) 0.000(2) -0.005(3) C236 0.023(2) 0.045(2) 0.018(2) -0.001(2) 0.004(3) 0.000(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 O13 1.899(3) 2 ? W1 O13 1.899(3) . ? W1 O12 1.902(3) 2 ? W1 O12 1.902(3) . ? W1 O11 1.906(3) . ? W1 O11 1.906(3) 2 ? O11 C111 1.384(5) . ? O12 C121 1.378(5) . ? O13 C131 1.387(5) . ? C111 C112 1.381(6) . ? C111 C116 1.388(6) . ? C112 C113 1.374(6) . ? C113 C114 1.379(7) . ? C114 C115 1.381(7) . ? C115 C116 1.392(6) . ? C116 C116 1.476(9) 2 ? C121 C122 1.387(6) . ? C121 C126 1.399(7) . ? C122 C123 1.379(7) . ? C123 C124 1.372(8) . ? C124 C125 1.367(7) . ? C125 C126 1.400(6) . ? C126 C136 1.470(7) 2 ? C131 C132 1.371(6) . ? C131 C136 1.407(6) . ? C132 C133 1.370(7) . ? C133 C134 1.368(7) . ? C134 C135 1.372(7) . ? C135 C136 1.403(6) . ? C136 C126 1.470(7) 2 ? W2 O23 1.893(3) 2_655 ? W2 O23 1.893(3) . ? W2 O21 1.900(3) 2_655 ? W2 O21 1.900(3) . ? W2 O22 1.905(3) 2_655 ? W2 O22 1.905(3) . ? O21 C211 1.369(5) . ? O22 C221 1.389(5) . ? O23 C231 1.375(5) . ? C211 C216 1.391(6) . ? C211 C212 1.399(6) . ? C212 C213 1.409(6) . ? C212 C226 1.477(6) 2_655 ? C213 C214 1.367(7) . ? C214 C215 1.383(7) . ? C215 C216 1.383(6) . ? C221 C222 1.375(6) . ? C221 C226 1.398(6) . ? C222 C223 1.371(7) . ? C223 C224 1.381(7) . ? C224 C225 1.387(7) . ? C225 C226 1.397(6) . ? C226 C212 1.477(6) 2_655 ? C231 C232 1.389(6) . ? C231 C236 1.391(6) . ? C232 C233 1.378(7) . ? C233 C234 1.371(7) . ? C234 C235 1.387(7) . ? C235 C236 1.399(6) . ? C236 C236 1.491(8) 2_655 ? 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 O13 W1 O13 102.84(18) 2 . ? O13 W1 O12 89.93(12) 2 2 ? O13 W1 O12 82.85(12) . 2 ? O13 W1 O12 82.85(12) 2 . ? O13 W1 O12 89.93(12) . . ? O12 W1 O12 168.44(17) 2 . ? O13 W1 O11 164.43(12) 2 . ? O13 W1 O11 88.33(12) . . ? O12 W1 O11 102.34(12) 2 . ? O12 W1 O11 86.39(12) . . ? O13 W1 O11 88.33(12) 2 2 ? O13 W1 O11 164.43(11) . 2 ? O12 W1 O11 86.40(12) 2 2 ? O12 W1 O11 102.34(12) . 2 ? O11 W1 O11 82.99(17) . 2 ? C111 O11 W1 128.7(3) . . ? C121 O12 W1 132.8(3) . . ? C131 O13 W1 128.9(3) . . ? C112 C111 O11 117.3(4) . . ? C112 C111 C116 122.3(4) . . ? O11 C111 C116 120.4(4) . . ? C113 C112 C111 119.5(4) . . ? C112 C113 C114 119.6(5) . . ? C113 C114 C115 120.5(5) . . ? C114 C115 C116 121.1(5) . . ? C111 C116 C115 117.0(4) . . ? C111 C116 C116 121.7(3) . 2 ? C115 C116 C116 121.3(3) . 2 ? O12 C121 C122 117.4(5) . . ? O12 C121 C126 120.8(4) . . ? C122 C121 C126 121.7(5) . . ? C123 C122 C121 119.5(5) . . ? C124 C123 C122 119.8(5) . . ? C125 C124 C123 120.8(5) . . ? C124 C125 C126 121.5(5) . . ? C121 C126 C125 116.7(5) . . ? C121 C126 C136 122.7(4) . 2 ? C125 C126 C136 120.6(5) . 2 ? C132 C131 O13 118.6(4) . . ? C132 C131 C136 121.3(5) . . ? O13 C131 C136 120.0(4) . . ? C133 C132 C131 121.1(5) . . ? C134 C133 C132 119.3(5) . . ? C133 C134 C135 120.5(5) . . ? C134 C135 C136 122.0(5) . . ? C135 C136 C131 115.9(5) . . ? C135 C136 C126 121.3(4) . 2 ? C131 C136 C126 122.8(4) . 2 ? O23 W2 O23 84.40(17) 2_655 . ? O23 W2 O21 89.93(12) 2_655 2_655 ? O23 W2 O21 172.23(11) . 2_655 ? O23 W2 O21 172.23(11) 2_655 . ? O23 W2 O21 89.93(12) . . ? O21 W2 O21 96.18(17) 2_655 . ? O23 W2 O22 91.08(12) 2_655 2_655 ? O23 W2 O22 98.10(12) . 2_655 ? O21 W2 O22 87.29(12) 2_655 2_655 ? O21 W2 O22 84.44(12) . 2_655 ? O23 W2 O22 98.10(12) 2_655 . ? O23 W2 O22 91.08(12) . . ? O21 W2 O22 84.44(12) 2_655 . ? O21 W2 O22 87.30(12) . . ? O22 W2 O22 167.61(17) 2_655 . ? C211 O21 W2 135.5(3) . . ? C221 O22 W2 128.0(3) . . ? C231 O23 W2 134.5(3) . . ? O21 C211 C216 117.6(4) . . ? O21 C211 C212 120.5(4) . . ? C216 C211 C212 121.7(4) . . ? C211 C212 C213 116.9(4) . . ? C211 C212 C226 122.5(4) . 2_655 ? C213 C212 C226 120.6(4) . 2_655 ? C214 C213 C212 121.4(5) . . ? C213 C214 C215 120.5(5) . . ? C216 C215 C214 120.0(5) . . ? C215 C216 C211 119.3(5) . . ? C222 C221 O22 117.7(4) . . ? C222 C221 C226 122.6(5) . . ? O22 C221 C226 119.7(4) . . ? C223 C222 C221 119.8(5) . . ? C222 C223 C224 120.1(5) . . ? C223 C224 C225 119.6(5) . . ? C224 C225 C226 121.9(5) . . ? C225 C226 C221 116.1(5) . . ? C225 C226 C212 119.8(4) . 2_655 ? C221 C226 C212 124.1(4) . 2_655 ? O23 C231 C232 116.8(4) . . ? O23 C231 C236 121.3(4) . . ? C232 C231 C236 121.9(4) . . ? C233 C232 C231 119.1(5) . . ? C234 C233 C232 120.9(5) . . ? C233 C234 C235 119.6(5) . . ? C234 C235 C236 121.5(5) . . ? C231 C236 C235 117.1(4) . . ? C231 C236 C236 123.6(3) . 2_655 ? C235 C236 C236 119.3(3) . 2_655 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 22.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.551 _refine_diff_density_min -0.510 _refine_diff_density_rms 0.078 #=END data_freshs _database_code_CSD 199484 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H24 Cl6 O6 W2' _chemical_formula_weight 1132.95 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' 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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.985(2) _cell_length_b 22.734(5) _cell_length_c 16.038(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.85(2) _cell_angle_gamma 90.00 _cell_volume 3632.2(12) _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 red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.072 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2152 _exptl_absorpt_coefficient_mu 6.816 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.23 _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 23703 _diffrn_reflns_av_R_equivalents 0.0755 _diffrn_reflns_av_sigmaI/netI 0.0997 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8307 _reflns_number_gt 5235 _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^)+(0.0224P)^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 8307 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0888 _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.0736 _refine_ls_wR_factor_gt 0.0631 _refine_ls_goodness_of_fit_ref 0.926 _refine_ls_restrained_S_all 0.926 _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 0.72008(3) -0.379167(12) 0.580634(18) 0.02001(8) Uani 1 1 d . . . W2 W 0.54881(3) -0.161103(12) 0.630517(18) 0.02096(8) Uani 1 1 d . . . Cl11 Cl 0.51410(18) -0.34318(8) 0.52807(12) 0.0302(4) Uani 1 1 d . . . Cl12 Cl 0.93117(18) -0.41400(8) 0.63076(11) 0.0295(4) Uani 1 1 d . . . Cl13 Cl 0.80654(19) -0.34223(8) 0.45918(11) 0.0290(4) Uani 1 1 d . . . Cl21 Cl 0.35215(19) -0.20182(9) 0.56879(13) 0.0380(5) Uani 1 1 d . . . Cl22 Cl 0.6591(2) -0.19609(8) 0.51692(11) 0.0340(5) Uani 1 1 d . . . Cl23 Cl 0.4287(2) -0.12627(8) 0.74047(12) 0.0366(5) Uani 1 1 d . . . O11 O 0.6249(5) -0.40991(19) 0.6678(3) 0.0234(11) Uani 1 1 d . . . O12 O 0.7004(5) -0.45293(19) 0.5321(3) 0.0213(11) Uani 1 1 d . . . O13 O 0.7651(5) -0.31286(19) 0.6436(3) 0.0238(11) Uani 1 1 d . . . O21 O 0.7122(5) -0.1274(2) 0.6696(3) 0.0305(12) Uani 1 1 d . . . O22 O 0.5102(5) -0.0886(2) 0.5790(3) 0.0241(11) Uani 1 1 d . . . O23 O 0.5845(5) -0.22700(19) 0.6956(3) 0.0243(11) Uani 1 1 d . . . C111 C 0.5159(7) -0.4467(3) 0.6711(4) 0.0243(17) Uani 1 1 d . . . C112 C 0.5205(7) -0.5058(3) 0.6462(4) 0.0253(17) Uani 1 1 d . . . C113 C 0.4051(8) -0.5384(3) 0.6525(4) 0.033(2) Uani 1 1 d . . . H11A H 0.4053 -0.5788 0.6373 0.040 Uiso 1 1 calc R . . C114 C 0.2895(8) -0.5142(4) 0.6801(5) 0.040(2) Uani 1 1 d . . . H11B H 0.2111 -0.5376 0.6829 0.048 Uiso 1 1 calc R . . C115 C 0.2880(8) -0.4554(4) 0.7038(5) 0.041(2) Uani 1 1 d . . . H11C H 0.2079 -0.4382 0.7213 0.049 Uiso 1 1 calc R . . C116 C 0.4030(7) -0.4221(4) 0.7019(4) 0.0324(19) Uani 1 1 d . . . H11D H 0.4045 -0.3827 0.7216 0.039 Uiso 1 1 calc R . . C121 C 0.7237(7) -0.5110(3) 0.5558(4) 0.0255(17) Uani 1 1 d . . . C122 C 0.6415(7) -0.5354(3) 0.6138(4) 0.0233(16) Uani 1 1 d . . . C123 C 0.6717(8) -0.5934(3) 0.6377(4) 0.0306(18) Uani 1 1 d . . . H12A H 0.6184 -0.6124 0.6765 0.037 Uiso 1 1 calc R . . C124 C 0.7785(8) -0.6238(3) 0.6058(5) 0.0354(19) Uani 1 1 d . . . H12B H 0.8003 -0.6625 0.6248 0.043 Uiso 1 1 calc R . . C125 C 0.8527(8) -0.5970(3) 0.5459(5) 0.037(2) Uani 1 1 d . . . H12C H 0.9223 -0.6184 0.5221 0.044 Uiso 1 1 calc R . . C126 C 0.8267(7) -0.5399(3) 0.5208(4) 0.0266(18) Uani 1 1 d . . . H12D H 0.8782 -0.5213 0.4806 0.032 Uiso 1 1 calc R . . C131 C 0.8604(7) -0.2839(3) 0.6947(4) 0.0243(17) Uani 1 1 d . . . C132 C 0.8278(7) -0.2704(3) 0.7759(4) 0.0247(17) Uani 1 1 d . . . C133 C 0.9318(8) -0.2459(3) 0.8287(5) 0.0319(19) Uani 1 1 d . . . H13A H 0.9168 -0.2380 0.8854 0.038 Uiso 1 1 calc R . . C134 C 1.0544(8) -0.2334(3) 0.7994(6) 0.038(2) Uani 1 1 d . . . H13B H 1.1224 -0.2159 0.8355 0.046 Uiso 1 1 calc R . . C135 C 1.0801(8) -0.2461(3) 0.7170(6) 0.039(2) Uani 1 1 d . . . H13C H 1.1646 -0.2368 0.6965 0.047 Uiso 1 1 calc R . . C136 C 0.9816(7) -0.2723(3) 0.6657(5) 0.0319(19) Uani 1 1 d . . . H13D H 0.9987 -0.2822 0.6099 0.038 Uiso 1 1 calc R . . C211 C 0.8008(7) -0.0865(3) 0.6479(4) 0.0263(17) Uani 1 1 d . . . C212 C 0.7649(7) -0.0277(3) 0.6297(4) 0.0251(17) Uani 1 1 d . . . C213 C 0.8700(8) 0.0091(3) 0.6097(5) 0.0333(19) Uani 1 1 d . . . H21A H 0.8501 0.0488 0.5953 0.040 Uiso 1 1 calc R . . C214 C 0.9997(8) -0.0094(4) 0.6100(5) 0.041(2) Uani 1 1 d . . . H21B H 1.0678 0.0174 0.5965 0.049 Uiso 1 1 calc R . . C215 C 1.0332(8) -0.0674(3) 0.6299(5) 0.036(2) Uani 1 1 d . . . H21C H 1.1237 -0.0804 0.6307 0.043 Uiso 1 1 calc R . . C216 C 0.9331(8) -0.1051(3) 0.6483(5) 0.035(2) Uani 1 1 d . . . H21D H 0.9544 -0.1448 0.6617 0.042 Uiso 1 1 calc R . . C221 C 0.5073(7) -0.0307(3) 0.5996(4) 0.0241(17) Uani 1 1 d . . . C222 C 0.6268(8) -0.0020(3) 0.6291(4) 0.0253(17) Uani 1 1 d . . . C223 C 0.6129(8) 0.0572(3) 0.6531(5) 0.034(2) Uani 1 1 d . . . H22A H 0.6885 0.0780 0.6771 0.040 Uiso 1 1 calc R . . C224 C 0.4904(9) 0.0853(3) 0.6421(5) 0.035(2) Uani 1 1 d . . . H22B H 0.4836 0.1253 0.6581 0.042 Uiso 1 1 calc R . . C225 C 0.3779(8) 0.0566(3) 0.6084(5) 0.0317(19) Uani 1 1 d . . . H22C H 0.2954 0.0770 0.5985 0.038 Uiso 1 1 calc R . . C226 C 0.3873(7) -0.0017(3) 0.5895(4) 0.0244(17) Uani 1 1 d . . . H22D H 0.3094 -0.0225 0.5690 0.029 Uiso 1 1 calc R . . C231 C 0.5765(7) -0.2607(3) 0.7657(4) 0.0225(17) Uani 1 1 d . . . C232 C 0.6936(8) -0.2822(3) 0.8066(4) 0.0230(17) Uani 1 1 d . . . C233 C 0.6796(9) -0.3134(3) 0.8805(5) 0.035(2) Uani 1 1 d . . . H23A H 0.7569 -0.3291 0.9103 0.042 Uiso 1 1 calc R . . C234 C 0.5537(10) -0.3218(4) 0.9111(5) 0.049(3) Uani 1 1 d . . . H23B H 0.5464 -0.3430 0.9616 0.059 Uiso 1 1 calc R . . C235 C 0.4424(10) -0.3003(3) 0.8700(5) 0.042(2) Uani 1 1 d . . . H23C H 0.3573 -0.3067 0.8916 0.051 Uiso 1 1 calc R . . C236 C 0.4514(8) -0.2688(3) 0.7960(5) 0.0312(19) Uani 1 1 d . . . H23D H 0.3732 -0.2533 0.7671 0.037 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 0.02047(16) 0.02084(15) 0.01877(15) -0.00300(13) 0.00156(12) -0.00052(14) W2 0.02005(16) 0.02314(16) 0.01973(15) 0.00174(13) 0.00167(12) 0.00272(14) Cl11 0.0232(10) 0.0298(10) 0.0367(11) -0.0025(9) -0.0045(8) 0.0014(9) Cl12 0.0251(10) 0.0328(10) 0.0304(10) -0.0025(8) 0.0004(8) 0.0055(9) Cl13 0.0326(11) 0.0295(10) 0.0252(9) 0.0035(8) 0.0044(8) 0.0002(9) Cl21 0.0285(11) 0.0420(12) 0.0420(12) 0.0052(10) -0.0078(9) -0.0069(10) Cl22 0.0428(12) 0.0315(10) 0.0294(10) 0.0020(8) 0.0151(9) 0.0051(10) Cl23 0.0453(13) 0.0370(11) 0.0291(10) 0.0005(9) 0.0137(9) 0.0141(10) O11 0.022(3) 0.025(3) 0.022(3) -0.006(2) 0.001(2) 0.001(2) O12 0.027(3) 0.019(2) 0.017(3) -0.002(2) 0.001(2) -0.001(2) O13 0.023(3) 0.029(3) 0.019(3) -0.005(2) 0.000(2) 0.004(2) O21 0.028(3) 0.036(3) 0.027(3) 0.007(2) -0.005(2) 0.001(3) O22 0.029(3) 0.028(3) 0.015(2) -0.004(2) -0.004(2) -0.004(2) O23 0.023(3) 0.022(3) 0.027(3) -0.001(2) 0.002(2) 0.001(2) C111 0.023(4) 0.035(4) 0.016(4) -0.004(3) 0.001(3) -0.010(4) C112 0.024(4) 0.035(4) 0.017(4) -0.002(3) 0.002(3) -0.002(4) C113 0.029(5) 0.042(5) 0.028(4) 0.009(4) 0.002(4) -0.016(4) C114 0.033(5) 0.053(6) 0.033(5) 0.005(4) 0.002(4) -0.025(5) C115 0.027(5) 0.062(6) 0.034(5) 0.002(4) 0.006(4) 0.004(5) C116 0.018(4) 0.049(5) 0.031(4) 0.000(4) 0.008(3) 0.001(4) C121 0.030(4) 0.023(4) 0.023(4) 0.003(3) -0.008(3) -0.001(4) C122 0.021(4) 0.025(4) 0.022(4) 0.000(3) -0.007(3) 0.002(3) C123 0.030(5) 0.039(5) 0.022(4) -0.004(4) 0.001(3) -0.009(4) C124 0.038(5) 0.031(4) 0.035(5) 0.007(4) -0.016(4) -0.002(4) C125 0.024(5) 0.039(5) 0.047(5) 0.001(4) 0.003(4) 0.002(4) C126 0.030(5) 0.029(4) 0.021(4) -0.001(3) 0.002(3) -0.005(4) C131 0.019(4) 0.022(4) 0.031(4) -0.011(3) -0.006(3) 0.005(3) C132 0.024(4) 0.021(4) 0.029(4) -0.007(3) -0.004(3) 0.008(3) C133 0.038(5) 0.022(4) 0.034(5) -0.008(4) -0.008(4) 0.011(4) C134 0.021(5) 0.029(5) 0.060(6) -0.002(4) -0.021(4) 0.005(4) C135 0.019(4) 0.037(5) 0.061(6) 0.005(4) 0.000(4) 0.000(4) C136 0.022(4) 0.035(5) 0.039(5) -0.006(4) 0.002(4) 0.002(4) C211 0.024(4) 0.031(4) 0.023(4) 0.000(3) -0.002(3) -0.001(4) C212 0.029(4) 0.027(4) 0.019(4) -0.003(3) 0.002(3) -0.005(4) C213 0.030(5) 0.041(5) 0.030(4) -0.001(4) 0.002(4) -0.008(4) C214 0.034(5) 0.060(6) 0.029(5) 0.002(4) 0.006(4) -0.015(5) C215 0.023(4) 0.050(5) 0.035(5) 0.006(4) 0.005(4) -0.005(4) C216 0.031(5) 0.040(5) 0.033(5) -0.003(4) -0.005(4) 0.008(4) C221 0.027(4) 0.029(4) 0.016(4) 0.004(3) 0.002(3) 0.003(4) C222 0.032(5) 0.022(4) 0.022(4) 0.006(3) -0.001(3) -0.004(4) C223 0.044(5) 0.023(4) 0.034(5) -0.002(4) 0.001(4) -0.004(4) C224 0.050(6) 0.020(4) 0.035(5) 0.000(4) 0.012(4) 0.006(4) C225 0.032(5) 0.027(4) 0.037(5) 0.011(4) 0.007(4) 0.010(4) C226 0.023(4) 0.023(4) 0.028(4) 0.010(3) 0.007(3) -0.003(3) C231 0.033(4) 0.016(4) 0.019(4) 0.004(3) 0.005(3) 0.002(3) C232 0.036(5) 0.013(4) 0.020(4) -0.008(3) 0.000(3) 0.003(3) C233 0.053(6) 0.022(4) 0.030(5) -0.002(3) -0.003(4) 0.014(4) C234 0.071(7) 0.045(6) 0.034(5) 0.010(4) 0.028(5) 0.010(5) C235 0.048(6) 0.033(5) 0.048(5) 0.004(4) 0.026(5) -0.001(5) C236 0.040(5) 0.027(4) 0.029(4) 0.009(3) 0.012(4) 0.009(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 O13 1.853(4) . ? W1 O12 1.854(4) . ? W1 O11 1.878(4) . ? W1 Cl11 2.3189(19) . ? W1 Cl13 2.3388(17) . ? W1 Cl12 2.3426(19) . ? W2 O23 1.847(4) . ? W2 O22 1.871(5) . ? W2 O21 1.872(5) . ? W2 Cl21 2.331(2) . ? W2 Cl22 2.3308(18) . ? W2 Cl23 2.3366(18) . ? O11 C111 1.375(8) . ? O12 C121 1.389(8) . ? O13 C131 1.380(8) . ? O21 C211 1.345(8) . ? O22 C221 1.359(8) . ? O23 C231 1.367(7) . ? C111 C116 1.380(9) . ? C111 C112 1.403(9) . ? C112 C113 1.380(9) . ? C112 C122 1.507(10) . ? C113 C114 1.379(10) . ? C114 C115 1.390(11) . ? C115 C116 1.377(10) . ? C121 C126 1.372(9) . ? C121 C122 1.396(9) . ? C122 C123 1.401(9) . ? C123 C124 1.396(10) . ? C124 C125 1.392(10) . ? C125 C126 1.379(10) . ? C131 C136 1.351(9) . ? C131 C132 1.398(9) . ? C132 C133 1.409(10) . ? C132 C232 1.482(10) . ? C133 C134 1.370(10) . ? C134 C135 1.392(11) . ? C135 C136 1.375(10) . ? C211 C216 1.386(10) . ? C211 C212 1.409(9) . ? C212 C213 1.395(10) . ? C212 C222 1.497(10) . ? C213 C214 1.362(11) . ? C214 C215 1.392(11) . ? C215 C216 1.364(10) . ? C221 C226 1.367(9) . ? C221 C222 1.412(10) . ? C222 C223 1.410(9) . ? C223 C224 1.380(10) . ? C224 C225 1.378(10) . ? C225 C226 1.364(9) . ? C231 C236 1.383(9) . ? C231 C232 1.391(10) . ? C232 C233 1.396(9) . ? C233 C234 1.393(11) . ? C234 C235 1.345(12) . ? C235 C236 1.394(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O13 W1 O12 168.5(2) . . ? O13 W1 O11 90.76(19) . . ? O12 W1 O11 86.05(18) . . ? O13 W1 Cl11 95.05(15) . . ? O12 W1 Cl11 95.75(15) . . ? O11 W1 Cl11 85.47(15) . . ? O13 W1 Cl13 94.15(14) . . ? O12 W1 Cl13 90.57(14) . . ? O11 W1 Cl13 170.91(15) . . ? Cl11 W1 Cl13 86.47(7) . . ? O13 W1 Cl12 84.73(15) . . ? O12 W1 Cl12 84.60(15) . . ? O11 W1 Cl12 96.17(15) . . ? Cl11 W1 Cl12 178.35(7) . . ? Cl13 W1 Cl12 91.91(7) . . ? O23 W2 O22 171.78(19) . . ? O23 W2 O21 90.7(2) . . ? O22 W2 O21 86.4(2) . . ? O23 W2 Cl21 92.46(16) . . ? O22 W2 Cl21 91.11(15) . . ? O21 W2 Cl21 174.42(15) . . ? O23 W2 Cl22 94.68(14) . . ? O22 W2 Cl22 92.86(14) . . ? O21 W2 Cl22 87.39(16) . . ? Cl21 W2 Cl22 87.77(7) . . ? O23 W2 Cl23 86.43(14) . . ? O22 W2 Cl23 86.18(14) . . ? O21 W2 Cl23 95.09(16) . . ? Cl21 W2 Cl23 89.69(8) . . ? Cl22 W2 Cl23 177.27(8) . . ? C111 O11 W1 134.0(4) . . ? C121 O12 W1 137.2(4) . . ? C131 O13 W1 147.6(4) . . ? C211 O21 W2 140.4(4) . . ? C221 O22 W2 138.9(4) . . ? C231 O23 W2 154.1(4) . . ? O11 C111 C116 115.8(6) . . ? O11 C111 C112 122.0(6) . . ? C116 C111 C112 122.2(7) . . ? C113 C112 C111 116.8(7) . . ? C113 C112 C122 118.5(7) . . ? C111 C112 C122 124.7(6) . . ? C114 C113 C112 122.0(7) . . ? C113 C114 C115 119.7(7) . . ? C116 C115 C114 119.9(8) . . ? C115 C116 C111 119.2(7) . . ? C126 C121 O12 117.4(6) . . ? C126 C121 C122 124.9(7) . . ? O12 C121 C122 117.7(6) . . ? C121 C122 C123 115.6(6) . . ? C121 C122 C112 125.0(6) . . ? C123 C122 C112 119.3(6) . . ? C124 C123 C122 121.4(7) . . ? C125 C124 C123 119.4(7) . . ? C126 C125 C124 121.0(7) . . ? C121 C126 C125 117.6(7) . . ? C136 C131 O13 119.1(6) . . ? C136 C131 C132 123.2(7) . . ? O13 C131 C132 117.6(6) . . ? C131 C132 C133 116.0(7) . . ? C131 C132 C232 122.8(7) . . ? C133 C132 C232 121.2(6) . . ? C134 C133 C132 121.1(7) . . ? C133 C134 C135 120.5(8) . . ? C136 C135 C134 119.2(8) . . ? C131 C136 C135 120.0(7) . . ? O21 C211 C216 115.5(7) . . ? O21 C211 C212 123.2(7) . . ? C216 C211 C212 121.2(7) . . ? C213 C212 C211 115.6(7) . . ? C213 C212 C222 118.1(6) . . ? C211 C212 C222 126.3(7) . . ? C214 C213 C212 122.9(8) . . ? C213 C214 C215 120.5(8) . . ? C216 C215 C214 118.4(7) . . ? C215 C216 C211 121.3(7) . . ? O22 C221 C226 118.1(7) . . ? O22 C221 C222 119.8(6) . . ? C226 C221 C222 122.1(7) . . ? C223 C222 C221 115.8(7) . . ? C223 C222 C212 118.5(7) . . ? C221 C222 C212 125.5(6) . . ? C224 C223 C222 120.6(7) . . ? C225 C224 C223 121.5(7) . . ? C226 C225 C224 118.8(7) . . ? C225 C226 C221 120.9(7) . . ? O23 C231 C236 117.9(7) . . ? O23 C231 C232 119.4(6) . . ? C236 C231 C232 122.5(6) . . ? C231 C232 C233 116.7(7) . . ? C231 C232 C132 122.0(6) . . ? C233 C232 C132 121.2(7) . . ? C234 C233 C232 120.9(8) . . ? C235 C234 C233 120.9(8) . . ? C234 C235 C236 120.3(8) . . ? C231 C236 C235 118.6(8) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.869 _refine_diff_density_min -0.803 _refine_diff_density_rms 0.199 #=END