# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'N Connelly' _publ_contact_author_email NEIL.CONNELLY@BRISTOL.AC.UK _publ_section_title ; The d3/d2 alkyne complexes [MX2(?-RC?CR)Tp']z (X = halide, z = 0 and +1): final links in a d6-d2 redox family tree ; loop_ _publ_author_name 'N Connelly' 'Chris Adams' 'Kirsty Anderson' 'David J Harding' 'Owen D Hayward' 'A Orpen' ; E.Patron ; 'Philip Rieger' # Attachment 'revised cifs.cif' data_1[I3] _database_code_depnum_ccdc_archive 'CCDC 697668' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H28 B F2 I3 N6 W' _chemical_formula_weight 953.83 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.7911(15) _cell_length_b 16.443(3) _cell_length_c 14.028(2) _cell_angle_alpha 90.000(12) _cell_angle_beta 95.492(15) _cell_angle_gamma 90.000(15) _cell_volume 2707.3(7) _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 block _exptl_crystal_colour 'Dark purple' _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 2.340 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760 _exptl_absorpt_coefficient_mu 7.720 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.26 _exptl_absorpt_correction_T_max 0.37 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 17474 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_av_sigmaI/netI 0.0467 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 27.52 _reflns_number_total 6206 _reflns_number_gt 4761 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0290P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6206 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0442 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0633 _refine_ls_wR_factor_gt 0.0602 _refine_ls_goodness_of_fit_ref 0.933 _refine_ls_restrained_S_all 0.933 _refine_ls_shift/su_max 0.005 _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 0.722577(17) 0.321592(11) 0.475307(13) 0.02423(6) Uani 1 1 d . . . F1 F 0.6297(2) 0.35842(16) 0.3629(2) 0.0342(7) Uani 1 1 d . . . F2 F 0.8569(2) 0.28645(16) 0.42267(19) 0.0320(6) Uani 1 1 d . . . N1 N 0.7976(3) 0.4431(2) 0.4664(3) 0.0248(9) Uani 1 1 d . . . N2 N 0.8110(3) 0.4935(2) 0.5448(3) 0.0262(9) Uani 1 1 d . . . C1 C 0.8327(5) 0.4484(3) 0.2941(3) 0.0366(12) Uani 1 1 d . . . H1A H 0.8561 0.3912 0.2982 0.055 Uiso 1 1 calc R . . H1B H 0.8842 0.4787 0.2563 0.055 Uiso 1 1 calc R . . H1C H 0.7547 0.4521 0.2632 0.055 Uiso 1 1 calc R . . C2 C 0.8372(4) 0.4834(3) 0.3920(3) 0.0270(10) Uani 1 1 d . . . C3 C 0.8772(4) 0.5583(3) 0.4239(3) 0.0293(11) Uani 1 1 d . . . H3A H 0.9104 0.5986 0.3867 0.035 Uiso 1 1 calc R . . C4 C 0.8603(4) 0.5641(3) 0.5193(3) 0.0273(10) Uani 1 1 d . . . C5 C 0.8883(4) 0.6309(3) 0.5888(4) 0.0360(12) Uani 1 1 d . . . H5A H 0.8272 0.6362 0.6311 0.054 Uiso 1 1 calc R . . H5B H 0.8962 0.6820 0.5541 0.054 Uiso 1 1 calc R . . H5C H 0.9601 0.6185 0.6271 0.054 Uiso 1 1 calc R . . N3 N 0.8287(3) 0.3181(2) 0.6086(3) 0.0288(9) Uani 1 1 d . . . N4 N 0.8356(3) 0.3841(2) 0.6693(3) 0.0271(9) Uani 1 1 d . . . C6 C 0.9189(5) 0.1804(3) 0.6003(4) 0.0416(13) Uani 1 1 d . . . H6A H 0.8459 0.1530 0.5835 0.062 Uiso 1 1 calc R . . H6B H 0.9676 0.1459 0.6440 0.062 Uiso 1 1 calc R . . H6C H 0.9565 0.1904 0.5421 0.062 Uiso 1 1 calc R . . C7 C 0.8986(4) 0.2598(3) 0.6483(4) 0.0326(11) Uani 1 1 d . . . C8 C 0.9489(4) 0.2883(3) 0.7354(4) 0.0360(12) Uani 1 1 d . . . H8A H 1.0013 0.2596 0.7789 0.043 Uiso 1 1 calc R . . C9 C 0.9084(4) 0.3661(3) 0.7470(3) 0.0294(11) Uani 1 1 d . . . C10 C 0.9336(5) 0.4241(4) 0.8289(3) 0.0423(14) Uani 1 1 d . . . H10A H 0.9298 0.4801 0.8048 0.063 Uiso 1 1 calc R . . H10B H 1.0101 0.4133 0.8601 0.063 Uiso 1 1 calc R . . H10C H 0.8774 0.4167 0.8753 0.063 Uiso 1 1 calc R . . N5 N 0.6069(3) 0.3854(2) 0.5548(3) 0.0265(9) Uani 1 1 d . . . N6 N 0.6427(3) 0.4424(2) 0.6230(3) 0.0255(9) Uani 1 1 d . . . C11 C 0.4199(4) 0.3289(3) 0.4834(4) 0.0338(11) Uani 1 1 d . . . H11A H 0.4401 0.2717 0.4951 0.051 Uiso 1 1 calc R . . H11B H 0.4333 0.3434 0.4176 0.051 Uiso 1 1 calc R . . H11C H 0.3393 0.3371 0.4924 0.051 Uiso 1 1 calc R . . C12 C 0.4910(4) 0.3811(3) 0.5515(3) 0.0271(10) Uani 1 1 d . . . C13 C 0.4553(4) 0.4337(3) 0.6188(3) 0.0300(11) Uani 1 1 d . . . H13A H 0.3789 0.4427 0.6323 0.036 Uiso 1 1 calc R . . C14 C 0.5511(4) 0.4709(3) 0.6632(3) 0.0278(10) Uani 1 1 d . . . C15 C 0.5600(4) 0.5317(3) 0.7421(3) 0.0346(12) Uani 1 1 d . . . H15A H 0.6279 0.5202 0.7860 0.052 Uiso 1 1 calc R . . H15B H 0.4920 0.5284 0.7771 0.052 Uiso 1 1 calc R . . H15C H 0.5658 0.5864 0.7154 0.052 Uiso 1 1 calc R . . C16 C 0.6487(4) 0.2208(3) 0.5278(3) 0.0300(11) Uani 1 1 d . . . C17 C 0.6534(4) 0.2122(3) 0.4365(3) 0.0296(11) Uani 1 1 d . . . C18 C 0.6226(5) 0.1652(3) 0.3492(4) 0.0442(14) Uani 1 1 d . . . H18A H 0.5850 0.1146 0.3656 0.066 Uiso 1 1 calc R . . H18B H 0.6916 0.1524 0.3184 0.066 Uiso 1 1 calc R . . H18C H 0.5706 0.1972 0.3052 0.066 Uiso 1 1 calc R . . C19 C 0.6100(5) 0.1868(3) 0.6159(4) 0.0426(14) Uani 1 1 d . . . H19A H 0.6032 0.1276 0.6097 0.064 Uiso 1 1 calc R . . H19B H 0.5358 0.2100 0.6265 0.064 Uiso 1 1 calc R . . H19C H 0.6654 0.2001 0.6703 0.064 Uiso 1 1 calc R . . B1 B 0.7702(5) 0.4638(3) 0.6398(4) 0.0259(12) Uani 1 1 d . . . H1 H 0.7838 0.5062 0.6907 0.031 Uiso 1 1 calc R . . I1 I 0.7254(7) -0.0296(4) 0.5159(4) 0.0615(17) Uani 0.56(6) 1 d P A 1 I1' I 0.704(3) -0.0363(10) 0.5217(9) 0.092(2) Uani 0.44(6) 1 d P A 2 I2 I 0.72819(3) -0.15568(2) 0.67172(3) 0.04337(10) Uani 1 1 d . . . I3 I 0.73965(4) -0.27622(2) 0.82198(3) 0.05528(13) 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 W1 0.02613(11) 0.02261(10) 0.02398(9) -0.00152(8) 0.00259(7) 0.00003(9) F1 0.0311(17) 0.0274(15) 0.0437(17) 0.0028(12) 0.0026(13) 0.0001(13) F2 0.0275(16) 0.0336(15) 0.0357(16) 0.0020(12) 0.0069(12) -0.0029(13) N1 0.027(2) 0.024(2) 0.024(2) -0.0038(16) 0.0065(16) 0.0031(17) N2 0.024(2) 0.020(2) 0.034(2) -0.0040(16) -0.0001(16) 0.0006(17) C1 0.042(3) 0.039(3) 0.029(3) 0.008(2) 0.008(2) 0.004(3) C2 0.022(3) 0.028(3) 0.032(3) 0.009(2) 0.006(2) 0.006(2) C3 0.024(3) 0.024(2) 0.041(3) 0.008(2) 0.005(2) 0.001(2) C4 0.018(3) 0.023(2) 0.042(3) 0.001(2) 0.003(2) 0.003(2) C5 0.030(3) 0.029(3) 0.048(3) -0.003(2) 0.002(2) -0.005(2) N3 0.031(2) 0.026(2) 0.029(2) -0.0021(17) 0.0030(17) 0.0002(19) N4 0.026(2) 0.030(2) 0.026(2) 0.0036(17) 0.0033(17) 0.0006(18) C6 0.044(3) 0.031(3) 0.050(3) 0.008(3) 0.004(3) 0.010(3) C7 0.028(3) 0.034(3) 0.036(3) 0.008(2) 0.002(2) 0.003(2) C8 0.028(3) 0.043(3) 0.036(3) 0.014(2) 0.001(2) 0.004(2) C9 0.022(3) 0.044(3) 0.023(2) 0.008(2) 0.0057(19) 0.001(2) C10 0.032(3) 0.066(4) 0.029(3) -0.005(3) 0.001(2) -0.003(3) N5 0.027(2) 0.023(2) 0.029(2) -0.0024(16) 0.0034(17) -0.0022(18) N6 0.031(2) 0.021(2) 0.025(2) -0.0025(15) 0.0028(17) 0.0019(17) C11 0.022(3) 0.039(3) 0.040(3) -0.002(2) 0.001(2) -0.002(2) C12 0.024(3) 0.029(3) 0.028(2) 0.0037(19) 0.0015(19) 0.001(2) C13 0.023(3) 0.033(3) 0.034(3) 0.002(2) 0.003(2) 0.007(2) C14 0.031(3) 0.023(2) 0.030(3) 0.0039(19) 0.008(2) 0.002(2) C15 0.040(3) 0.030(3) 0.034(3) -0.004(2) 0.005(2) 0.003(2) C16 0.026(3) 0.026(3) 0.038(3) -0.003(2) 0.003(2) -0.001(2) C17 0.027(3) 0.025(2) 0.037(3) -0.003(2) 0.004(2) 0.002(2) C18 0.057(4) 0.036(3) 0.039(3) -0.011(2) 0.001(3) -0.002(3) C19 0.051(4) 0.026(3) 0.051(3) 0.007(2) 0.009(3) -0.005(3) B1 0.027(3) 0.024(3) 0.027(3) -0.005(2) 0.005(2) 0.003(2) I1 0.096(2) 0.0463(18) 0.0385(14) 0.0039(9) -0.0134(8) -0.0007(17) I1' 0.138(6) 0.076(3) 0.056(2) -0.0081(18) -0.019(3) 0.027(3) I2 0.0363(2) 0.0403(2) 0.0530(2) -0.01718(16) 0.00219(16) -0.00398(16) I3 0.0641(3) 0.0422(2) 0.0638(3) -0.00942(19) 0.0277(2) -0.0143(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 F2 1.900(3) . ? W1 F1 1.929(3) . ? W1 C17 2.027(5) . ? W1 C16 2.042(5) . ? W1 N5 2.120(4) . ? W1 N3 2.149(4) . ? W1 N1 2.193(4) . ? N1 C2 1.357(5) . ? N1 N2 1.374(5) . ? N2 C4 1.361(6) . ? N2 B1 1.538(6) . ? C1 C2 1.485(6) . ? C2 C3 1.378(7) . ? C3 C4 1.375(7) . ? C4 C5 1.485(7) . ? N3 C7 1.350(6) . ? N3 N4 1.376(5) . ? N4 C9 1.354(6) . ? N4 B1 1.557(6) . ? C6 C7 1.498(7) . ? C7 C8 1.388(7) . ? C8 C9 1.381(7) . ? C9 C10 1.501(7) . ? N5 C12 1.365(6) . ? N5 N6 1.377(5) . ? N6 C14 1.349(6) . ? N6 B1 1.541(7) . ? C11 C12 1.482(7) . ? C12 C13 1.376(6) . ? C13 C14 1.379(7) . ? C14 C15 1.487(6) . ? C16 C17 1.295(6) . ? C16 C19 1.468(7) . ? C17 C18 1.464(7) . ? I1 I2 3.011(5) . ? I1' I2 2.872(17) . ? I2 I3 2.8871(7) . ? 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 F2 W1 F1 101.93(11) . . ? F2 W1 C17 87.40(16) . . ? F1 W1 C17 82.92(16) . . ? F2 W1 C16 107.07(15) . . ? F1 W1 C16 108.73(16) . . ? C17 W1 C16 37.10(18) . . ? F2 W1 N5 163.10(13) . . ? F1 W1 N5 86.06(13) . . ? C17 W1 N5 108.52(17) . . ? C16 W1 N5 83.91(16) . . ? F2 W1 N3 83.84(13) . . ? F1 W1 N3 163.20(13) . . ? C17 W1 N3 113.31(18) . . ? C16 W1 N3 84.12(18) . . ? N5 W1 N3 84.60(15) . . ? F2 W1 N1 84.22(12) . . ? F1 W1 N1 82.42(13) . . ? C17 W1 N1 161.22(16) . . ? C16 W1 N1 161.45(16) . . ? N5 W1 N1 82.10(13) . . ? N3 W1 N1 82.49(14) . . ? C2 N1 N2 107.4(4) . . ? C2 N1 W1 131.2(3) . . ? N2 N1 W1 121.4(3) . . ? C4 N2 N1 108.9(4) . . ? C4 N2 B1 132.5(4) . . ? N1 N2 B1 118.7(4) . . ? N1 C2 C3 108.6(4) . . ? N1 C2 C1 122.5(4) . . ? C3 C2 C1 128.9(4) . . ? C4 C3 C2 107.5(4) . . ? N2 C4 C3 107.6(4) . . ? N2 C4 C5 122.1(4) . . ? C3 C4 C5 130.3(4) . . ? C7 N3 N4 107.9(4) . . ? C7 N3 W1 131.3(3) . . ? N4 N3 W1 120.8(3) . . ? C9 N4 N3 108.7(4) . . ? C9 N4 B1 131.1(4) . . ? N3 N4 B1 120.1(4) . . ? N3 C7 C8 108.4(4) . . ? N3 C7 C6 123.5(5) . . ? C8 C7 C6 128.0(5) . . ? C9 C8 C7 107.0(5) . . ? N4 C9 C8 107.9(4) . . ? N4 C9 C10 122.8(5) . . ? C8 C9 C10 129.3(5) . . ? C12 N5 N6 107.4(4) . . ? C12 N5 W1 130.5(3) . . ? N6 N5 W1 122.2(3) . . ? C14 N6 N5 108.8(4) . . ? C14 N6 B1 131.7(4) . . ? N5 N6 B1 119.5(3) . . ? N5 C12 C13 108.3(4) . . ? N5 C12 C11 123.7(4) . . ? C13 C12 C11 128.0(4) . . ? C12 C13 C14 107.3(4) . . ? N6 C14 C13 108.1(4) . . ? N6 C14 C15 122.9(5) . . ? C13 C14 C15 129.0(5) . . ? C17 C16 C19 146.9(5) . . ? C17 C16 W1 70.8(3) . . ? C19 C16 W1 142.2(4) . . ? C16 C17 C18 148.6(5) . . ? C16 C17 W1 72.1(3) . . ? C18 C17 W1 139.0(4) . . ? N2 B1 N6 108.7(4) . . ? N2 B1 N4 108.0(4) . . ? N6 B1 N4 107.4(4) . . ? I1' I2 I3 177.0(7) . . ? I1' I2 I1 5.1(6) . . ? I3 I2 I1 177.94(15) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.131 _refine_diff_density_min -1.533 _refine_diff_density_rms 0.136 #===END data_2[BF4] _database_code_depnum_ccdc_archive 'CCDC 697669' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H32 B2 F6 N6 W' _chemical_formula_weight 784.08 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' F F 0.0171 0.0103 '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 12.2631(16) _cell_length_b 12.5168(17) _cell_length_c 20.124(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.574(2) _cell_angle_gamma 90.00 _cell_volume 3045.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 205 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.710 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1544 _exptl_absorpt_coefficient_mu 3.860 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.362619 _exptl_absorpt_correction_T_max 0.491509 _exptl_absorpt_process_details 'SADABS (Sheldrick 1996)' _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 CCD area detector' _diffrn_measurement_method '\w scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 15983 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0486 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5366 _reflns_number_gt 4171 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0265P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5366 _refine_ls_number_parameters 403 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0436 _refine_ls_R_factor_gt 0.0271 _refine_ls_wR_factor_ref 0.0594 _refine_ls_wR_factor_gt 0.0555 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.974 _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 0.763440(14) 0.959124(14) 0.111052(9) 0.01926(6) Uani 1 1 d . . . F1 F 0.6658(2) 1.06489(18) 0.06943(12) 0.0262(6) Uani 1 1 d . . . F2 F 0.89125(18) 1.0408(2) 0.14332(12) 0.0264(6) Uani 1 1 d . . . N1 N 0.8272(3) 0.9679(3) 0.01551(18) 0.0218(8) Uani 1 1 d . . . N2 N 0.8363(3) 0.8769(3) -0.02184(18) 0.0239(9) Uani 1 1 d . . . C1 C 0.8542(4) 1.1635(3) 0.0039(2) 0.0289(11) Uani 1 1 d . . . H1A H 0.8892 1.1668 0.0513 0.043 Uiso 1 1 calc R . . H1B H 0.7775 1.1885 -0.0006 0.043 Uiso 1 1 calc R . . H1C H 0.8949 1.2091 -0.0231 0.043 Uiso 1 1 calc R . . C2 C 0.8554(3) 1.0510(4) -0.0205(2) 0.0232(10) Uani 1 1 d . . . C3 C 0.8824(4) 1.0132(4) -0.0799(2) 0.0287(12) Uani 1 1 d . . . H3A H 0.9058 1.0548 -0.1145 0.034 Uiso 1 1 calc R . . C4 C 0.8693(3) 0.9038(4) -0.0799(2) 0.0240(11) Uani 1 1 d . . . C5 C 0.8848(4) 0.8232(4) -0.1323(2) 0.0342(12) Uani 1 1 d . . . H5A H 0.9330 0.7657 -0.1115 0.051 Uiso 1 1 calc R . . H5B H 0.9187 0.8576 -0.1676 0.051 Uiso 1 1 calc R . . H5C H 0.8128 0.7935 -0.1522 0.051 Uiso 1 1 calc R . . N3 N 0.6514(3) 0.8498(3) 0.05547(18) 0.0223(9) Uani 1 1 d . . . N4 N 0.6881(3) 0.7691(3) 0.01700(18) 0.0223(8) Uani 1 1 d . . . C6 C 0.4706(4) 0.9130(4) 0.0823(2) 0.0315(12) Uani 1 1 d . . . H6A H 0.4870 0.9867 0.0707 0.047 Uiso 1 1 calc R . . H6B H 0.4870 0.9040 0.1313 0.047 Uiso 1 1 calc R . . H6C H 0.3923 0.8978 0.0663 0.047 Uiso 1 1 calc R . . C7 C 0.5399(3) 0.8382(4) 0.0499(2) 0.0247(11) Uani 1 1 d . . . C8 C 0.5068(4) 0.7517(4) 0.0094(2) 0.0292(11) Uani 1 1 d . . . H8A H 0.4333 0.7258 -0.0028 0.035 Uiso 1 1 calc R . . C9 C 0.6007(4) 0.7095(4) -0.0102(2) 0.0254(11) Uani 1 1 d . . . C10 C 0.6111(4) 0.6135(4) -0.0529(2) 0.0316(11) Uani 1 1 d . . . H10A H 0.6574 0.6309 -0.0867 0.047 Uiso 1 1 calc R . . H10B H 0.5376 0.5916 -0.0756 0.047 Uiso 1 1 calc R . . H10C H 0.6451 0.5549 -0.0244 0.047 Uiso 1 1 calc R . . N5 N 0.8727(3) 0.8273(3) 0.12784(18) 0.0215(8) Uani 1 1 d . . . N6 N 0.8836(3) 0.7550(3) 0.07731(19) 0.0224(9) Uani 1 1 d . . . C11 C 0.9608(4) 0.8592(4) 0.2478(2) 0.0329(12) Uani 1 1 d . . . H11A H 0.8927 0.8573 0.2673 0.049 Uiso 1 1 calc R . . H11B H 0.9789 0.9334 0.2387 0.049 Uiso 1 1 calc R . . H11C H 1.0215 0.8277 0.2796 0.049 Uiso 1 1 calc R . . C12 C 0.9444(3) 0.7968(4) 0.1834(2) 0.0246(11) Uani 1 1 d . . . C13 C 0.9989(4) 0.7070(4) 0.1681(2) 0.0309(12) Uani 1 1 d . . . H13A H 1.0537 0.6689 0.1977 0.037 Uiso 1 1 calc R . . C14 C 0.9595(4) 0.6818(4) 0.1014(3) 0.0282(11) Uani 1 1 d . . . C15 C 0.9923(4) 0.5925(4) 0.0599(3) 0.0371(13) Uani 1 1 d . . . H15A H 0.9266 0.5641 0.0309 0.056 Uiso 1 1 calc R . . H15B H 1.0273 0.5357 0.0895 0.056 Uiso 1 1 calc R . . H15C H 1.0447 0.6190 0.0318 0.056 Uiso 1 1 calc R . . B1 B 0.8093(4) 0.7666(4) 0.0074(3) 0.0247(12) Uani 1 1 d . . . H1 H 0.8229 0.7071 -0.0233 0.030 Uiso 1 1 calc R . . C16 C 0.6984(3) 0.8967(4) 0.1907(2) 0.0196(10) Uani 1 1 d . . . C17 C 0.7155(3) 1.0017(4) 0.1995(2) 0.0231(11) Uani 1 1 d . . . C18 C 0.7159(3) 1.0962(4) 0.2419(2) 0.0226(10) Uani 1 1 d . . . C19 C 0.7301(4) 1.1965(4) 0.2156(2) 0.0287(11) Uani 1 1 d . . . H19A H 0.7404 1.2037 0.1700 0.034 Uiso 1 1 calc R . . C20 C 0.7293(4) 1.2864(4) 0.2557(3) 0.0358(12) Uani 1 1 d . . . H20A H 0.7368 1.3556 0.2375 0.043 Uiso 1 1 calc R . . C21 C 0.7174(4) 1.2747(4) 0.3222(3) 0.0406(14) Uani 1 1 d . . . H21A H 0.7182 1.3361 0.3499 0.049 Uiso 1 1 calc R . . C22 C 0.7045(4) 1.1750(4) 0.3491(3) 0.0408(14) Uani 1 1 d . . . H22A H 0.6962 1.1681 0.3950 0.049 Uiso 1 1 calc R . . C23 C 0.7035(4) 1.0859(4) 0.3093(2) 0.0315(12) Uani 1 1 d . . . H23A H 0.6943 1.0172 0.3276 0.038 Uiso 1 1 calc R . . C24 C 0.6599(4) 0.8025(4) 0.2166(2) 0.0266(11) Uani 1 1 d . . . C25 C 0.5990(4) 0.8065(4) 0.2702(2) 0.0284(11) Uani 1 1 d . . . H25A H 0.5838 0.8738 0.2885 0.034 Uiso 1 1 calc R . . C26 C 0.5610(4) 0.7148(4) 0.2967(3) 0.0391(13) Uani 1 1 d . . . H26A H 0.5209 0.7192 0.3331 0.047 Uiso 1 1 calc R . . C27 C 0.5814(4) 0.6163(4) 0.2700(3) 0.0409(13) Uani 1 1 d . . . H27A H 0.5566 0.5530 0.2888 0.049 Uiso 1 1 calc R . . C28 C 0.6385(4) 0.6100(4) 0.2156(3) 0.0381(13) Uani 1 1 d . . . H28A H 0.6508 0.5427 0.1964 0.046 Uiso 1 1 calc R . . C29 C 0.6764(4) 0.7016(4) 0.1902(2) 0.0278(11) Uani 1 1 d . . . H29A H 0.7154 0.6965 0.1533 0.033 Uiso 1 1 calc R . . B2 B 1.2394(6) 0.9166(5) 0.4175(3) 0.0402(16) Uani 1 1 d . . . F3 F 1.2475(3) 0.9002(3) 0.48584(16) 0.0638(10) Uani 1 1 d . . . F4 F 1.2358(3) 1.0254(2) 0.40489(18) 0.0614(10) Uani 1 1 d . . . F5 F 1.1456(3) 0.8670(3) 0.38448(17) 0.0649(10) Uani 1 1 d . . . F6 F 1.3320(3) 0.8750(3) 0.39519(18) 0.0640(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 0.02254(10) 0.01995(10) 0.01596(9) -0.00089(9) 0.00513(7) -0.00029(9) F1 0.0314(14) 0.0273(16) 0.0207(14) 0.0023(11) 0.0066(12) 0.0048(11) F2 0.0278(13) 0.0278(14) 0.0249(14) -0.0028(13) 0.0081(11) -0.0022(12) N1 0.0239(19) 0.024(2) 0.0185(19) -0.0018(18) 0.0057(16) -0.0003(18) N2 0.027(2) 0.025(2) 0.021(2) -0.0010(18) 0.0056(17) 0.0033(18) C1 0.031(3) 0.025(3) 0.032(3) 0.006(2) 0.009(2) -0.004(2) C2 0.019(2) 0.027(3) 0.023(2) 0.004(2) 0.0034(19) 0.000(2) C3 0.033(3) 0.029(3) 0.027(3) 0.006(2) 0.012(2) 0.001(2) C4 0.020(2) 0.038(3) 0.014(2) -0.002(2) 0.003(2) 0.002(2) C5 0.037(3) 0.043(3) 0.025(3) -0.006(2) 0.012(2) -0.003(2) N3 0.025(2) 0.023(2) 0.020(2) 0.0000(17) 0.0062(17) 0.0014(16) N4 0.030(2) 0.019(2) 0.018(2) -0.0031(16) 0.0067(17) 0.0002(16) C6 0.025(3) 0.037(3) 0.033(3) -0.002(2) 0.007(2) 0.003(2) C7 0.023(2) 0.034(3) 0.018(2) 0.004(2) 0.005(2) 0.001(2) C8 0.026(3) 0.034(3) 0.028(3) 0.001(2) 0.004(2) -0.005(2) C9 0.032(3) 0.028(3) 0.015(2) -0.001(2) -0.002(2) -0.004(2) C10 0.037(3) 0.024(3) 0.031(3) -0.006(2) -0.001(2) 0.001(2) N5 0.024(2) 0.023(2) 0.019(2) -0.0013(17) 0.0055(17) -0.0016(16) N6 0.0215(19) 0.022(2) 0.025(2) -0.0042(17) 0.0069(17) -0.0008(16) C11 0.037(3) 0.043(3) 0.017(3) 0.003(2) 0.000(2) 0.001(2) C12 0.022(2) 0.025(3) 0.027(3) 0.006(2) 0.007(2) -0.004(2) C13 0.034(3) 0.026(3) 0.031(3) 0.007(2) 0.000(2) 0.005(2) C14 0.023(2) 0.023(3) 0.039(3) 0.003(2) 0.008(2) 0.003(2) C15 0.040(3) 0.022(3) 0.049(3) -0.003(2) 0.009(3) 0.013(2) B1 0.028(3) 0.025(3) 0.021(3) -0.007(2) 0.005(2) 0.002(2) C16 0.009(2) 0.041(3) 0.009(2) -0.003(2) 0.0004(18) 0.005(2) C17 0.016(2) 0.030(3) 0.024(3) 0.007(2) 0.004(2) 0.0009(19) C18 0.020(2) 0.031(3) 0.018(2) -0.009(2) 0.005(2) -0.001(2) C19 0.034(3) 0.028(3) 0.024(3) -0.004(2) 0.005(2) 0.003(2) C20 0.036(3) 0.028(3) 0.043(3) -0.003(2) 0.004(3) 0.003(2) C21 0.036(3) 0.043(4) 0.043(4) -0.026(3) 0.008(3) -0.001(3) C22 0.046(3) 0.050(4) 0.029(3) -0.019(3) 0.016(3) -0.013(3) C23 0.035(3) 0.036(3) 0.026(3) -0.004(2) 0.012(2) -0.010(2) C24 0.024(2) 0.029(3) 0.023(3) -0.004(2) -0.006(2) 0.004(2) C25 0.030(3) 0.032(3) 0.024(3) -0.002(2) 0.005(2) -0.009(2) C26 0.034(3) 0.052(4) 0.032(3) 0.005(3) 0.011(2) -0.012(3) C27 0.044(3) 0.038(3) 0.040(3) 0.011(3) 0.005(3) -0.015(3) C28 0.049(3) 0.024(3) 0.041(3) 0.004(2) 0.009(3) -0.001(2) C29 0.028(3) 0.031(3) 0.024(3) 0.001(2) 0.004(2) -0.003(2) B2 0.051(4) 0.033(3) 0.033(4) -0.002(3) -0.003(3) 0.007(3) F3 0.101(3) 0.054(2) 0.0332(19) 0.0040(17) 0.0009(19) -0.034(2) F4 0.078(2) 0.036(2) 0.075(3) 0.0218(18) 0.027(2) 0.0153(18) F5 0.058(2) 0.073(2) 0.055(2) -0.007(2) -0.0176(18) -0.0055(19) F6 0.056(2) 0.060(2) 0.072(3) -0.0168(19) -0.0037(19) 0.0235(18) _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 F1 1.886(2) . ? W1 F2 1.893(2) . ? W1 C17 2.037(5) . ? W1 C16 2.060(4) . ? W1 N5 2.117(3) . ? W1 N3 2.121(4) . ? W1 N1 2.196(3) . ? N1 C2 1.345(5) . ? N1 N2 1.379(5) . ? N2 C4 1.342(5) . ? N2 B1 1.558(6) . ? C1 C2 1.493(6) . ? C2 C3 1.376(6) . ? C3 C4 1.379(6) . ? C4 C5 1.494(6) . ? N3 C7 1.361(5) . ? N3 N4 1.391(5) . ? N4 C9 1.345(5) . ? N4 B1 1.531(6) . ? C6 C7 1.487(6) . ? C7 C8 1.375(6) . ? C8 C9 1.383(6) . ? C9 C10 1.495(6) . ? N5 C12 1.358(6) . ? N5 N6 1.384(5) . ? N6 C14 1.338(5) . ? N6 B1 1.550(6) . ? C11 C12 1.498(6) . ? C12 C13 1.369(6) . ? C13 C14 1.385(6) . ? C14 C15 1.490(6) . ? C16 C17 1.338(6) . ? C16 C24 1.402(6) . ? C17 C18 1.457(6) . ? C18 C19 1.385(6) . ? C18 C23 1.396(6) . ? C19 C20 1.386(6) . ? C20 C21 1.377(7) . ? C21 C22 1.379(7) . ? C22 C23 1.372(6) . ? C24 C29 1.398(6) . ? C24 C25 1.412(6) . ? C25 C26 1.379(6) . ? C26 C27 1.383(7) . ? C27 C28 1.397(7) . ? C28 C29 1.368(6) . ? B2 F3 1.377(7) . ? B2 F5 1.377(7) . ? B2 F4 1.385(7) . ? B2 F6 1.391(7) . ? 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 F1 W1 F2 101.64(11) . . ? F1 W1 C17 87.14(14) . . ? F2 W1 C17 84.35(14) . . ? F1 W1 C16 108.21(13) . . ? F2 W1 C16 110.08(14) . . ? C17 W1 C16 38.13(17) . . ? F1 W1 N5 163.06(12) . . ? F2 W1 N5 84.29(12) . . ? C17 W1 N5 109.36(16) . . ? C16 W1 N5 84.07(15) . . ? F1 W1 N3 84.90(12) . . ? F2 W1 N3 162.88(12) . . ? C17 W1 N3 111.98(15) . . ? C16 W1 N3 82.26(15) . . ? N5 W1 N3 85.30(13) . . ? F1 W1 N1 82.43(12) . . ? F2 W1 N1 82.99(11) . . ? C17 W1 N1 161.62(17) . . ? C16 W1 N1 160.25(16) . . ? N5 W1 N1 82.57(13) . . ? N3 W1 N1 82.21(13) . . ? C2 N1 N2 107.1(3) . . ? C2 N1 W1 132.2(3) . . ? N2 N1 W1 120.5(3) . . ? C4 N2 N1 109.3(4) . . ? C4 N2 B1 131.7(4) . . ? N1 N2 B1 119.0(3) . . ? N1 C2 C3 108.9(4) . . ? N1 C2 C1 122.3(4) . . ? C3 C2 C1 128.8(4) . . ? C2 C3 C4 107.2(4) . . ? N2 C4 C3 107.5(4) . . ? N2 C4 C5 122.5(4) . . ? C3 C4 C5 130.0(4) . . ? C7 N3 N4 106.8(4) . . ? C7 N3 W1 131.7(3) . . ? N4 N3 W1 121.4(3) . . ? C9 N4 N3 108.7(3) . . ? C9 N4 B1 131.4(4) . . ? N3 N4 B1 119.7(3) . . ? N3 C7 C8 109.1(4) . . ? N3 C7 C6 122.4(4) . . ? C8 C7 C6 128.5(4) . . ? C7 C8 C9 106.9(4) . . ? N4 C9 C8 108.5(4) . . ? N4 C9 C10 122.8(4) . . ? C8 C9 C10 128.7(4) . . ? C12 N5 N6 107.0(3) . . ? C12 N5 W1 131.0(3) . . ? N6 N5 W1 121.9(3) . . ? C14 N6 N5 109.2(4) . . ? C14 N6 B1 131.4(4) . . ? N5 N6 B1 119.4(3) . . ? N5 C12 C13 108.6(4) . . ? N5 C12 C11 122.8(4) . . ? C13 C12 C11 128.6(4) . . ? C12 C13 C14 107.5(4) . . ? N6 C14 C13 107.7(4) . . ? N6 C14 C15 123.2(4) . . ? C13 C14 C15 129.1(4) . . ? N4 B1 N6 109.0(4) . . ? N4 B1 N2 107.5(4) . . ? N6 B1 N2 107.2(4) . . ? C17 C16 C24 146.3(4) . . ? C17 C16 W1 70.0(3) . . ? C24 C16 W1 143.7(3) . . ? C16 C17 C18 149.3(4) . . ? C16 C17 W1 71.9(3) . . ? C18 C17 W1 138.6(3) . . ? C19 C18 C23 119.7(4) . . ? C19 C18 C17 120.1(4) . . ? C23 C18 C17 120.2(4) . . ? C18 C19 C20 120.0(5) . . ? C21 C20 C19 119.4(5) . . ? C20 C21 C22 121.0(5) . . ? C23 C22 C21 119.7(5) . . ? C22 C23 C18 120.1(5) . . ? C29 C24 C16 122.6(4) . . ? C29 C24 C25 116.8(4) . . ? C16 C24 C25 120.5(4) . . ? C26 C25 C24 121.4(5) . . ? C25 C26 C27 119.8(5) . . ? C26 C27 C28 120.1(5) . . ? C29 C28 C27 119.4(5) . . ? C28 C29 C24 122.3(5) . . ? F3 B2 F5 109.3(5) . . ? F3 B2 F4 108.9(5) . . ? F5 B2 F4 110.8(5) . . ? F3 B2 F6 109.9(5) . . ? F5 B2 F6 109.7(5) . . ? F4 B2 F6 108.2(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.839 _refine_diff_density_min -0.653 _refine_diff_density_rms 0.104 #===END data_3[SbCl6] _database_code_depnum_ccdc_archive 'CCDC 697670' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H32 B Cl7 F N6 Sb W' _chemical_formula_weight 1048.17 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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' 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 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 13.5069(18) _cell_length_b 16.1788(15) _cell_length_c 19.1244(15) _cell_angle_alpha 90.00 _cell_angle_beta 102.369(9) _cell_angle_gamma 90.00 _cell_volume 4082.2(7) _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 Block _exptl_crystal_colour Red-brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.705 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2024 _exptl_absorpt_coefficient_mu 3.968 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.518 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'omega scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 45157 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 27.49 _reflns_number_total 9360 _reflns_number_gt 8183 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0296P)^2^+5.8950P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9360 _refine_ls_number_parameters 416 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0249 _refine_ls_wR_factor_ref 0.0634 _refine_ls_wR_factor_gt 0.0615 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 W1 W 1.432631(9) 0.924039(7) 0.268067(6) 0.01437(4) Uani 1 1 d . . . F1 F 1.36193(14) 1.02592(11) 0.27261(10) 0.0233(4) Uani 1 1 d . . . Cl1 Cl 1.43705(7) 0.86822(5) 0.38022(4) 0.02816(18) Uani 1 1 d . . . N1 N 1.5601(2) 1.00013(16) 0.32508(14) 0.0209(6) Uani 1 1 d . . . N2 N 1.6513(2) 0.99943(16) 0.30407(14) 0.0211(6) Uani 1 1 d . . . C1 C 1.4863(3) 1.0728(2) 0.4182(2) 0.0377(9) Uani 1 1 d . . . H1A H 1.4252 1.0421 0.3958 0.057 Uiso 1 1 calc R . . H1B H 1.4729 1.1323 0.4128 0.057 Uiso 1 1 calc R . . H1C H 1.5052 1.0589 0.4692 0.057 Uiso 1 1 calc R . . C2 C 1.5707(3) 1.0504(2) 0.38291(18) 0.0274(8) Uani 1 1 d . . . C3 C 1.6697(3) 1.0795(2) 0.3992(2) 0.0342(9) Uani 1 1 d . . . H3A H 1.6982 1.1154 0.4375 0.041 Uiso 1 1 calc R . . C4 C 1.7192(3) 1.0468(2) 0.34972(19) 0.0287(8) Uani 1 1 d . . . C5 C 1.8271(3) 1.0559(3) 0.3431(2) 0.0435(10) Uani 1 1 d . . . H5A H 1.8378 1.0244 0.3016 0.065 Uiso 1 1 calc R . . H5B H 1.8721 1.0349 0.3866 0.065 Uiso 1 1 calc R . . H5C H 1.8418 1.1144 0.3368 0.065 Uiso 1 1 calc R . . N3 N 1.47586(19) 0.98013(15) 0.17754(13) 0.0174(5) Uani 1 1 d . . . N4 N 1.57652(19) 0.98434(15) 0.17460(13) 0.0177(5) Uani 1 1 d . . . C6 C 1.3098(3) 1.0300(2) 0.10398(18) 0.0282(8) Uani 1 1 d . . . H6A H 1.2825 1.0030 0.1417 0.042 Uiso 1 1 calc R . . H6B H 1.2796 1.0051 0.0576 0.042 Uiso 1 1 calc R . . H6C H 1.2937 1.0891 0.1028 0.042 Uiso 1 1 calc R . . C7 C 1.4218(3) 1.01896(19) 0.11884(16) 0.0210(7) Uani 1 1 d . . . C8 C 1.4888(3) 1.0474(2) 0.07843(17) 0.0254(7) Uani 1 1 d . . . H8A H 1.4717 1.0772 0.0347 0.030 Uiso 1 1 calc R . . C9 C 1.5850(3) 1.0242(2) 0.11383(17) 0.0229(7) Uani 1 1 d . . . C10 C 1.6842(3) 1.0381(2) 0.0940(2) 0.0348(9) Uani 1 1 d . . . H10A H 1.7383 1.0137 0.1306 0.052 Uiso 1 1 calc R . . H10B H 1.6960 1.0976 0.0908 0.052 Uiso 1 1 calc R . . H10C H 1.6836 1.0121 0.0476 0.052 Uiso 1 1 calc R . . N5 N 1.5427(2) 0.83598(15) 0.25604(13) 0.0180(5) Uani 1 1 d . . . N6 N 1.63784(19) 0.86008(16) 0.24873(13) 0.0191(5) Uani 1 1 d . . . C11 C 1.4567(3) 0.7001(2) 0.2699(2) 0.0298(8) Uani 1 1 d . . . H11A H 1.3983 0.7359 0.2700 0.045 Uiso 1 1 calc R . . H11B H 1.4743 0.6699 0.3153 0.045 Uiso 1 1 calc R . . H11C H 1.4398 0.6606 0.2302 0.045 Uiso 1 1 calc R . . C12 C 1.5445(3) 0.75128(19) 0.26081(17) 0.0213(7) Uani 1 1 d . . . C13 C 1.6399(3) 0.7242(2) 0.25724(18) 0.0277(8) Uani 1 1 d . . . H13A H 1.6624 0.6685 0.2593 0.033 Uiso 1 1 calc R . . C14 C 1.6969(3) 0.7936(2) 0.25016(17) 0.0233(7) Uani 1 1 d . . . C15 C 1.8072(3) 0.7993(2) 0.2475(2) 0.0344(9) Uani 1 1 d . . . H15A H 1.8254 0.8573 0.2425 0.052 Uiso 1 1 calc R . . H15B H 1.8194 0.7676 0.2064 0.052 Uiso 1 1 calc R . . H15C H 1.8486 0.7766 0.2917 0.052 Uiso 1 1 calc R . . B1 B 1.6602(3) 0.9518(2) 0.23673(19) 0.0203(7) Uani 1 1 d . . . H1 H 1.7290 0.9589 0.2259 0.024 Uiso 1 1 calc R . . C16 C 1.3386(2) 0.85543(18) 0.19233(16) 0.0165(6) Uani 1 1 d . . . C17 C 1.2945(2) 0.86795(18) 0.24601(16) 0.0183(6) Uani 1 1 d . . . C18 C 1.2116(2) 0.8511(2) 0.28062(17) 0.0231(7) Uani 1 1 d . . . C19 C 1.1904(3) 0.9049(2) 0.33244(19) 0.0304(8) Uani 1 1 d . . . H19A H 1.2297 0.9536 0.3443 0.037 Uiso 1 1 calc R . . C20 C 1.1122(3) 0.8877(3) 0.3668(2) 0.0435(10) Uani 1 1 d . . . H20A H 1.0966 0.9254 0.4009 0.052 Uiso 1 1 calc R . . C21 C 1.0575(3) 0.8164(3) 0.3513(2) 0.0507(13) Uani 1 1 d . . . H21A H 1.0049 0.8044 0.3758 0.061 Uiso 1 1 calc R . . C22 C 1.0774(3) 0.7612(3) 0.3006(2) 0.0496(12) Uani 1 1 d . . . H22A H 1.0394 0.7115 0.2910 0.059 Uiso 1 1 calc R . . C23 C 1.1539(3) 0.7793(3) 0.26354(19) 0.0335(9) Uani 1 1 d . . . H23A H 1.1664 0.7431 0.2273 0.040 Uiso 1 1 calc R . . C24 C 1.3251(2) 0.82052(19) 0.12087(16) 0.0190(6) Uani 1 1 d . . . C25 C 1.2273(3) 0.8000(2) 0.08411(17) 0.0233(7) Uani 1 1 d . . . H25A H 1.1718 0.8066 0.1069 0.028 Uiso 1 1 calc R . . C26 C 1.2105(3) 0.7702(2) 0.01450(18) 0.0291(8) Uani 1 1 d . . . H26A H 1.1436 0.7578 -0.0107 0.035 Uiso 1 1 calc R . . C27 C 1.2918(3) 0.7586(2) -0.01815(17) 0.0302(8) Uani 1 1 d . . . H27A H 1.2806 0.7377 -0.0656 0.036 Uiso 1 1 calc R . . C28 C 1.3894(3) 0.7772(2) 0.01822(18) 0.0284(8) Uani 1 1 d . . . H28A H 1.4449 0.7685 -0.0042 0.034 Uiso 1 1 calc R . . C29 C 1.4064(3) 0.80875(19) 0.08734(17) 0.0222(7) Uani 1 1 d . . . H29A H 1.4733 0.8223 0.1118 0.027 Uiso 1 1 calc R . . Sb1 Sb 0.826741(17) 0.794548(14) 0.525125(12) 0.02298(6) Uani 1 1 d . . . Cl2 Cl 0.71293(8) 0.69219(7) 0.55206(6) 0.0441(2) Uani 1 1 d . . . Cl3 Cl 0.86588(11) 0.70681(7) 0.43558(6) 0.0557(3) Uani 1 1 d . . . Cl4 Cl 0.96062(8) 0.73326(9) 0.60892(6) 0.0582(3) Uani 1 1 d . . . Cl5 Cl 0.69405(10) 0.85256(10) 0.44104(7) 0.0730(4) Uani 1 1 d . . . Cl6 Cl 0.79029(11) 0.87770(7) 0.61691(7) 0.0572(3) Uani 1 1 d . . . Cl7 Cl 0.94101(10) 0.89547(8) 0.49915(6) 0.0539(3) 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 0.01637(7) 0.01429(6) 0.01194(6) -0.00012(4) 0.00187(4) -0.00110(5) F1 0.0279(10) 0.0191(9) 0.0226(9) 0.0018(7) 0.0050(8) 0.0018(8) Cl1 0.0307(5) 0.0318(4) 0.0206(4) 0.0032(3) 0.0024(3) -0.0043(3) N1 0.0249(15) 0.0197(13) 0.0170(12) -0.0015(10) 0.0020(10) -0.0043(11) N2 0.0189(14) 0.0201(13) 0.0223(13) 0.0018(10) 0.0002(11) -0.0051(11) C1 0.048(3) 0.037(2) 0.0278(19) -0.0146(16) 0.0089(17) -0.0059(18) C2 0.035(2) 0.0221(16) 0.0216(16) -0.0032(13) -0.0010(14) -0.0040(15) C3 0.042(2) 0.0269(18) 0.0277(18) -0.0077(14) -0.0058(16) -0.0089(16) C4 0.0298(19) 0.0209(16) 0.0292(18) 0.0004(14) -0.0077(15) -0.0058(14) C5 0.031(2) 0.041(2) 0.053(3) -0.0061(19) -0.0030(19) -0.0148(18) N3 0.0186(13) 0.0181(12) 0.0158(12) 0.0032(10) 0.0041(10) -0.0006(10) N4 0.0181(13) 0.0180(12) 0.0177(12) 0.0025(10) 0.0054(10) -0.0024(10) C6 0.0286(19) 0.0320(19) 0.0216(16) 0.0085(14) -0.0001(14) 0.0087(15) C7 0.0285(18) 0.0170(14) 0.0159(14) 0.0020(11) 0.0012(12) 0.0043(13) C8 0.036(2) 0.0227(16) 0.0179(15) 0.0044(12) 0.0077(14) 0.0025(15) C9 0.0308(19) 0.0188(15) 0.0212(15) 0.0030(12) 0.0101(13) -0.0020(13) C10 0.035(2) 0.039(2) 0.036(2) 0.0103(17) 0.0184(17) -0.0011(17) N5 0.0182(13) 0.0165(12) 0.0183(12) 0.0021(10) 0.0018(10) -0.0017(10) N6 0.0149(13) 0.0219(13) 0.0199(13) 0.0007(10) 0.0023(10) -0.0001(11) C11 0.035(2) 0.0160(15) 0.038(2) 0.0044(14) 0.0063(16) -0.0026(14) C12 0.0268(18) 0.0162(14) 0.0200(15) 0.0001(12) 0.0026(13) 0.0006(13) C13 0.0312(19) 0.0212(16) 0.0292(17) 0.0032(13) 0.0026(14) 0.0086(14) C14 0.0238(17) 0.0256(16) 0.0194(15) 0.0004(12) 0.0018(13) 0.0066(13) C15 0.0223(19) 0.042(2) 0.038(2) 0.0011(17) 0.0055(15) 0.0084(16) B1 0.0156(17) 0.0222(17) 0.0224(17) 0.0024(14) 0.0023(14) -0.0027(14) C16 0.0136(15) 0.0162(14) 0.0188(14) 0.0025(11) 0.0014(11) 0.0017(11) C17 0.0169(15) 0.0173(14) 0.0198(14) 0.0017(11) 0.0020(12) 0.0023(12) C18 0.0161(16) 0.0330(18) 0.0203(15) 0.0050(13) 0.0040(12) -0.0016(13) C19 0.0259(19) 0.039(2) 0.0286(18) 0.0011(15) 0.0108(15) 0.0047(15) C20 0.029(2) 0.071(3) 0.033(2) 0.004(2) 0.0127(17) 0.012(2) C21 0.022(2) 0.099(4) 0.031(2) 0.021(2) 0.0052(16) -0.005(2) C22 0.029(2) 0.077(3) 0.039(2) 0.015(2) -0.0011(18) -0.025(2) C23 0.0229(19) 0.048(2) 0.0273(18) 0.0013(16) 0.0004(14) -0.0126(17) C24 0.0207(16) 0.0182(14) 0.0171(14) -0.0003(11) 0.0019(12) 0.0002(12) C25 0.0206(17) 0.0257(16) 0.0216(16) -0.0022(13) 0.0001(13) 0.0001(13) C26 0.032(2) 0.0275(17) 0.0225(16) -0.0048(13) -0.0059(14) 0.0001(15) C27 0.051(2) 0.0236(17) 0.0137(15) -0.0016(12) 0.0008(15) -0.0033(16) C28 0.039(2) 0.0248(17) 0.0238(17) -0.0005(13) 0.0132(15) 0.0002(15) C29 0.0256(18) 0.0206(15) 0.0198(15) -0.0006(12) 0.0036(13) -0.0028(13) Sb1 0.01927(11) 0.02618(11) 0.02266(11) 0.00055(8) 0.00263(8) -0.00075(9) Cl2 0.0418(6) 0.0512(6) 0.0412(5) -0.0036(4) 0.0133(4) -0.0212(5) Cl3 0.0796(9) 0.0485(6) 0.0509(6) -0.0205(5) 0.0403(6) -0.0210(6) Cl4 0.0259(5) 0.0937(9) 0.0521(6) 0.0242(6) 0.0019(5) 0.0171(6) Cl5 0.0547(8) 0.0879(10) 0.0642(8) 0.0333(7) -0.0141(6) 0.0168(7) Cl6 0.0765(9) 0.0434(6) 0.0611(7) -0.0198(5) 0.0357(6) -0.0013(6) Cl7 0.0655(8) 0.0514(6) 0.0499(6) -0.0063(5) 0.0237(6) -0.0322(6) _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 F1 1.9162(18) . ? W1 C17 2.035(3) . ? W1 C16 2.038(3) . ? W1 N5 2.107(3) . ? W1 N3 2.144(2) . ? W1 N1 2.206(3) . ? W1 Cl1 2.3161(8) . ? N1 C2 1.356(4) . ? N1 N2 1.375(4) . ? N2 C4 1.359(4) . ? N2 B1 1.527(5) . ? C1 C2 1.489(6) . ? C2 C3 1.389(5) . ? C3 C4 1.375(6) . ? C4 C5 1.496(6) . ? N3 C7 1.355(4) . ? N3 N4 1.374(4) . ? N4 C9 1.356(4) . ? N4 B1 1.546(4) . ? C6 C7 1.488(5) . ? C7 C8 1.388(5) . ? C8 C9 1.383(5) . ? C9 C10 1.484(5) . ? N5 C12 1.373(4) . ? N5 N6 1.379(4) . ? N6 C14 1.336(4) . ? N6 B1 1.542(4) . ? C11 C12 1.486(5) . ? C12 C13 1.377(5) . ? C13 C14 1.383(5) . ? C14 C15 1.504(5) . ? C16 C17 1.308(4) . ? C16 C24 1.453(4) . ? C17 C18 1.444(4) . ? C18 C19 1.394(5) . ? C18 C23 1.398(5) . ? C19 C20 1.386(5) . ? C20 C21 1.368(7) . ? C21 C22 1.386(7) . ? C22 C23 1.404(6) . ? C24 C25 1.397(4) . ? C24 C29 1.399(5) . ? C25 C26 1.388(5) . ? C26 C27 1.388(5) . ? C27 C28 1.385(5) . ? C28 C29 1.389(4) . ? Sb1 Cl5 2.3333(11) . ? Sb1 Cl6 2.3460(11) . ? Sb1 Cl4 2.3621(10) . ? Sb1 Cl3 2.3696(11) . ? Sb1 Cl7 2.3714(11) . ? Sb1 Cl2 2.3896(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 F1 W1 C17 87.10(10) . . ? F1 W1 C16 105.07(10) . . ? C17 W1 C16 37.47(12) . . ? F1 W1 N5 163.09(9) . . ? C17 W1 N5 108.20(11) . . ? C16 W1 N5 84.30(11) . . ? F1 W1 N3 84.09(9) . . ? C17 W1 N3 114.67(11) . . ? C16 W1 N3 83.83(11) . . ? N5 W1 N3 82.97(10) . . ? F1 W1 N1 80.87(9) . . ? C17 W1 N1 159.22(11) . . ? C16 W1 N1 163.08(11) . . ? N5 W1 N1 86.40(10) . . ? N3 W1 N1 81.03(10) . . ? F1 W1 Cl1 101.98(6) . . ? C17 W1 Cl1 81.88(9) . . ? C16 W1 Cl1 109.54(9) . . ? N5 W1 Cl1 87.63(7) . . ? N3 W1 Cl1 162.85(7) . . ? N1 W1 Cl1 84.11(7) . . ? C2 N1 N2 107.4(3) . . ? C2 N1 W1 132.3(2) . . ? N2 N1 W1 120.29(19) . . ? C4 N2 N1 109.3(3) . . ? C4 N2 B1 131.5(3) . . ? N1 N2 B1 119.2(2) . . ? N1 C2 C3 108.3(3) . . ? N1 C2 C1 124.0(3) . . ? C3 C2 C1 127.6(3) . . ? C4 C3 C2 107.6(3) . . ? N2 C4 C3 107.4(3) . . ? N2 C4 C5 122.4(3) . . ? C3 C4 C5 130.2(3) . . ? C7 N3 N4 107.8(2) . . ? C7 N3 W1 132.3(2) . . ? N4 N3 W1 119.80(18) . . ? C9 N4 N3 109.0(2) . . ? C9 N4 B1 129.7(3) . . ? N3 N4 B1 121.2(2) . . ? N3 C7 C8 108.3(3) . . ? N3 C7 C6 124.0(3) . . ? C8 C7 C6 127.6(3) . . ? C9 C8 C7 107.1(3) . . ? N4 C9 C8 107.8(3) . . ? N4 C9 C10 122.5(3) . . ? C8 C9 C10 129.7(3) . . ? C12 N5 N6 106.6(3) . . ? C12 N5 W1 132.1(2) . . ? N6 N5 W1 120.98(19) . . ? C14 N6 N5 109.6(3) . . ? C14 N6 B1 130.0(3) . . ? N5 N6 B1 120.3(2) . . ? N5 C12 C13 108.5(3) . . ? N5 C12 C11 124.1(3) . . ? C13 C12 C11 127.4(3) . . ? C12 C13 C14 107.1(3) . . ? N6 C14 C13 108.2(3) . . ? N6 C14 C15 122.8(3) . . ? C13 C14 C15 129.0(3) . . ? N2 B1 N6 107.8(3) . . ? N2 B1 N4 107.5(3) . . ? N6 B1 N4 107.9(2) . . ? C17 C16 C24 144.2(3) . . ? C17 C16 W1 71.15(19) . . ? C24 C16 W1 144.5(2) . . ? C16 C17 C18 149.2(3) . . ? C16 C17 W1 71.38(19) . . ? C18 C17 W1 139.1(2) . . ? C19 C18 C23 119.8(3) . . ? C19 C18 C17 120.4(3) . . ? C23 C18 C17 119.8(3) . . ? C20 C19 C18 120.3(4) . . ? C21 C20 C19 119.9(4) . . ? C20 C21 C22 121.1(4) . . ? C21 C22 C23 119.6(4) . . ? C18 C23 C22 119.2(4) . . ? C25 C24 C29 119.2(3) . . ? C25 C24 C16 118.7(3) . . ? C29 C24 C16 122.0(3) . . ? C26 C25 C24 120.5(3) . . ? C27 C26 C25 119.8(3) . . ? C28 C27 C26 120.3(3) . . ? C27 C28 C29 120.2(3) . . ? C28 C29 C24 120.0(3) . . ? Cl5 Sb1 Cl6 91.82(6) . . ? Cl5 Sb1 Cl4 178.83(6) . . ? Cl6 Sb1 Cl4 89.20(5) . . ? Cl5 Sb1 Cl3 90.01(6) . . ? Cl6 Sb1 Cl3 177.91(5) . . ? Cl4 Sb1 Cl3 88.97(5) . . ? Cl5 Sb1 Cl7 90.97(5) . . ? Cl6 Sb1 Cl7 90.70(4) . . ? Cl4 Sb1 Cl7 89.60(5) . . ? Cl3 Sb1 Cl7 90.29(4) . . ? Cl5 Sb1 Cl2 89.58(5) . . ? Cl6 Sb1 Cl2 89.33(4) . . ? Cl4 Sb1 Cl2 89.84(4) . . ? Cl3 Sb1 Cl2 89.66(4) . . ? Cl7 Sb1 Cl2 179.44(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.749 _refine_diff_density_min -0.981 _refine_diff_density_rms 0.107 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.000 263.6 98.7 2 0.000 0.500 0.500 263.6 98.1 _platon_squeeze_details ; ; #===END data_4[SbCl6] _database_code_depnum_ccdc_archive 'CCDC 697671' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H31.91 B Cl2.09 N6 W, Cl6 Sb' _chemical_formula_sum 'C29 H31.91 B Cl8.09 N6 Sb W' _chemical_formula_weight 1067.63 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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 10.2104(13) _cell_length_b 16.872(2) _cell_length_c 22.063(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.636(2) _cell_angle_gamma 90.00 _cell_volume 3775.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 201 _cell_measurement_theta_min 2.587 _cell_measurement_theta_max 29.9585 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.878 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2062 _exptl_absorpt_coefficient_mu 4.363 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.520 _exptl_absorpt_correction_T_max 0.647 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 24085 _diffrn_reflns_av_R_equivalents 0.0612 _diffrn_reflns_av_sigmaI/netI 0.0806 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8670 _reflns_number_gt 5855 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 1998)' _computing_cell_refinement 'Bruker SMART (Bruker, 1998)' _computing_data_reduction 'Bruker SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1998)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1998)' _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^)+(0.0202P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8670 _refine_ls_number_parameters 428 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0764 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.0716 _refine_ls_wR_factor_gt 0.0622 _refine_ls_goodness_of_fit_ref 0.958 _refine_ls_restrained_S_all 0.958 _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 0.413002(19) 0.839048(11) 0.849023(10) 0.02021(6) Uani 1 1 d . . . Cl1 Cl 0.61488(12) 0.86867(8) 0.90245(6) 0.0308(3) Uani 1 1 d . . . Cl2 Cl 0.45671(13) 0.85242(7) 0.74792(6) 0.0285(3) Uani 1 1 d . . . N1 N 0.5026(4) 0.7200(2) 0.84076(19) 0.0222(10) Uani 1 1 d . . . N2 N 0.4369(4) 0.6536(2) 0.85695(19) 0.0234(10) Uani 1 1 d . . . C1 C 0.7241(5) 0.7460(3) 0.8037(3) 0.0366(15) Uani 1 1 d . . . H1A H 0.6833 0.7940 0.7850 0.055 Uiso 1 1 calc R . . H1B H 0.7691 0.7173 0.7735 0.055 Uiso 1 1 calc R . . H1C H 0.7881 0.7607 0.8384 0.055 Uiso 1 1 calc R . . C2 C 0.6204(5) 0.6944(3) 0.8251(2) 0.0275(12) Uani 1 1 d . A . C3 C 0.6273(5) 0.6137(3) 0.8308(2) 0.0334(14) Uani 1 1 d . . . H3A H 0.6990 0.5812 0.8225 0.040 Uiso 0.911(5) 1 calc PR A 1 Cl3 Cl 0.7319(5) 0.5416(3) 0.8174(2) 0.049(7) Uani 0.089(5) 1 d PR A 2 C4 C 0.5109(5) 0.5880(3) 0.8511(2) 0.0281(13) Uani 1 1 d . A . C5 C 0.4676(5) 0.5070(3) 0.8658(3) 0.0384(15) Uani 1 1 d . . . H5A H 0.3894 0.4925 0.8379 0.058 Uiso 1 1 calc R A . H5B H 0.4460 0.5056 0.9079 0.058 Uiso 1 1 calc R . . H5C H 0.5387 0.4692 0.8612 0.058 Uiso 1 1 calc R . . N3 N 0.2358(4) 0.7807(2) 0.81167(19) 0.0229(10) Uani 1 1 d . . . N4 N 0.2091(4) 0.7043(2) 0.82995(18) 0.0205(9) Uani 1 1 d . . . C6 C 0.1274(5) 0.8789(3) 0.7343(3) 0.0343(14) Uani 1 1 d . . . H6A H 0.1343 0.9223 0.7640 0.051 Uiso 1 1 calc R . . H6B H 0.0427 0.8823 0.7086 0.051 Uiso 1 1 calc R . . H6C H 0.1995 0.8828 0.7087 0.051 Uiso 1 1 calc R . . C7 C 0.1362(5) 0.8010(3) 0.7675(2) 0.0251(12) Uani 1 1 d . . . C8 C 0.0503(5) 0.7386(3) 0.7580(2) 0.0264(12) Uani 1 1 d . . . H8A H -0.0269 0.7367 0.7295 0.032 Uiso 1 1 calc R . . C9 C 0.0967(5) 0.6791(3) 0.7977(2) 0.0263(12) Uani 1 1 d . . . C10 C 0.0388(5) 0.5989(3) 0.8082(3) 0.0360(14) Uani 1 1 d . . . H10A H 0.1059 0.5580 0.8053 0.054 Uiso 1 1 calc R . . H10B H -0.0364 0.5892 0.7773 0.054 Uiso 1 1 calc R . . H10C H 0.0092 0.5974 0.8489 0.054 Uiso 1 1 calc R . . N5 N 0.3589(4) 0.7939(2) 0.93198(19) 0.0212(9) Uani 1 1 d . . . N6 N 0.3188(4) 0.7157(2) 0.93692(18) 0.0197(9) Uani 1 1 d . . . C11 C 0.4023(5) 0.9085(3) 1.0056(3) 0.0307(13) Uani 1 1 d . . . H11A H 0.3525 0.9452 0.9772 0.046 Uiso 1 1 calc R . . H11B H 0.4968 0.9146 1.0026 0.046 Uiso 1 1 calc R . . H11C H 0.3844 0.9202 1.0473 0.046 Uiso 1 1 calc R . . C12 C 0.3614(4) 0.8252(3) 0.9896(2) 0.0234(12) Uani 1 1 d . . . C13 C 0.3263(5) 0.7675(3) 1.0289(2) 0.0261(12) Uani 1 1 d . . . H13A H 0.3209 0.7731 1.0714 0.031 Uiso 1 1 calc R . . C14 C 0.3007(5) 0.6999(3) 0.9943(2) 0.0233(12) Uani 1 1 d . . . C15 C 0.2614(5) 0.6195(3) 1.0150(3) 0.0312(13) Uani 1 1 d . . . H15A H 0.1763 0.6046 0.9927 0.047 Uiso 1 1 calc R . . H15B H 0.2538 0.6209 1.0588 0.047 Uiso 1 1 calc R . . H15C H 0.3284 0.5806 1.0068 0.047 Uiso 1 1 calc R . . B1 B 0.3026(5) 0.6627(3) 0.8795(3) 0.0225(13) Uani 1 1 d . . . H1 H 0.2665 0.6097 0.8893 0.027 Uiso 1 1 calc R . . C16 C 0.2892(5) 0.9296(3) 0.8637(2) 0.0218(11) Uani 1 1 d . . . C17 C 0.3951(5) 0.9592(3) 0.8441(2) 0.0213(11) Uani 1 1 d . . . C18 C 0.4707(5) 1.0277(3) 0.8300(2) 0.0217(11) Uani 1 1 d . . . C19 C 0.5949(5) 1.0192(3) 0.8087(2) 0.0287(13) Uani 1 1 d . . . H19A H 0.6286 0.9678 0.8021 0.034 Uiso 1 1 calc R . . C20 C 0.6665(5) 1.0847(3) 0.7976(3) 0.0332(14) Uani 1 1 d . . . H20A H 0.7501 1.0783 0.7832 0.040 Uiso 1 1 calc R . . C21 C 0.6198(5) 1.1601(3) 0.8068(2) 0.0318(13) Uani 1 1 d . . . H21A H 0.6713 1.2050 0.7990 0.038 Uiso 1 1 calc R . . C22 C 0.4983(5) 1.1700(3) 0.8273(2) 0.0307(13) Uani 1 1 d . . . H22A H 0.4659 1.2218 0.8334 0.037 Uiso 1 1 calc R . . C23 C 0.4240(5) 1.1052(3) 0.8391(2) 0.0277(13) Uani 1 1 d . . . H23A H 0.3407 1.1125 0.8534 0.033 Uiso 1 1 calc R . . C24 C 0.1595(5) 0.9457(3) 0.8835(2) 0.0252(12) Uani 1 1 d . . . C25 C 0.1090(5) 1.0229(3) 0.8817(3) 0.0434(17) Uani 1 1 d . . . H25A H 0.1585 1.0649 0.8669 0.052 Uiso 1 1 calc R . . C26 C -0.0121(6) 1.0385(3) 0.9011(4) 0.058(2) Uani 1 1 d . . . H26A H -0.0456 1.0911 0.8995 0.070 Uiso 1 1 calc R . . C27 C -0.0846(5) 0.9782(3) 0.9229(3) 0.0476(18) Uani 1 1 d . . . H27A H -0.1670 0.9895 0.9371 0.057 Uiso 1 1 calc R . . C28 C -0.0379(5) 0.9016(3) 0.9242(3) 0.0387(15) Uani 1 1 d . . . H28A H -0.0884 0.8598 0.9388 0.046 Uiso 1 1 calc R . . C29 C 0.0835(5) 0.8855(3) 0.9043(3) 0.0287(13) Uani 1 1 d . . . H29A H 0.1149 0.8325 0.9048 0.034 Uiso 1 1 calc R . . Sb1 Sb 0.83424(3) 0.67515(2) 0.052758(16) 0.02586(9) Uani 1 1 d . . . Cl4 Cl 0.73845(16) 0.80235(9) 0.04153(7) 0.0484(4) Uani 1 1 d . . . Cl5 Cl 0.75994(14) 0.66576(9) 0.15088(6) 0.0397(3) Uani 1 1 d . . . Cl6 Cl 0.63661(15) 0.61838(11) 0.00705(8) 0.0534(4) Uani 1 1 d . . . Cl7 Cl 0.93323(15) 0.54958(8) 0.06765(7) 0.0421(4) Uani 1 1 d . . . Cl8 Cl 0.91154(14) 0.68553(8) -0.04413(6) 0.0392(4) Uani 1 1 d . . . Cl9 Cl 1.03200(13) 0.73593(8) 0.09769(7) 0.0348(3) 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 0.02136(11) 0.01839(10) 0.02099(12) 0.00134(10) 0.00290(8) -0.00089(9) Cl1 0.0235(7) 0.0344(7) 0.0338(9) 0.0041(6) -0.0002(6) -0.0047(6) Cl2 0.0376(8) 0.0250(7) 0.0243(8) 0.0016(5) 0.0101(6) 0.0002(6) N1 0.022(2) 0.020(2) 0.026(3) 0.0032(19) 0.0053(19) 0.0034(18) N2 0.029(2) 0.020(2) 0.022(3) 0.0033(19) 0.0064(19) 0.0023(19) C1 0.024(3) 0.046(4) 0.040(4) 0.007(3) 0.005(3) 0.010(3) C2 0.028(3) 0.035(3) 0.020(3) 0.004(2) 0.006(2) 0.007(2) C3 0.041(4) 0.029(3) 0.031(4) 0.002(3) 0.004(3) 0.012(3) Cl3 0.034(11) 0.045(11) 0.070(16) -0.002(9) 0.006(9) 0.013(8) C4 0.040(3) 0.023(3) 0.020(3) 0.000(2) 0.001(3) 0.006(2) C5 0.054(4) 0.024(3) 0.038(4) -0.003(3) 0.009(3) 0.011(3) N3 0.023(2) 0.020(2) 0.026(3) 0.0000(19) 0.0039(19) 0.0005(18) N4 0.027(2) 0.016(2) 0.019(2) -0.0007(18) 0.0008(19) -0.0016(18) C6 0.036(3) 0.028(3) 0.037(4) 0.007(3) -0.005(3) 0.000(3) C7 0.028(3) 0.024(3) 0.022(3) 0.000(2) 0.000(2) 0.002(2) C8 0.023(3) 0.031(3) 0.023(3) 0.000(2) -0.003(2) -0.001(2) C9 0.027(3) 0.026(3) 0.027(3) -0.002(2) 0.006(2) -0.004(2) C10 0.037(3) 0.035(3) 0.034(4) -0.001(3) 0.001(3) -0.018(3) N5 0.024(2) 0.016(2) 0.023(3) -0.0027(18) 0.0022(19) -0.0026(17) N6 0.025(2) 0.018(2) 0.017(2) 0.0021(18) 0.0057(18) -0.0006(17) C11 0.030(3) 0.029(3) 0.033(4) -0.006(3) 0.004(3) -0.006(2) C12 0.016(3) 0.029(3) 0.024(3) -0.005(2) 0.000(2) 0.000(2) C13 0.036(3) 0.034(3) 0.008(3) -0.001(2) 0.000(2) -0.006(2) C14 0.024(3) 0.027(3) 0.019(3) 0.003(2) 0.003(2) 0.002(2) C15 0.040(3) 0.025(3) 0.029(3) 0.009(2) 0.007(3) -0.004(2) B1 0.029(3) 0.017(3) 0.022(3) -0.002(3) 0.006(3) 0.000(3) C16 0.031(3) 0.014(2) 0.019(3) 0.001(2) -0.001(2) 0.000(2) C17 0.025(3) 0.021(3) 0.019(3) 0.003(2) 0.002(2) -0.001(2) C18 0.027(3) 0.023(3) 0.014(3) 0.003(2) 0.001(2) -0.005(2) C19 0.032(3) 0.026(3) 0.028(3) 0.003(2) 0.004(2) -0.007(2) C20 0.028(3) 0.037(3) 0.036(4) 0.007(3) 0.012(3) -0.004(3) C21 0.040(3) 0.024(3) 0.031(3) 0.001(3) 0.007(3) -0.010(3) C22 0.040(3) 0.020(3) 0.033(4) -0.005(2) 0.010(3) -0.003(2) C23 0.031(3) 0.022(3) 0.030(4) 0.002(2) 0.005(3) -0.001(2) C24 0.021(3) 0.021(3) 0.034(4) -0.002(2) 0.002(2) 0.000(2) C25 0.028(3) 0.020(3) 0.083(5) -0.004(3) 0.010(3) -0.005(2) C26 0.031(4) 0.028(3) 0.118(7) -0.013(4) 0.015(4) 0.003(3) C27 0.022(3) 0.040(4) 0.084(6) -0.015(4) 0.022(3) -0.004(3) C28 0.031(3) 0.033(3) 0.053(4) -0.001(3) 0.011(3) -0.005(3) C29 0.027(3) 0.023(3) 0.036(4) -0.001(2) 0.003(3) 0.002(2) Sb1 0.0301(2) 0.0273(2) 0.0203(2) -0.00095(15) 0.00342(15) -0.00088(15) Cl4 0.0620(11) 0.0436(9) 0.0395(10) 0.0033(7) 0.0056(8) 0.0234(8) Cl5 0.0417(8) 0.0543(9) 0.0249(8) 0.0001(7) 0.0122(6) -0.0061(7) Cl6 0.0397(9) 0.0787(12) 0.0401(11) -0.0066(9) -0.0030(7) -0.0184(8) Cl7 0.0590(10) 0.0234(7) 0.0450(10) 0.0026(7) 0.0104(8) 0.0017(7) Cl8 0.0536(10) 0.0429(9) 0.0228(8) 0.0019(6) 0.0116(7) 0.0025(7) Cl9 0.0360(8) 0.0331(8) 0.0347(9) -0.0011(6) 0.0020(6) -0.0081(6) _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 C16 2.033(5) . ? W1 C17 2.037(5) . ? W1 N5 2.114(4) . ? W1 N3 2.139(4) . ? W1 N1 2.224(4) . ? W1 Cl1 2.3080(13) . ? W1 Cl2 2.3358(13) . ? N1 C2 1.360(6) . ? N1 N2 1.374(5) . ? N2 C4 1.354(6) . ? N2 B1 1.520(6) . ? C1 C2 1.489(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.369(7) . ? C3 C4 1.387(7) . ? C3 Cl3 1.6677 . ? C3 H3A 0.9500 . ? C4 C5 1.485(7) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? N3 C7 1.368(6) . ? N3 N4 1.387(5) . ? N4 C9 1.348(6) . ? N4 B1 1.536(7) . ? C6 C7 1.502(7) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.370(7) . ? C8 C9 1.380(7) . ? C8 H8A 0.9500 . ? C9 C10 1.505(6) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? N5 C12 1.373(6) . ? N5 N6 1.390(5) . ? N6 C14 1.327(6) . ? N6 B1 1.544(7) . ? C11 C12 1.497(6) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.378(6) . ? C13 C14 1.379(7) . ? C13 H13A 0.9500 . ? C14 C15 1.501(6) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? B1 H1 1.0000 . ? C16 C17 1.308(6) . ? C16 C24 1.467(6) . ? C17 C18 1.444(6) . ? C18 C19 1.410(6) . ? C18 C23 1.414(6) . ? C19 C20 1.363(6) . ? C19 H19A 0.9500 . ? C20 C21 1.382(7) . ? C20 H20A 0.9500 . ? C21 C22 1.380(7) . ? C21 H21A 0.9500 . ? C22 C23 1.372(6) . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? C24 C29 1.387(6) . ? C24 C25 1.399(7) . ? C25 C26 1.381(7) . ? C25 H25A 0.9500 . ? C26 C27 1.377(8) . ? C26 H26A 0.9500 . ? C27 C28 1.378(7) . ? C27 H27A 0.9500 . ? C28 C29 1.389(7) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? Sb1 Cl6 2.3528(15) . ? Sb1 Cl7 2.3540(14) . ? Sb1 Cl4 2.3598(15) . ? Sb1 Cl8 2.3692(14) . ? Sb1 Cl9 2.3768(14) . ? Sb1 Cl5 2.3805(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 C16 W1 C17 37.51(17) . . ? C16 W1 N5 84.47(17) . . ? C17 W1 N5 111.95(17) . . ? C16 W1 N3 83.86(17) . . ? C17 W1 N3 111.73(17) . . ? N5 W1 N3 82.76(15) . . ? C16 W1 N1 164.04(16) . . ? C17 W1 N1 158.43(16) . . ? N5 W1 N1 84.07(14) . . ? N3 W1 N1 83.71(14) . . ? C16 W1 Cl1 106.94(15) . . ? C17 W1 Cl1 83.19(14) . . ? N5 W1 Cl1 86.74(11) . . ? N3 W1 Cl1 164.17(11) . . ? N1 W1 Cl1 83.45(11) . . ? C16 W1 Cl2 105.67(14) . . ? C17 W1 Cl2 83.04(14) . . ? N5 W1 Cl2 163.65(11) . . ? N3 W1 Cl2 85.58(11) . . ? N1 W1 Cl2 83.29(11) . . ? Cl1 W1 Cl2 102.06(5) . . ? C2 N1 N2 106.3(4) . . ? C2 N1 W1 133.8(3) . . ? N2 N1 W1 119.8(3) . . ? C4 N2 N1 110.3(4) . . ? C4 N2 B1 130.5(4) . . ? N1 N2 B1 119.2(4) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 109.2(5) . . ? N1 C2 C1 125.3(5) . . ? C3 C2 C1 125.5(5) . . ? C2 C3 C4 107.7(5) . . ? C2 C3 Cl3 137.5(3) . . ? C4 C3 Cl3 114.8(3) . . ? C2 C3 H3A 126.2 . . ? C4 C3 H3A 126.2 . . ? N2 C4 C3 106.5(4) . . ? N2 C4 C5 123.2(5) . . ? C3 C4 C5 130.3(5) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 N3 N4 106.5(4) . . ? C7 N3 W1 133.3(3) . . ? N4 N3 W1 120.1(3) . . ? C9 N4 N3 108.9(4) . . ? C9 N4 B1 130.7(4) . . ? N3 N4 B1 120.3(4) . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N3 C7 C8 109.2(4) . . ? N3 C7 C6 124.3(4) . . ? C8 C7 C6 126.6(5) . . ? C7 C8 C9 107.1(5) . . ? C7 C8 H8A 126.4 . . ? C9 C8 H8A 126.4 . . ? N4 C9 C8 108.3(4) . . ? N4 C9 C10 121.9(5) . . ? C8 C9 C10 129.8(5) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 N5 N6 105.4(4) . . ? C12 N5 W1 133.2(3) . . ? N6 N5 W1 121.2(3) . . ? C14 N6 N5 109.8(4) . . ? C14 N6 B1 130.8(4) . . ? N5 N6 B1 119.4(4) . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N5 C12 C13 109.4(4) . . ? N5 C12 C11 123.6(4) . . ? C13 C12 C11 126.9(5) . . ? C12 C13 C14 106.4(5) . . ? C12 C13 H13A 126.8 . . ? C14 C13 H13A 126.8 . . ? N6 C14 C13 108.9(4) . . ? N6 C14 C15 122.8(5) . . ? C13 C14 C15 128.3(5) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N2 B1 N4 108.9(4) . . ? N2 B1 N6 108.2(4) . . ? N4 B1 N6 108.6(4) . . ? N2 B1 H1 110.4 . . ? N4 B1 H1 110.4 . . ? N6 B1 H1 110.4 . . ? C17 C16 C24 146.8(5) . . ? C17 C16 W1 71.4(3) . . ? C24 C16 W1 141.8(3) . . ? C16 C17 C18 149.2(5) . . ? C16 C17 W1 71.1(3) . . ? C18 C17 W1 139.6(4) . . ? C19 C18 C23 118.2(4) . . ? C19 C18 C17 121.0(4) . . ? C23 C18 C17 120.8(4) . . ? C20 C19 C18 120.0(5) . . ? C20 C19 H19A 120.0 . . ? C18 C19 H19A 120.0 . . ? C19 C20 C21 121.2(5) . . ? C19 C20 H20A 119.4 . . ? C21 C20 H20A 119.4 . . ? C22 C21 C20 119.9(5) . . ? C22 C21 H21A 120.1 . . ? C20 C21 H21A 120.1 . . ? C23 C22 C21 120.2(5) . . ? C23 C22 H22A 119.9 . . ? C21 C22 H22A 119.9 . . ? C22 C23 C18 120.5(5) . . ? C22 C23 H23A 119.7 . . ? C18 C23 H23A 119.7 . . ? C29 C24 C25 118.2(4) . . ? C29 C24 C16 121.5(4) . . ? C25 C24 C16 120.4(4) . . ? C26 C25 C24 120.6(5) . . ? C26 C25 H25A 119.7 . . ? C24 C25 H25A 119.7 . . ? C27 C26 C25 120.3(5) . . ? C27 C26 H26A 119.9 . . ? C25 C26 H26A 119.9 . . ? C26 C27 C28 120.1(5) . . ? C26 C27 H27A 119.9 . . ? C28 C27 H27A 119.9 . . ? C27 C28 C29 119.7(5) . . ? C27 C28 H28A 120.1 . . ? C29 C28 H28A 120.1 . . ? C24 C29 C28 121.1(5) . . ? C24 C29 H29A 119.5 . . ? C28 C29 H29A 119.5 . . ? Cl6 Sb1 Cl7 91.52(6) . . ? Cl6 Sb1 Cl4 90.04(6) . . ? Cl7 Sb1 Cl4 177.86(6) . . ? Cl6 Sb1 Cl8 90.12(6) . . ? Cl7 Sb1 Cl8 90.58(5) . . ? Cl4 Sb1 Cl8 90.88(5) . . ? Cl6 Sb1 Cl9 178.41(6) . . ? Cl7 Sb1 Cl9 89.99(5) . . ? Cl4 Sb1 Cl9 88.46(6) . . ? Cl8 Sb1 Cl9 89.36(5) . . ? Cl6 Sb1 Cl5 90.86(5) . . ? Cl7 Sb1 Cl5 89.43(5) . . ? Cl4 Sb1 Cl5 89.09(5) . . ? Cl8 Sb1 Cl5 179.02(5) . . ? Cl9 Sb1 Cl5 89.66(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.764 _refine_diff_density_min -0.848 _refine_diff_density_rms 0.155 #===END data_6[SbCl6] _database_code_depnum_ccdc_archive 'CCDC 697672' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H31 B Cl9 N6 Sb W' _chemical_formula_weight 1099.06 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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 10.4365(11) _cell_length_b 16.9979(13) _cell_length_c 21.716(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.078(12) _cell_angle_gamma 90.00 _cell_volume 3837.4(7) _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 Block _exptl_crystal_colour 'Dark red' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.902 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2120 _exptl_absorpt_coefficient_mu 4.357 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.320 _exptl_absorpt_correction_T_max 0.491 _exptl_absorpt_process_details 'SADABS (Sheldrick 1996)' _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 'CCD area detector' _diffrn_measurement_method 'omega scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 24624 _diffrn_reflns_av_R_equivalents 0.0372 _diffrn_reflns_av_sigmaI/netI 0.0505 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 27.49 _reflns_number_total 8797 _reflns_number_gt 6536 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0322P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8797 _refine_ls_number_parameters 430 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0506 _refine_ls_R_factor_gt 0.0304 _refine_ls_wR_factor_ref 0.0693 _refine_ls_wR_factor_gt 0.0643 _refine_ls_goodness_of_fit_ref 0.948 _refine_ls_restrained_S_all 0.948 _refine_ls_shift/su_max 0.005 _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 0.593999(16) 1.331095(9) 0.652654(7) 0.02598(5) Uani 1 1 d . . . Cl1 Cl 0.39531(11) 1.35887(7) 0.60186(5) 0.0375(3) Uani 1 1 d . . . Cl2 Cl 0.55054(11) 1.33958(6) 0.75582(5) 0.0347(2) Uani 1 1 d . . . N3 N 0.7690(3) 1.27289(18) 0.68743(15) 0.0276(8) Uani 1 1 d . . . N4 N 0.7940(3) 1.19793(19) 0.66695(15) 0.0275(8) Uani 1 1 d . . . C6 C 0.8731(5) 1.3681(3) 0.7659(2) 0.0417(11) Uani 1 1 d . . . H6A H 0.8595 1.4119 0.7367 0.062 Uiso 1 1 calc R . . H6B H 0.9583 1.3730 0.7885 0.062 Uiso 1 1 calc R . . H6C H 0.8070 1.3694 0.7952 0.062 Uiso 1 1 calc R . . C7 C 0.8649(4) 1.2917(3) 0.73124(19) 0.0330(10) Uani 1 1 d . . . C8 C 0.9478(4) 1.2289(3) 0.7394(2) 0.0372(11) Uani 1 1 d . . . H8A H 1.0223 1.2258 0.7678 0.045 Uiso 1 1 calc R . . C9 C 0.9022(4) 1.1710(3) 0.69834(19) 0.0339(10) Uani 1 1 d . . . C10 C 0.9550(5) 1.0908(3) 0.6878(2) 0.0453(12) Uani 1 1 d . . . H10A H 0.8849 1.0523 0.6858 0.068 Uiso 1 1 calc R . . H10B H 1.0189 1.0773 0.7220 0.068 Uiso 1 1 calc R . . H10C H 0.9956 1.0903 0.6489 0.068 Uiso 1 1 calc R . . N1 N 0.5089(3) 1.21086(19) 0.65871(15) 0.0302(8) Uani 1 1 d . . . N2 N 0.5742(3) 1.14626(19) 0.63977(15) 0.0298(8) Uani 1 1 d . . . C1 C 0.2908(4) 1.2314(3) 0.6999(2) 0.0433(12) Uani 1 1 d . . . H1A H 0.3255 1.2828 0.7132 0.065 Uiso 1 1 calc R . . H1B H 0.2582 1.2043 0.7351 0.065 Uiso 1 1 calc R . . H1C H 0.2205 1.2387 0.6673 0.065 Uiso 1 1 calc R . . C2 C 0.3946(4) 1.1832(3) 0.67539(19) 0.0337(10) Uani 1 1 d . . . C3 C 0.3915(4) 1.1028(3) 0.6666(2) 0.0357(10) Uani 1 1 d . . . Cl3 Cl 0.27046(13) 1.03930(8) 0.68080(7) 0.0579(4) Uani 1 1 d . . . C4 C 0.5056(4) 1.0804(2) 0.64398(19) 0.0343(10) Uani 1 1 d . . . C5 C 0.5462(5) 1.0015(3) 0.6254(2) 0.0459(12) Uani 1 1 d . . . H5A H 0.6375 0.9940 0.6388 0.069 Uiso 1 1 calc R . . H5B H 0.5329 0.9965 0.5804 0.069 Uiso 1 1 calc R . . H5C H 0.4952 0.9615 0.6448 0.069 Uiso 1 1 calc R . . N5 N 0.6489(3) 1.29031(19) 0.56642(14) 0.0273(7) Uani 1 1 d . . . N6 N 0.6885(3) 1.21405(19) 0.55941(15) 0.0282(8) Uani 1 1 d . . . C11 C 0.6055(5) 1.4081(3) 0.4960(2) 0.0416(12) Uani 1 1 d . . . H11A H 0.6585 1.4439 0.5229 0.062 Uiso 1 1 calc R . . H11B H 0.5149 1.4145 0.5036 0.062 Uiso 1 1 calc R . . H11C H 0.6164 1.4203 0.4527 0.062 Uiso 1 1 calc R . . C12 C 0.6463(4) 1.3246(3) 0.50962(19) 0.0333(10) Uani 1 1 d . . . C13 C 0.6817(4) 1.2698(3) 0.46803(19) 0.0357(10) Uani 1 1 d . . . H13A H 0.6864 1.2777 0.4250 0.043 Uiso 1 1 calc R . . C14 C 0.7093(4) 1.2006(3) 0.5004(2) 0.0350(10) Uani 1 1 d . . . C15 C 0.7488(5) 1.1224(3) 0.4773(2) 0.0445(12) Uani 1 1 d . . . H15A H 0.6874 1.0822 0.4882 0.067 Uiso 1 1 calc R . . H15B H 0.8348 1.1092 0.4962 0.067 Uiso 1 1 calc R . . H15C H 0.7500 1.1245 0.4323 0.067 Uiso 1 1 calc R . . B1 B 0.7054(5) 1.1582(3) 0.6160(2) 0.0314(11) Uani 1 1 d . . . H1 H 0.7423 1.1067 0.6041 0.038 Uiso 1 1 calc R . . C16 C 0.7129(4) 1.4230(2) 0.63909(17) 0.0265(9) Uani 1 1 d . . . C17 C 0.6073(4) 1.4505(2) 0.65897(17) 0.0273(9) Uani 1 1 d . . . C18 C 0.5300(4) 1.5176(2) 0.67300(18) 0.0283(9) Uani 1 1 d . . . C19 C 0.5693(4) 1.5938(2) 0.66013(18) 0.0334(10) Uani 1 1 d . . . H19A H 0.6497 1.6018 0.6437 0.040 Uiso 1 1 calc R . . C20 C 0.4933(5) 1.6579(3) 0.6709(2) 0.0409(11) Uani 1 1 d . . . H20A H 0.5208 1.7095 0.6618 0.049 Uiso 1 1 calc R . . C21 C 0.3761(5) 1.6462(3) 0.6954(2) 0.0418(12) Uani 1 1 d . . . H21A H 0.3238 1.6903 0.7031 0.050 Uiso 1 1 calc R . . C22 C 0.3347(5) 1.5717(3) 0.7087(2) 0.0412(11) Uani 1 1 d . . . H22A H 0.2547 1.5646 0.7256 0.049 Uiso 1 1 calc R . . C23 C 0.4094(4) 1.5078(3) 0.69749(19) 0.0368(11) Uani 1 1 d . . . H23A H 0.3800 1.4565 0.7062 0.044 Uiso 1 1 calc R . . C24 C 0.8413(4) 1.4419(2) 0.62095(19) 0.0301(9) Uani 1 1 d . . . C25 C 0.9181(4) 1.3849(3) 0.59581(19) 0.0356(10) Uani 1 1 d . . . H25A H 0.8877 1.3324 0.5906 0.043 Uiso 1 1 calc R . . C26 C 1.0371(5) 1.4047(3) 0.5786(2) 0.0487(13) Uani 1 1 d . . . H26A H 1.0882 1.3660 0.5609 0.058 Uiso 1 1 calc R . . C27 C 1.0836(5) 1.4802(3) 0.5868(3) 0.0664(17) Uani 1 1 d . . . H27A H 1.1665 1.4931 0.5749 0.080 Uiso 1 1 calc R . . C28 C 1.0106(5) 1.5369(3) 0.6121(3) 0.0698(19) Uani 1 1 d . . . H28A H 1.0431 1.5889 0.6178 0.084 Uiso 1 1 calc R . . C29 C 0.8892(5) 1.5182(3) 0.6293(2) 0.0490(13) Uani 1 1 d . . . H29A H 0.8387 1.5574 0.6469 0.059 Uiso 1 1 calc R . . Sb1 Sb 0.82368(3) 0.686186(17) 1.049956(13) 0.03494(8) Uani 1 1 d . . . Cl4 Cl 0.90388(14) 0.69423(7) 0.95164(5) 0.0519(3) Uani 1 1 d . . . Cl5 Cl 0.90768(15) 0.55825(7) 1.06266(6) 0.0571(4) Uani 1 1 d . . . Cl6 Cl 0.74295(15) 0.81610(8) 1.04053(6) 0.0553(4) Uani 1 1 d . . . Cl7 Cl 0.62650(14) 0.63805(10) 1.00405(6) 0.0660(4) Uani 1 1 d . . . Cl8 Cl 1.02038(12) 0.73960(7) 1.09469(6) 0.0466(3) Uani 1 1 d . . . Cl9 Cl 0.74853(13) 0.67798(8) 1.14980(5) 0.0526(3) 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 0.02121(9) 0.02825(9) 0.02878(9) -0.00104(7) 0.00388(7) 0.00068(8) Cl1 0.0235(6) 0.0449(6) 0.0433(6) -0.0041(5) -0.0018(5) 0.0033(5) Cl2 0.0370(6) 0.0362(6) 0.0321(5) -0.0015(4) 0.0097(5) 0.0003(5) N3 0.026(2) 0.0256(17) 0.0321(19) 0.0046(14) 0.0066(16) 0.0017(15) N4 0.0254(19) 0.0275(17) 0.0304(18) -0.0001(14) 0.0069(16) 0.0049(15) C6 0.040(3) 0.047(3) 0.037(3) -0.007(2) -0.005(2) -0.002(2) C7 0.026(2) 0.044(3) 0.029(2) 0.0023(18) 0.002(2) 0.002(2) C8 0.028(3) 0.049(3) 0.034(2) 0.002(2) -0.001(2) 0.009(2) C9 0.029(2) 0.040(2) 0.034(2) 0.0072(19) 0.010(2) 0.004(2) C10 0.038(3) 0.044(3) 0.054(3) 0.000(2) 0.008(3) 0.017(2) N1 0.025(2) 0.0296(19) 0.037(2) -0.0032(14) 0.0081(17) -0.0042(16) N2 0.027(2) 0.0296(18) 0.0341(19) -0.0015(14) 0.0068(17) -0.0018(15) C1 0.026(3) 0.057(3) 0.048(3) -0.007(2) 0.011(2) -0.005(2) C2 0.026(2) 0.045(3) 0.031(2) -0.0021(18) 0.0063(19) -0.003(2) C3 0.030(3) 0.038(2) 0.039(2) 0.0029(19) 0.004(2) -0.010(2) Cl3 0.0395(8) 0.0559(8) 0.0795(9) 0.0065(7) 0.0118(7) -0.0145(6) C4 0.031(3) 0.035(2) 0.037(2) 0.0028(18) 0.007(2) -0.007(2) C5 0.043(3) 0.035(3) 0.061(3) 0.000(2) 0.010(3) -0.006(2) N5 0.0229(19) 0.0287(18) 0.0300(18) -0.0015(14) 0.0009(16) -0.0014(15) N6 0.0224(19) 0.0325(19) 0.0299(18) -0.0040(14) 0.0042(16) 0.0000(15) C11 0.042(3) 0.047(3) 0.036(2) 0.014(2) 0.001(2) 0.008(2) C12 0.024(2) 0.045(3) 0.031(2) 0.0033(19) 0.0006(19) 0.001(2) C13 0.030(3) 0.052(3) 0.025(2) 0.0013(19) 0.003(2) 0.004(2) C14 0.023(2) 0.045(3) 0.037(2) -0.0103(19) 0.006(2) -0.003(2) C15 0.050(3) 0.042(3) 0.043(3) -0.012(2) 0.015(3) -0.001(2) B1 0.029(3) 0.028(3) 0.038(3) 0.000(2) 0.007(2) 0.002(2) C16 0.024(2) 0.026(2) 0.029(2) 0.0003(16) 0.0001(19) 0.0001(18) C17 0.026(2) 0.031(2) 0.023(2) 0.0009(16) -0.0008(18) -0.0022(19) C18 0.023(2) 0.032(2) 0.029(2) -0.0032(17) 0.0028(19) 0.0048(18) C19 0.029(3) 0.032(2) 0.039(2) -0.0028(18) 0.009(2) 0.0002(19) C20 0.041(3) 0.034(3) 0.048(3) -0.002(2) 0.008(2) 0.001(2) C21 0.037(3) 0.039(3) 0.050(3) -0.012(2) 0.005(2) 0.015(2) C22 0.032(3) 0.047(3) 0.046(3) -0.006(2) 0.012(2) 0.006(2) C23 0.033(3) 0.038(2) 0.039(2) -0.0019(19) 0.007(2) 0.003(2) C24 0.020(2) 0.030(2) 0.040(2) 0.0056(18) 0.001(2) 0.0017(18) C25 0.028(2) 0.036(2) 0.043(3) 0.0001(19) 0.007(2) 0.000(2) C26 0.032(3) 0.046(3) 0.070(3) 0.004(2) 0.017(3) 0.007(2) C27 0.032(3) 0.054(4) 0.117(5) 0.019(3) 0.024(3) -0.001(3) C28 0.032(3) 0.033(3) 0.146(6) 0.012(3) 0.016(4) -0.002(2) C29 0.028(3) 0.030(3) 0.089(4) 0.004(2) 0.002(3) 0.002(2) Sb1 0.03618(18) 0.03981(17) 0.02969(15) 0.00087(12) 0.00787(14) 0.00097(14) Cl4 0.0676(9) 0.0564(7) 0.0346(6) 0.0023(5) 0.0201(6) 0.0064(7) Cl5 0.0712(10) 0.0345(6) 0.0677(8) 0.0064(6) 0.0187(8) 0.0022(6) Cl6 0.0654(9) 0.0570(8) 0.0444(7) 0.0020(6) 0.0092(7) 0.0259(7) Cl7 0.0488(9) 0.0961(11) 0.0519(8) -0.0075(7) -0.0022(7) -0.0178(8) Cl8 0.0417(7) 0.0459(7) 0.0522(7) 0.0030(5) 0.0039(6) -0.0043(6) Cl9 0.0538(8) 0.0713(9) 0.0349(6) 0.0032(6) 0.0168(6) -0.0042(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 W1 C16 2.033(4) . ? W1 C17 2.037(4) . ? W1 N5 2.123(3) . ? W1 N3 2.155(3) . ? W1 N1 2.237(3) . ? W1 Cl1 2.3097(11) . ? W1 Cl2 2.3293(10) . ? N3 C7 1.356(5) . ? N3 N4 1.382(4) . ? N4 C9 1.347(5) . ? N4 B1 1.534(6) . ? C6 C7 1.499(6) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.376(6) . ? C8 C9 1.384(6) . ? C8 H8A 0.9500 . ? C9 C10 1.494(6) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? N1 C2 1.360(5) . ? N1 N2 1.375(5) . ? N2 C4 1.336(5) . ? N2 B1 1.519(6) . ? C1 C2 1.494(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.379(6) . ? C3 C4 1.382(6) . ? C3 Cl3 1.710(4) . ? C4 C5 1.473(6) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? N5 C12 1.363(5) . ? N5 N6 1.373(4) . ? N6 C14 1.338(5) . ? N6 B1 1.551(6) . ? C11 C12 1.504(6) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.371(6) . ? C13 C14 1.388(6) . ? C13 H13A 0.9500 . ? C14 C15 1.491(6) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? B1 H1 1.0000 . ? C16 C17 1.305(5) . ? C16 C24 1.465(6) . ? C17 C18 1.445(5) . ? C18 C19 1.396(6) . ? C18 C23 1.420(6) . ? C19 C20 1.380(6) . ? C19 H19A 0.9500 . ? C20 C21 1.390(7) . ? C20 H20A 0.9500 . ? C21 C22 1.378(6) . ? C21 H21A 0.9500 . ? C22 C23 1.370(6) . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? C24 C29 1.396(6) . ? C24 C25 1.399(6) . ? C25 C26 1.370(6) . ? C25 H25A 0.9500 . ? C26 C27 1.378(7) . ? C26 H26A 0.9500 . ? C27 C28 1.372(7) . ? C27 H27A 0.9500 . ? C28 C29 1.389(7) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? Sb1 Cl5 2.3518(13) . ? Sb1 Cl7 2.3526(15) . ? Sb1 Cl4 2.3653(12) . ? Sb1 Cl6 2.3660(13) . ? Sb1 Cl8 2.3726(13) . ? Sb1 Cl9 2.3744(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C16 W1 C17 37.40(15) . . ? C16 W1 N5 84.68(14) . . ? C17 W1 N5 111.25(14) . . ? C16 W1 N3 83.93(14) . . ? C17 W1 N3 112.53(15) . . ? N5 W1 N3 82.69(13) . . ? C16 W1 N1 164.03(14) . . ? C17 W1 N1 158.57(15) . . ? N5 W1 N1 83.86(12) . . ? N3 W1 N1 83.61(12) . . ? C16 W1 Cl1 107.91(12) . . ? C17 W1 Cl1 83.20(12) . . ? N5 W1 Cl1 86.92(10) . . ? N3 W1 Cl1 163.49(9) . . ? N1 W1 Cl1 82.55(10) . . ? C16 W1 Cl2 105.37(11) . . ? C17 W1 Cl2 83.77(11) . . ? N5 W1 Cl2 163.65(9) . . ? N3 W1 Cl2 85.56(9) . . ? N1 W1 Cl2 83.56(9) . . ? Cl1 W1 Cl2 101.75(4) . . ? C7 N3 N4 107.2(3) . . ? C7 N3 W1 133.4(3) . . ? N4 N3 W1 119.3(3) . . ? C9 N4 N3 108.9(3) . . ? C9 N4 B1 129.8(4) . . ? N3 N4 B1 121.3(3) . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N3 C7 C8 108.9(4) . . ? N3 C7 C6 124.2(4) . . ? C8 C7 C6 126.9(4) . . ? C7 C8 C9 107.0(4) . . ? C7 C8 H8A 126.5 . . ? C9 C8 H8A 126.5 . . ? N4 C9 C8 108.0(4) . . ? N4 C9 C10 122.5(4) . . ? C8 C9 C10 129.5(4) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C2 N1 N2 105.8(3) . . ? C2 N1 W1 133.9(3) . . ? N2 N1 W1 120.1(2) . . ? C4 N2 N1 111.5(3) . . ? C4 N2 B1 129.8(4) . . ? N1 N2 B1 118.7(3) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 108.5(4) . . ? N1 C2 C1 125.8(4) . . ? C3 C2 C1 125.7(4) . . ? C2 C3 C4 108.1(4) . . ? C2 C3 Cl3 127.6(4) . . ? C4 C3 Cl3 124.3(3) . . ? N2 C4 C3 106.1(4) . . ? N2 C4 C5 125.1(4) . . ? C3 C4 C5 128.8(4) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C12 N5 N6 106.6(3) . . ? C12 N5 W1 132.4(3) . . ? N6 N5 W1 120.9(2) . . ? C14 N6 N5 110.1(3) . . ? C14 N6 B1 129.6(4) . . ? N5 N6 B1 120.3(3) . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N5 C12 C13 108.7(4) . . ? N5 C12 C11 124.4(4) . . ? C13 C12 C11 126.9(4) . . ? C12 C13 C14 107.3(4) . . ? C12 C13 H13A 126.3 . . ? C14 C13 H13A 126.3 . . ? N6 C14 C13 107.2(4) . . ? N6 C14 C15 123.3(4) . . ? C13 C14 C15 129.4(4) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N2 B1 N4 108.6(3) . . ? N2 B1 N6 107.9(4) . . ? N4 B1 N6 108.8(3) . . ? N2 B1 H1 110.5 . . ? N4 B1 H1 110.5 . . ? N6 B1 H1 110.5 . . ? C17 C16 C24 146.1(4) . . ? C17 C16 W1 71.5(3) . . ? C24 C16 W1 142.4(3) . . ? C16 C17 C18 148.8(4) . . ? C16 C17 W1 71.1(2) . . ? C18 C17 W1 139.9(3) . . ? C19 C18 C23 118.0(4) . . ? C19 C18 C17 120.8(4) . . ? C23 C18 C17 121.2(4) . . ? C20 C19 C18 121.0(4) . . ? C20 C19 H19A 119.5 . . ? C18 C19 H19A 119.5 . . ? C19 C20 C21 119.4(4) . . ? C19 C20 H20A 120.3 . . ? C21 C20 H20A 120.3 . . ? C22 C21 C20 120.9(4) . . ? C22 C21 H21A 119.5 . . ? C20 C21 H21A 119.5 . . ? C23 C22 C21 119.9(4) . . ? C23 C22 H22A 120.1 . . ? C21 C22 H22A 120.1 . . ? C22 C23 C18 120.8(4) . . ? C22 C23 H23A 119.6 . . ? C18 C23 H23A 119.6 . . ? C29 C24 C25 118.9(4) . . ? C29 C24 C16 119.6(4) . . ? C25 C24 C16 121.4(4) . . ? C26 C25 C24 120.0(4) . . ? C26 C25 H25A 120.0 . . ? C24 C25 H25A 120.0 . . ? C25 C26 C27 120.7(5) . . ? C25 C26 H26A 119.6 . . ? C27 C26 H26A 119.6 . . ? C28 C27 C26 120.3(5) . . ? C28 C27 H27A 119.9 . . ? C26 C27 H27A 119.9 . . ? C27 C28 C29 119.9(5) . . ? C27 C28 H28A 120.0 . . ? C29 C28 H28A 120.0 . . ? C28 C29 C24 120.1(5) . . ? C28 C29 H29A 119.9 . . ? C24 C29 H29A 119.9 . . ? Cl5 Sb1 Cl7 91.78(6) . . ? Cl5 Sb1 Cl4 90.08(5) . . ? Cl7 Sb1 Cl4 90.21(5) . . ? Cl5 Sb1 Cl6 178.01(5) . . ? Cl7 Sb1 Cl6 89.80(6) . . ? Cl4 Sb1 Cl6 91.13(4) . . ? Cl5 Sb1 Cl8 90.33(5) . . ? Cl7 Sb1 Cl8 177.79(5) . . ? Cl4 Sb1 Cl8 89.14(5) . . ? Cl6 Sb1 Cl8 88.10(5) . . ? Cl5 Sb1 Cl9 89.33(5) . . ? Cl7 Sb1 Cl9 91.11(5) . . ? Cl4 Sb1 Cl9 178.57(5) . . ? Cl6 Sb1 Cl9 89.42(5) . . ? Cl8 Sb1 Cl9 89.56(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C16 W1 N3 C7 53.6(4) . . . . ? C17 W1 N3 C7 29.0(4) . . . . ? N5 W1 N3 C7 139.0(4) . . . . ? N1 W1 N3 C7 -136.4(4) . . . . ? Cl1 W1 N3 C7 -169.6(3) . . . . ? Cl2 W1 N3 C7 -52.4(3) . . . . ? C16 W1 N3 N4 -131.8(3) . . . . ? C17 W1 N3 N4 -156.5(3) . . . . ? N5 W1 N3 N4 -46.4(3) . . . . ? N1 W1 N3 N4 38.2(3) . . . . ? Cl1 W1 N3 N4 5.0(5) . . . . ? Cl2 W1 N3 N4 122.2(3) . . . . ? C7 N3 N4 C9 0.9(4) . . . . ? W1 N3 N4 C9 -175.0(2) . . . . ? C7 N3 N4 B1 -178.9(3) . . . . ? W1 N3 N4 B1 5.2(4) . . . . ? N4 N3 C7 C8 -1.3(4) . . . . ? W1 N3 C7 C8 173.7(3) . . . . ? N4 N3 C7 C6 -179.2(4) . . . . ? W1 N3 C7 C6 -4.2(6) . . . . ? N3 C7 C8 C9 1.3(5) . . . . ? C6 C7 C8 C9 179.1(4) . . . . ? N3 N4 C9 C8 -0.1(4) . . . . ? B1 N4 C9 C8 179.7(4) . . . . ? N3 N4 C9 C10 179.1(4) . . . . ? B1 N4 C9 C10 -1.1(7) . . . . ? C7 C8 C9 N4 -0.7(5) . . . . ? C7 C8 C9 C10 -179.8(4) . . . . ? C16 W1 N1 C2 -179.5(5) . . . . ? C17 W1 N1 C2 1.3(6) . . . . ? N5 W1 N1 C2 -135.1(4) . . . . ? N3 W1 N1 C2 141.6(4) . . . . ? Cl1 W1 N1 C2 -47.4(4) . . . . ? Cl2 W1 N1 C2 55.4(4) . . . . ? C16 W1 N1 N2 -3.6(7) . . . . ? C17 W1 N1 N2 177.2(3) . . . . ? N5 W1 N1 N2 40.8(3) . . . . ? N3 W1 N1 N2 -42.5(3) . . . . ? Cl1 W1 N1 N2 128.5(3) . . . . ? Cl2 W1 N1 N2 -128.7(3) . . . . ? C2 N1 N2 C4 0.0(5) . . . . ? W1 N1 N2 C4 -176.9(3) . . . . ? C2 N1 N2 B1 178.1(4) . . . . ? W1 N1 N2 B1 1.1(5) . . . . ? N2 N1 C2 C3 0.1(5) . . . . ? W1 N1 C2 C3 176.4(3) . . . . ? N2 N1 C2 C1 179.3(4) . . . . ? W1 N1 C2 C1 -4.3(7) . . . . ? N1 C2 C3 C4 -0.1(5) . . . . ? C1 C2 C3 C4 -179.4(4) . . . . ? N1 C2 C3 Cl3 179.6(3) . . . . ? C1 C2 C3 Cl3 0.3(7) . . . . ? N1 N2 C4 C3 -0.1(5) . . . . ? B1 N2 C4 C3 -177.9(4) . . . . ? N1 N2 C4 C5 177.9(4) . . . . ? B1 N2 C4 C5 0.1(7) . . . . ? C2 C3 C4 N2 0.1(5) . . . . ? Cl3 C3 C4 N2 -179.6(3) . . . . ? C2 C3 C4 C5 -177.8(4) . . . . ? Cl3 C3 C4 C5 2.5(7) . . . . ? C16 W1 N5 C12 -53.8(4) . . . . ? C17 W1 N5 C12 -26.9(4) . . . . ? N3 W1 N5 C12 -138.3(4) . . . . ? N1 W1 N5 C12 137.4(4) . . . . ? Cl1 W1 N5 C12 54.5(4) . . . . ? Cl2 W1 N5 C12 177.3(3) . . . . ? C16 W1 N5 N6 131.3(3) . . . . ? C17 W1 N5 N6 158.1(3) . . . . ? N3 W1 N5 N6 46.7(3) . . . . ? N1 W1 N5 N6 -37.6(3) . . . . ? Cl1 W1 N5 N6 -120.4(3) . . . . ? Cl2 W1 N5 N6 2.3(6) . . . . ? C12 N5 N6 C14 -0.4(4) . . . . ? W1 N5 N6 C14 175.7(3) . . . . ? C12 N5 N6 B1 178.4(4) . . . . ? W1 N5 N6 B1 -5.4(5) . . . . ? N6 N5 C12 C13 1.1(5) . . . . ? W1 N5 C12 C13 -174.4(3) . . . . ? N6 N5 C12 C11 178.7(4) . . . . ? W1 N5 C12 C11 3.2(7) . . . . ? N5 C12 C13 C14 -1.3(5) . . . . ? C11 C12 C13 C14 -178.8(4) . . . . ? N5 N6 C14 C13 -0.4(5) . . . . ? B1 N6 C14 C13 -179.1(4) . . . . ? N5 N6 C14 C15 -177.8(4) . . . . ? B1 N6 C14 C15 3.5(7) . . . . ? C12 C13 C14 N6 1.0(5) . . . . ? C12 C13 C14 C15 178.2(4) . . . . ? C4 N2 B1 N4 -124.0(4) . . . . ? N1 N2 B1 N4 58.3(5) . . . . ? C4 N2 B1 N6 118.2(4) . . . . ? N1 N2 B1 N6 -59.4(5) . . . . ? C9 N4 B1 N2 116.0(4) . . . . ? N3 N4 B1 N2 -64.2(4) . . . . ? C9 N4 B1 N6 -126.8(4) . . . . ? N3 N4 B1 N6 53.0(5) . . . . ? C14 N6 B1 N2 -117.0(5) . . . . ? N5 N6 B1 N2 64.3(5) . . . . ? C14 N6 B1 N4 125.4(4) . . . . ? N5 N6 B1 N4 -53.3(5) . . . . ? N5 W1 C16 C17 136.1(3) . . . . ? N3 W1 C16 C17 -140.7(3) . . . . ? N1 W1 C16 C17 -179.5(4) . . . . ? Cl1 W1 C16 C17 51.1(2) . . . . ? Cl2 W1 C16 C17 -57.0(2) . . . . ? C17 W1 C16 C24 177.1(6) . . . . ? N5 W1 C16 C24 -46.7(5) . . . . ? N3 W1 C16 C24 36.4(5) . . . . ? N1 W1 C16 C24 -2.4(9) . . . . ? Cl1 W1 C16 C24 -131.8(5) . . . . ? Cl2 W1 C16 C24 120.1(5) . . . . ? C24 C16 C17 C18 9.1(12) . . . . ? W1 C16 C17 C18 -174.1(7) . . . . ? C24 C16 C17 W1 -176.8(7) . . . . ? N5 W1 C17 C16 -47.7(3) . . . . ? N3 W1 C17 C16 43.0(3) . . . . ? N1 W1 C17 C16 179.6(3) . . . . ? Cl1 W1 C17 C16 -131.7(2) . . . . ? Cl2 W1 C17 C16 125.6(2) . . . . ? C16 W1 C17 C18 175.3(6) . . . . ? N5 W1 C17 C18 127.5(4) . . . . ? N3 W1 C17 C18 -141.7(4) . . . . ? N1 W1 C17 C18 -5.1(7) . . . . ? Cl1 W1 C17 C18 43.5(4) . . . . ? Cl2 W1 C17 C18 -59.2(4) . . . . ? C16 C17 C18 C19 4.2(9) . . . . ? W1 C17 C18 C19 -167.1(3) . . . . ? C16 C17 C18 C23 -178.8(6) . . . . ? W1 C17 C18 C23 9.9(7) . . . . ? C23 C18 C19 C20 0.1(6) . . . . ? C17 C18 C19 C20 177.2(4) . . . . ? C18 C19 C20 C21 0.4(7) . . . . ? C19 C20 C21 C22 -0.3(7) . . . . ? C20 C21 C22 C23 -0.3(7) . . . . ? C21 C22 C23 C18 0.8(7) . . . . ? C19 C18 C23 C22 -0.7(6) . . . . ? C17 C18 C23 C22 -177.8(4) . . . . ? C17 C16 C24 C29 6.7(9) . . . . ? W1 C16 C24 C29 -168.4(4) . . . . ? C17 C16 C24 C25 -173.9(6) . . . . ? W1 C16 C24 C25 11.0(7) . . . . ? C29 C24 C25 C26 -1.4(7) . . . . ? C16 C24 C25 C26 179.2(4) . . . . ? C24 C25 C26 C27 1.1(8) . . . . ? C25 C26 C27 C28 -0.3(9) . . . . ? C26 C27 C28 C29 -0.2(10) . . . . ? C27 C28 C29 C24 -0.1(9) . . . . ? C25 C24 C29 C28 0.8(7) . . . . ? C16 C24 C29 C28 -179.8(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.414 _refine_diff_density_min -0.946 _refine_diff_density_rms 0.112 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 697673' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H32 B F2 N6 W' _chemical_formula_weight 697.27 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' F F 0.0171 0.0103 '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 9.6427(17) _cell_length_b 32.628(7) _cell_length_c 9.8228(17) _cell_angle_alpha 90.00 _cell_angle_beta 113.989(11) _cell_angle_gamma 90.00 _cell_volume 2823.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 123 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Magenta _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'Not measured' _exptl_crystal_density_diffrn 1.640 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1380 _exptl_absorpt_coefficient_mu 4.134 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.555 _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_process_details 'SADABS (Sheldrick 1996)' _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 'CCD area detector' _diffrn_measurement_method 'Omega scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% None _diffrn_reflns_number 29564 _diffrn_reflns_av_R_equivalents 0.0562 _diffrn_reflns_av_sigmaI/netI 0.0483 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6494 _reflns_number_gt 4725 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0250P)^2^+0.9972P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6494 _refine_ls_number_parameters 358 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0546 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0617 _refine_ls_wR_factor_gt 0.0567 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 -0.405019(17) 0.124971(5) -0.380783(17) 0.01906(5) Uani 1 1 d . . . F1 F -0.2193(2) 0.09308(7) -0.3080(3) 0.0270(5) Uani 1 1 d . . . F2 F -0.3250(3) 0.15847(7) -0.1966(2) 0.0266(5) Uani 1 1 d . . . N1 N -0.4673(4) 0.08479(10) -0.2279(4) 0.0210(7) Uani 1 1 d . . . N2 N -0.6129(4) 0.07022(10) -0.2738(4) 0.0216(7) Uani 1 1 d . . . C1 C -0.2325(5) 0.08544(16) 0.0077(5) 0.0362(12) Uani 1 1 d . . . H1A H -0.1730 0.0797 -0.0506 0.054 Uiso 1 1 calc R . . H1B H -0.1938 0.0689 0.0990 0.054 Uiso 1 1 calc R . . H1C H -0.2240 0.1146 0.0338 0.054 Uiso 1 1 calc R . . C2 C -0.3951(5) 0.07494(13) -0.0823(5) 0.0249(9) Uani 1 1 d . . . C3 C -0.4949(5) 0.05433(13) -0.0364(5) 0.0292(10) Uani 1 1 d . . . H3A H -0.4730 0.0436 0.0601 0.035 Uiso 1 1 calc R . . C4 C -0.6317(5) 0.05254(13) -0.1585(5) 0.0255(10) Uani 1 1 d . . . C5 C -0.7805(5) 0.03598(15) -0.1683(5) 0.0355(11) Uani 1 1 d . . . H5A H -0.8229 0.0174 -0.2537 0.053 Uiso 1 1 calc R . . H5B H -0.8512 0.0587 -0.1811 0.053 Uiso 1 1 calc R . . H5C H -0.7648 0.0211 -0.0766 0.053 Uiso 1 1 calc R . . N3 N -0.5127(3) 0.07341(10) -0.5255(4) 0.0201(7) Uani 1 1 d . . . N4 N -0.6541(4) 0.05970(10) -0.5407(4) 0.0218(7) Uani 1 1 d . . . C6 C -0.3251(5) 0.05770(14) -0.6314(5) 0.0299(10) Uani 1 1 d . . . H6A H -0.2462 0.0643 -0.5330 0.045 Uiso 1 1 calc R . . H6B H -0.3356 0.0805 -0.7000 0.045 Uiso 1 1 calc R . . H6C H -0.2968 0.0328 -0.6695 0.045 Uiso 1 1 calc R . . C7 C -0.4733(5) 0.05097(13) -0.6185(4) 0.0240(9) Uani 1 1 d . . . C8 C -0.5871(5) 0.02282(13) -0.6931(4) 0.0261(9) Uani 1 1 d . . . H8A H -0.5873 0.0031 -0.7644 0.031 Uiso 1 1 calc R . . C9 C -0.6999(5) 0.02918(12) -0.6429(5) 0.0246(9) Uani 1 1 d . . . C10 C -0.8500(5) 0.00840(14) -0.6907(5) 0.0346(11) Uani 1 1 d . . . H10A H -0.8679 0.0008 -0.6027 0.052 Uiso 1 1 calc R . . H10B H -0.8506 -0.0163 -0.7477 0.052 Uiso 1 1 calc R . . H10C H -0.9303 0.0270 -0.7533 0.052 Uiso 1 1 calc R . . N5 N -0.6255(4) 0.14930(10) -0.4187(4) 0.0210(7) Uani 1 1 d . . . N6 N -0.7485(3) 0.12351(11) -0.4607(3) 0.0222(7) Uani 1 1 d . . . C11 C -0.5770(5) 0.22449(14) -0.3948(6) 0.0385(12) Uani 1 1 d . . . H11A H -0.4782 0.2178 -0.3153 0.058 Uiso 1 1 calc R . . H11B H -0.6228 0.2473 -0.3626 0.058 Uiso 1 1 calc R . . H11C H -0.5632 0.2325 -0.4847 0.058 Uiso 1 1 calc R . . C12 C -0.6784(5) 0.18799(13) -0.4277(5) 0.0248(9) Uani 1 1 d . . . C13 C -0.8347(5) 0.18690(14) -0.4766(5) 0.0281(10) Uani 1 1 d . . . H13A H -0.9007 0.2098 -0.4941 0.034 Uiso 1 1 calc R . . C14 C -0.8757(4) 0.14625(13) -0.4948(5) 0.0245(9) Uani 1 1 d . . . C15 C -1.0300(5) 0.12735(16) -0.5447(5) 0.0363(11) Uani 1 1 d . . . H15A H -1.0400 0.1053 -0.6157 0.054 Uiso 1 1 calc R . . H15B H -1.1075 0.1483 -0.5929 0.054 Uiso 1 1 calc R . . H15C H -1.0434 0.1162 -0.4583 0.054 Uiso 1 1 calc R . . B1 B -0.7250(6) 0.07713(15) -0.4376(6) 0.0259(11) Uani 1 1 d . . . H1 H -0.8239 0.0633 -0.4576 0.031 Uiso 1 1 calc R . . C16 C -0.4307(4) 0.15221(12) -0.5776(5) 0.0219(9) Uani 1 1 d . . . C17 C -0.3213(4) 0.17054(13) -0.4653(4) 0.0216(9) Uani 1 1 d . . . C18 C -0.2126(5) 0.20451(13) -0.4200(5) 0.0232(9) Uani 1 1 d . . . C19 C -0.0828(4) 0.20214(13) -0.2872(5) 0.0255(9) Uani 1 1 d . . . H19A H -0.0650 0.1784 -0.2266 0.031 Uiso 1 1 calc R . . C20 C 0.0198(5) 0.23401(14) -0.2432(5) 0.0288(11) Uani 1 1 d . . . H20A H 0.1094 0.2317 -0.1542 0.035 Uiso 1 1 calc R . . C21 C -0.0065(5) 0.26914(13) -0.3272(5) 0.0311(10) Uani 1 1 d . . . H21A H 0.0646 0.2910 -0.2956 0.037 Uiso 1 1 calc R . . C22 C -0.1370(5) 0.27278(14) -0.4584(5) 0.0333(11) Uani 1 1 d . . . H22A H -0.1569 0.2974 -0.5149 0.040 Uiso 1 1 calc R . . C23 C -0.2376(5) 0.24021(14) -0.5059(5) 0.0287(10) Uani 1 1 d . . . H23A H -0.3243 0.2421 -0.5977 0.034 Uiso 1 1 calc R . . C24 C -0.5157(5) 0.15322(13) -0.7393(4) 0.0231(9) Uani 1 1 d . . . C25 C -0.4496(5) 0.16723(13) -0.8331(5) 0.0288(10) Uani 1 1 d . . . H25A H -0.3484 0.1773 -0.7914 0.035 Uiso 1 1 calc R . . C26 C -0.5299(6) 0.16671(14) -0.9867(5) 0.0358(11) Uani 1 1 d . . . H26A H -0.4823 0.1752 -1.0499 0.043 Uiso 1 1 calc R . . C27 C -0.6775(6) 0.15395(16) -1.0467(5) 0.0400(12) Uani 1 1 d . . . H27A H -0.7334 0.1544 -1.1517 0.048 Uiso 1 1 calc R . . C28 C -0.7467(5) 0.14026(15) -0.9556(5) 0.0374(12) Uani 1 1 d . . . H28A H -0.8497 0.1317 -0.9981 0.045 Uiso 1 1 calc R . . C29 C -0.6653(5) 0.13924(13) -0.8035(5) 0.0299(10) Uani 1 1 d . . . H29B H -0.7116 0.1289 -0.7416 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 0.01928(8) 0.02085(8) 0.01674(8) -0.00105(8) 0.00702(6) -0.00305(8) F1 0.0233(12) 0.0302(14) 0.0257(13) 0.0025(11) 0.0081(11) 0.0009(10) F2 0.0314(13) 0.0279(14) 0.0203(12) -0.0053(10) 0.0103(11) -0.0087(11) N1 0.0220(17) 0.022(2) 0.0180(17) -0.0006(14) 0.0072(14) -0.0034(15) N2 0.0240(18) 0.0199(19) 0.0221(19) -0.0006(15) 0.0105(15) -0.0024(14) C1 0.033(3) 0.045(3) 0.024(2) 0.005(2) 0.004(2) -0.006(2) C2 0.030(2) 0.021(2) 0.021(2) 0.0001(18) 0.0084(19) 0.0001(18) C3 0.040(3) 0.025(2) 0.023(2) 0.0059(19) 0.013(2) -0.001(2) C4 0.034(2) 0.023(2) 0.024(2) -0.0012(17) 0.016(2) -0.0037(18) C5 0.039(3) 0.035(3) 0.042(3) 0.002(2) 0.026(2) -0.007(2) N3 0.0185(17) 0.0196(18) 0.0213(18) -0.0046(14) 0.0072(15) -0.0036(14) N4 0.0201(17) 0.0213(19) 0.0225(19) -0.0004(15) 0.0073(15) -0.0019(14) C6 0.030(2) 0.035(3) 0.027(2) -0.005(2) 0.015(2) 0.001(2) C7 0.027(2) 0.024(2) 0.017(2) 0.0040(17) 0.0046(18) 0.0058(18) C8 0.032(2) 0.024(2) 0.018(2) -0.0032(18) 0.0071(19) 0.0011(19) C9 0.027(2) 0.019(2) 0.022(2) -0.0024(18) 0.0031(18) -0.0035(18) C10 0.031(3) 0.029(3) 0.036(3) -0.007(2) 0.007(2) -0.011(2) N5 0.0181(17) 0.0217(19) 0.0211(18) -0.0001(15) 0.0058(15) -0.0013(14) N6 0.0215(16) 0.0250(18) 0.0215(17) 0.0013(17) 0.0101(14) -0.0003(16) C11 0.039(3) 0.025(3) 0.056(3) -0.002(2) 0.024(3) 0.000(2) C12 0.028(2) 0.023(2) 0.026(2) 0.0038(19) 0.014(2) 0.0034(19) C13 0.030(2) 0.029(3) 0.027(2) 0.0055(19) 0.013(2) 0.0087(19) C14 0.020(2) 0.031(2) 0.023(2) 0.0048(19) 0.0086(18) 0.0035(18) C15 0.023(2) 0.042(3) 0.043(3) -0.003(3) 0.013(2) 0.002(2) B1 0.024(3) 0.024(3) 0.033(3) -0.006(2) 0.015(2) -0.003(2) C16 0.020(2) 0.022(2) 0.028(2) 0.0012(18) 0.0143(18) 0.0016(17) C17 0.018(2) 0.027(2) 0.021(2) 0.0002(18) 0.0085(17) 0.0014(17) C18 0.024(2) 0.022(2) 0.025(2) -0.0002(18) 0.0118(18) -0.0028(17) C19 0.024(2) 0.028(2) 0.023(2) 0.0013(18) 0.0083(19) -0.0004(18) C20 0.023(2) 0.035(3) 0.024(3) -0.0079(19) 0.0047(19) -0.0085(19) C21 0.037(3) 0.024(3) 0.033(3) -0.008(2) 0.016(2) -0.010(2) C22 0.043(3) 0.024(3) 0.035(3) 0.009(2) 0.019(2) -0.005(2) C23 0.029(2) 0.032(3) 0.024(2) 0.0063(19) 0.009(2) -0.0003(19) C24 0.027(2) 0.023(2) 0.018(2) 0.0005(17) 0.0083(19) 0.0031(17) C25 0.036(3) 0.027(3) 0.027(2) 0.0044(19) 0.016(2) 0.004(2) C26 0.050(3) 0.037(3) 0.027(3) 0.005(2) 0.022(2) 0.007(2) C27 0.052(3) 0.044(3) 0.013(2) 0.004(2) 0.002(2) 0.011(3) C28 0.030(2) 0.042(3) 0.027(3) 0.000(2) -0.002(2) -0.004(2) C29 0.030(2) 0.030(3) 0.027(2) 0.0038(19) 0.010(2) -0.0051(19) _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 F1 1.939(2) . ? W1 F2 1.982(2) . ? W1 C17 2.024(4) . ? W1 C16 2.049(4) . ? W1 N5 2.155(3) . ? W1 N3 2.175(3) . ? W1 N1 2.252(3) . ? N1 C2 1.351(5) . ? N1 N2 1.373(4) . ? N2 C4 1.347(5) . ? N2 B1 1.547(6) . ? C1 C2 1.493(6) . ? C2 C3 1.391(6) . ? C3 C4 1.377(6) . ? C4 C5 1.499(5) . ? N3 C7 1.340(5) . ? N3 N4 1.384(4) . ? N4 C9 1.354(5) . ? N4 B1 1.543(6) . ? C6 C7 1.501(5) . ? C7 C8 1.389(6) . ? C8 C9 1.379(6) . ? C9 C10 1.491(5) . ? N5 C12 1.351(5) . ? N5 N6 1.374(4) . ? N6 C14 1.354(5) . ? N6 B1 1.533(6) . ? C11 C12 1.491(6) . ? C12 C13 1.383(6) . ? C13 C14 1.375(6) . ? C14 C15 1.497(6) . ? C16 C17 1.319(5) . ? C16 C24 1.462(5) . ? C17 C18 1.465(5) . ? C18 C19 1.395(6) . ? C18 C23 1.401(6) . ? C19 C20 1.378(6) . ? C20 C21 1.374(6) . ? C21 C22 1.393(6) . ? C22 C23 1.386(6) . ? C24 C25 1.393(5) . ? C24 C29 1.396(6) . ? C25 C26 1.389(6) . ? C26 C27 1.365(7) . ? C27 C28 1.390(7) . ? C28 C29 1.377(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 F1 W1 F2 90.05(10) . . ? F1 W1 C17 94.75(13) . . ? F2 W1 C17 84.10(13) . . ? F1 W1 C16 108.65(12) . . ? F2 W1 C16 118.34(14) . . ? C17 W1 C16 37.78(15) . . ? F1 W1 N5 163.68(11) . . ? F2 W1 N5 86.86(11) . . ? C17 W1 N5 100.85(14) . . ? C16 W1 N5 86.84(13) . . ? F1 W1 N3 87.13(11) . . ? F2 W1 N3 158.21(11) . . ? C17 W1 N3 117.66(14) . . ? C16 W1 N3 82.91(14) . . ? N5 W1 N3 89.81(12) . . ? F1 W1 N1 84.18(11) . . ? F2 W1 N1 79.79(11) . . ? C17 W1 N1 163.85(14) . . ? C16 W1 N1 156.81(14) . . ? N5 W1 N1 79.50(12) . . ? N3 W1 N1 78.43(12) . . ? C2 N1 N2 106.5(3) . . ? C2 N1 W1 133.0(3) . . ? N2 N1 W1 119.8(2) . . ? C4 N2 N1 110.0(3) . . ? C4 N2 B1 131.3(3) . . ? N1 N2 B1 118.7(3) . . ? N1 C2 C3 109.3(4) . . ? N1 C2 C1 122.5(4) . . ? C3 C2 C1 128.1(4) . . ? C4 C3 C2 106.4(4) . . ? N2 C4 C3 107.8(4) . . ? N2 C4 C5 123.6(4) . . ? C3 C4 C5 128.6(4) . . ? C7 N3 N4 106.8(3) . . ? C7 N3 W1 132.5(3) . . ? N4 N3 W1 120.6(2) . . ? C9 N4 N3 109.1(3) . . ? C9 N4 B1 131.3(3) . . ? N3 N4 B1 119.3(3) . . ? N3 C7 C8 109.8(4) . . ? N3 C7 C6 121.4(4) . . ? C8 C7 C6 128.8(4) . . ? C9 C8 C7 106.3(4) . . ? N4 C9 C8 108.0(4) . . ? N4 C9 C10 123.4(4) . . ? C8 C9 C10 128.6(4) . . ? C12 N5 N6 107.2(3) . . ? C12 N5 W1 132.5(3) . . ? N6 N5 W1 119.8(2) . . ? C14 N6 N5 108.9(4) . . ? C14 N6 B1 129.9(3) . . ? N5 N6 B1 120.2(3) . . ? N5 C12 C13 109.1(4) . . ? N5 C12 C11 122.4(4) . . ? C13 C12 C11 128.4(4) . . ? C14 C13 C12 106.6(4) . . ? N6 C14 C13 108.2(4) . . ? N6 C14 C15 122.4(4) . . ? C13 C14 C15 129.4(4) . . ? N6 B1 N4 110.1(4) . . ? N6 B1 N2 107.2(3) . . ? N4 B1 N2 108.7(3) . . ? C17 C16 C24 143.4(4) . . ? C17 C16 W1 70.1(2) . . ? C24 C16 W1 146.5(3) . . ? C16 C17 C18 145.8(4) . . ? C16 C17 W1 72.1(3) . . ? C18 C17 W1 141.8(3) . . ? C19 C18 C23 118.6(4) . . ? C19 C18 C17 120.1(4) . . ? C23 C18 C17 121.3(4) . . ? C20 C19 C18 120.5(4) . . ? C21 C20 C19 120.5(4) . . ? C20 C21 C22 120.2(4) . . ? C23 C22 C21 119.4(4) . . ? C22 C23 C18 120.6(4) . . ? C25 C24 C29 118.4(4) . . ? C25 C24 C16 121.4(4) . . ? C29 C24 C16 120.2(4) . . ? C26 C25 C24 120.8(4) . . ? C27 C26 C25 119.7(4) . . ? C26 C27 C28 120.6(4) . . ? C29 C28 C27 119.7(4) . . ? C28 C29 C24 120.7(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.662 _refine_diff_density_min -1.206 _refine_diff_density_rms 0.114 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 697674' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H32 B Cl2 N6 W' _chemical_formula_sum 'C29 H32 B Cl2 N6 W' _chemical_formula_weight 730.17 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' 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 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 17.400(2) _cell_length_b 9.4934(15) _cell_length_c 18.149(3) _cell_angle_alpha 90.00 _cell_angle_beta 109.290(11) _cell_angle_gamma 90.00 _cell_volume 2829.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 230 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 24.962 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.025 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.714 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1444 _exptl_absorpt_coefficient_mu 4.302 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5753979 _exptl_absorpt_correction_T_max 0.9 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 24031 _diffrn_reflns_av_R_equivalents 0.0695 _diffrn_reflns_av_sigmaI/netI 0.1229 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5523 _reflns_number_gt 3889 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 1998)' _computing_cell_refinement 'Bruker SMART (Bruker, 1998)' _computing_data_reduction 'Bruker SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1998)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1998)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+3.0233P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5523 _refine_ls_number_parameters 358 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0540 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_ref 0.0928 _refine_ls_wR_factor_gt 0.0720 _refine_ls_goodness_of_fit_ref 0.803 _refine_ls_restrained_S_all 0.803 _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 0.228559(16) 1.06023(3) 0.260787(18) 0.01618(8) Uani 1 1 d . . . Cl1 Cl 0.26396(10) 1.29952(16) 0.24390(11) 0.0229(3) Uani 1 1 d . . . Cl2 Cl 0.11387(9) 1.04638(18) 0.14031(10) 0.0239(4) Uani 1 1 d . . . N1 N 0.1357(3) 1.1557(6) 0.3063(3) 0.0216(12) Uani 1 1 d . . . N2 N 0.1314(3) 1.1133(6) 0.3770(4) 0.0212(12) Uani 1 1 d . . . C1 C 0.0613(4) 1.3365(8) 0.2040(4) 0.0286(17) Uani 1 1 d . . . H1A H 0.1119 1.3743 0.1992 0.043 Uiso 1 1 calc R . . H1B H 0.0232 1.4138 0.2014 0.043 Uiso 1 1 calc R . . H1C H 0.0369 1.2700 0.1614 0.043 Uiso 1 1 calc R . . C2 C 0.0798(4) 1.2616(7) 0.2811(5) 0.0257(17) Uani 1 1 d . . . C3 C 0.0430(4) 1.2870(7) 0.3364(4) 0.0253(16) Uani 1 1 d . . . H3A H 0.0032 1.3569 0.3344 0.030 Uiso 1 1 calc R . . C4 C 0.0754(4) 1.1910(8) 0.3950(5) 0.0277(17) Uani 1 1 d . . . C5 C 0.0563(5) 1.1693(9) 0.4704(5) 0.038(2) Uani 1 1 d . . . H5A H 0.1070 1.1713 0.5149 0.057 Uiso 1 1 calc R . . H5B H 0.0295 1.0780 0.4687 0.057 Uiso 1 1 calc R . . H5C H 0.0201 1.2446 0.4761 0.057 Uiso 1 1 calc R . . N3 N 0.3038(3) 1.0804(6) 0.3843(3) 0.0191(12) Uani 1 1 d . . . N4 N 0.2749(3) 1.0308(5) 0.4407(3) 0.0173(12) Uani 1 1 d . . . C6 C 0.4371(4) 1.1780(8) 0.3805(4) 0.0229(15) Uani 1 1 d . . . H6A H 0.4299 1.1277 0.3315 0.034 Uiso 1 1 calc R . . H6B H 0.4940 1.1703 0.4144 0.034 Uiso 1 1 calc R . . H6C H 0.4231 1.2775 0.3693 0.034 Uiso 1 1 calc R . . C7 C 0.3830(4) 1.1151(7) 0.4205(4) 0.0195(14) Uani 1 1 d . . . C8 C 0.4037(4) 1.0844(7) 0.4994(4) 0.0228(15) Uani 1 1 d . . . H8A H 0.4555 1.0968 0.5381 0.027 Uiso 1 1 calc R . . C9 C 0.3346(4) 1.0323(7) 0.5106(4) 0.0207(15) Uani 1 1 d . . . C10 C 0.3233(4) 0.9904(8) 0.5857(4) 0.0253(15) Uani 1 1 d . . . H10A H 0.2888 0.9063 0.5773 0.038 Uiso 1 1 calc R . . H10B H 0.2972 1.0675 0.6045 0.038 Uiso 1 1 calc R . . H10C H 0.3764 0.9698 0.6246 0.038 Uiso 1 1 calc R . . N5 N 0.1840(3) 0.8678(6) 0.2953(3) 0.0180(12) Uani 1 1 d . . . N6 N 0.1677(3) 0.8612(6) 0.3646(3) 0.0190(12) Uani 1 1 d . . . C11 C 0.1827(4) 0.7025(7) 0.1876(4) 0.0269(16) Uani 1 1 d . . . H11A H 0.1630 0.7797 0.1502 0.040 Uiso 1 1 calc R . . H11B H 0.1526 0.6162 0.1663 0.040 Uiso 1 1 calc R . . H11C H 0.2409 0.6875 0.1970 0.040 Uiso 1 1 calc R . . C12 C 0.1698(4) 0.7392(7) 0.2628(4) 0.0217(15) Uani 1 1 d . . . C13 C 0.1453(4) 0.6511(7) 0.3131(4) 0.0236(15) Uani 1 1 d . . . H13A H 0.1321 0.5539 0.3051 0.028 Uiso 1 1 calc R . . C14 C 0.1439(4) 0.7291(7) 0.3745(4) 0.0201(14) Uani 1 1 d . . . C15 C 0.1223(4) 0.6860(7) 0.4447(4) 0.0247(15) Uani 1 1 d . . . H15A H 0.0908 0.5984 0.4334 0.037 Uiso 1 1 calc R . . H15B H 0.0898 0.7603 0.4577 0.037 Uiso 1 1 calc R . . H15C H 0.1723 0.6712 0.4890 0.037 Uiso 1 1 calc R . . B1 B 0.1852(5) 0.9909(9) 0.4204(5) 0.0227(17) Uani 1 1 d . . . H1 H 0.1727 0.9676 0.4690 0.027 Uiso 1 1 calc R . . C16 C 0.3259(4) 0.9433(7) 0.2560(4) 0.0188(13) Uani 1 1 d . . . C17 C 0.2907(4) 1.0019(7) 0.1886(4) 0.0156(13) Uani 1 1 d . . . C18 C 0.2934(4) 1.0044(7) 0.1092(4) 0.0177(14) Uani 1 1 d . . . C19 C 0.2593(4) 1.1131(7) 0.0571(4) 0.0196(14) Uani 1 1 d . . . H19A H 0.2318 1.1884 0.0722 0.024 Uiso 1 1 calc R . . C20 C 0.2658(4) 1.1106(7) -0.0170(4) 0.0224(15) Uani 1 1 d . . . H20A H 0.2437 1.1859 -0.0520 0.027 Uiso 1 1 calc R . . C21 C 0.3039(4) 1.0009(8) -0.0407(4) 0.0227(15) Uani 1 1 d . . . H21A H 0.3083 1.0009 -0.0915 0.027 Uiso 1 1 calc R . . C22 C 0.3356(4) 0.8909(7) 0.0102(4) 0.0193(14) Uani 1 1 d . . . H22A H 0.3603 0.8134 -0.0064 0.023 Uiso 1 1 calc R . . C23 C 0.3316(4) 0.8925(7) 0.0837(4) 0.0206(14) Uani 1 1 d . . . H23A H 0.3550 0.8173 0.1184 0.025 Uiso 1 1 calc R . . C24 C 0.3927(4) 0.8470(7) 0.2949(4) 0.0195(14) Uani 1 1 d . . . C25 C 0.4634(4) 0.8479(7) 0.2747(4) 0.0220(15) Uani 1 1 d . . . H25A H 0.4688 0.9133 0.2371 0.026 Uiso 1 1 calc R . . C26 C 0.5256(4) 0.7541(8) 0.3091(4) 0.0244(16) Uani 1 1 d . . . H26A H 0.5742 0.7556 0.2961 0.029 Uiso 1 1 calc R . . C27 C 0.5162(4) 0.6576(8) 0.3628(5) 0.0295(17) Uani 1 1 d . . . H27A H 0.5586 0.5921 0.3857 0.035 Uiso 1 1 calc R . . C28 C 0.4482(4) 0.6542(8) 0.3836(5) 0.0320(18) Uani 1 1 d . . . H28A H 0.4432 0.5869 0.4205 0.038 Uiso 1 1 calc R . . C29 C 0.3861(4) 0.7496(8) 0.3506(4) 0.0269(16) Uani 1 1 d . . . H29A H 0.3388 0.7492 0.3658 0.032 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 0.01598(13) 0.01650(13) 0.01706(13) 0.00054(13) 0.00684(9) 0.00047(12) Cl1 0.0248(8) 0.0183(8) 0.0269(8) 0.0018(8) 0.0103(6) -0.0012(7) Cl2 0.0192(8) 0.0282(9) 0.0224(8) 0.0009(7) 0.0045(7) -0.0010(7) N1 0.020(3) 0.018(3) 0.030(3) -0.002(3) 0.013(3) -0.002(2) N2 0.020(3) 0.017(3) 0.028(3) -0.007(3) 0.011(3) -0.003(2) C1 0.024(4) 0.021(4) 0.037(4) -0.003(3) 0.005(3) 0.003(3) C2 0.014(3) 0.020(4) 0.041(5) -0.005(3) 0.007(3) -0.002(3) C3 0.022(3) 0.018(4) 0.037(4) -0.005(3) 0.011(3) 0.000(3) C4 0.020(3) 0.028(4) 0.038(4) -0.012(4) 0.014(3) -0.004(3) C5 0.043(5) 0.035(5) 0.050(5) -0.010(4) 0.035(4) 0.000(4) N3 0.021(3) 0.016(3) 0.022(3) 0.001(2) 0.010(2) 0.003(2) N4 0.020(3) 0.014(3) 0.020(3) -0.004(2) 0.010(2) -0.001(2) C6 0.022(3) 0.027(4) 0.021(3) 0.004(3) 0.009(3) -0.002(3) C7 0.015(3) 0.020(3) 0.023(4) 0.001(3) 0.006(3) 0.001(3) C8 0.022(3) 0.025(4) 0.020(4) -0.003(3) 0.005(3) 0.002(3) C9 0.031(4) 0.015(3) 0.017(3) -0.004(3) 0.009(3) 0.003(3) C10 0.034(4) 0.022(4) 0.022(4) -0.002(3) 0.012(3) 0.000(3) N5 0.019(3) 0.018(3) 0.016(3) -0.001(2) 0.004(2) -0.003(2) N6 0.018(3) 0.020(3) 0.021(3) 0.000(2) 0.009(2) 0.001(2) C11 0.037(4) 0.018(4) 0.028(4) -0.004(3) 0.015(3) -0.003(3) C12 0.023(3) 0.017(3) 0.024(4) 0.001(3) 0.005(3) 0.003(3) C13 0.027(4) 0.017(3) 0.028(4) 0.002(3) 0.009(3) -0.005(3) C14 0.016(3) 0.018(3) 0.025(4) 0.005(3) 0.005(3) 0.005(3) C15 0.025(4) 0.023(4) 0.029(4) 0.006(3) 0.012(3) -0.001(3) B1 0.023(4) 0.028(4) 0.021(4) 0.001(4) 0.013(3) 0.002(3) C16 0.022(3) 0.016(3) 0.020(3) -0.006(3) 0.009(3) -0.003(3) C17 0.018(3) 0.014(3) 0.015(3) -0.006(3) 0.006(3) -0.006(3) C18 0.017(3) 0.019(3) 0.018(3) -0.003(3) 0.007(3) -0.005(3) C19 0.021(3) 0.017(3) 0.022(4) -0.002(3) 0.007(3) -0.002(3) C20 0.021(3) 0.022(3) 0.022(4) 0.004(3) 0.004(3) -0.005(3) C21 0.021(3) 0.027(4) 0.020(4) -0.004(3) 0.007(3) -0.006(3) C22 0.018(3) 0.021(3) 0.019(3) -0.008(3) 0.007(3) -0.003(3) C23 0.023(3) 0.015(3) 0.024(4) 0.002(3) 0.006(3) -0.002(3) C24 0.019(3) 0.023(4) 0.015(3) -0.001(3) 0.003(3) 0.004(3) C25 0.021(3) 0.029(4) 0.017(3) 0.003(3) 0.008(3) -0.001(3) C26 0.014(3) 0.038(4) 0.020(4) -0.007(3) 0.004(3) 0.001(3) C27 0.023(4) 0.032(4) 0.030(4) -0.002(4) 0.003(3) 0.008(3) C28 0.025(4) 0.032(4) 0.036(4) 0.015(4) 0.007(3) 0.005(3) C29 0.022(4) 0.038(4) 0.023(4) 0.004(3) 0.011(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 C17 2.032(6) . ? W1 C16 2.050(6) . ? W1 N5 2.157(5) . ? W1 N3 2.199(6) . ? W1 N1 2.234(5) . ? W1 Cl1 2.3996(16) . ? W1 Cl2 2.4284(17) . ? N1 C2 1.368(9) . ? N1 N2 1.371(8) . ? N2 C4 1.346(9) . ? N2 B1 1.537(10) . ? C1 C2 1.505(10) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.381(10) . ? C3 C4 1.373(10) . ? C3 H3A 0.9500 . ? C4 C5 1.525(11) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? N3 C7 1.358(8) . ? N3 N4 1.364(8) . ? N4 C9 1.349(9) . ? N4 B1 1.528(9) . ? C6 C7 1.490(9) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.386(10) . ? C8 C9 1.376(10) . ? C8 H8A 0.9500 . ? C9 C10 1.494(10) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? N5 C12 1.342(8) . ? N5 N6 1.380(8) . ? N6 C14 1.351(8) . ? N6 B1 1.559(10) . ? C11 C12 1.495(10) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.405(9) . ? C13 C14 1.346(10) . ? C13 H13A 0.9500 . ? C14 C15 1.499(9) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? B1 H1 1.0000 . ? C16 C17 1.300(9) . ? C16 C24 1.464(9) . ? C17 C18 1.456(9) . ? C18 C19 1.393(9) . ? C18 C23 1.411(10) . ? C19 C20 1.385(10) . ? C19 H19A 0.9500 . ? C20 C21 1.376(10) . ? C20 H20A 0.9500 . ? C21 C22 1.383(10) . ? C21 H21A 0.9500 . ? C22 C23 1.359(10) . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? C24 C25 1.395(9) . ? C24 C29 1.403(10) . ? C25 C26 1.381(9) . ? C25 H25A 0.9500 . ? C26 C27 1.386(10) . ? C26 H26A 0.9500 . ? C27 C28 1.356(11) . ? C27 H27A 0.9500 . ? C28 C29 1.385(10) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? 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 C17 W1 C16 37.1(3) . . ? C17 W1 N5 106.0(2) . . ? C16 W1 N5 86.3(2) . . ? C17 W1 N3 114.6(2) . . ? C16 W1 N3 82.4(2) . . ? N5 W1 N3 85.9(2) . . ? C17 W1 N1 162.2(2) . . ? C16 W1 N1 160.6(2) . . ? N5 W1 N1 82.2(2) . . ? N3 W1 N1 81.2(2) . . ? C17 W1 Cl1 87.81(19) . . ? C16 W1 Cl1 104.86(19) . . ? N5 W1 Cl1 166.18(15) . . ? N3 W1 Cl1 87.49(15) . . ? N1 W1 Cl1 84.87(14) . . ? C17 W1 Cl2 81.87(18) . . ? C16 W1 Cl2 112.17(19) . . ? N5 W1 Cl2 87.04(15) . . ? N3 W1 Cl2 163.29(14) . . ? N1 W1 Cl2 82.83(15) . . ? Cl1 W1 Cl2 96.05(6) . . ? C2 N1 N2 106.0(6) . . ? C2 N1 W1 134.1(5) . . ? N2 N1 W1 119.8(4) . . ? C4 N2 N1 109.6(6) . . ? C4 N2 B1 131.0(7) . . ? N1 N2 B1 119.3(5) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 109.6(7) . . ? N1 C2 C1 124.6(6) . . ? C3 C2 C1 125.8(6) . . ? C4 C3 C2 106.1(6) . . ? C4 C3 H3A 127.0 . . ? C2 C3 H3A 127.0 . . ? N2 C4 C3 108.7(7) . . ? N2 C4 C5 122.3(7) . . ? C3 C4 C5 129.0(7) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 N3 N4 106.7(5) . . ? C7 N3 W1 133.0(4) . . ? N4 N3 W1 119.5(4) . . ? C9 N4 N3 110.0(5) . . ? C9 N4 B1 129.5(6) . . ? N3 N4 B1 120.3(6) . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N3 C7 C8 108.9(6) . . ? N3 C7 C6 124.4(6) . . ? C8 C7 C6 126.7(6) . . ? C9 C8 C7 106.7(6) . . ? C9 C8 H8A 126.7 . . ? C7 C8 H8A 126.7 . . ? N4 C9 C8 107.6(7) . . ? N4 C9 C10 124.3(6) . . ? C8 C9 C10 128.0(7) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 N5 N6 107.2(5) . . ? C12 N5 W1 132.4(5) . . ? N6 N5 W1 120.3(4) . . ? C14 N6 N5 109.1(6) . . ? C14 N6 B1 130.5(6) . . ? N5 N6 B1 120.1(5) . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N5 C12 C13 107.9(6) . . ? N5 C12 C11 123.5(6) . . ? C13 C12 C11 128.5(6) . . ? C14 C13 C12 107.6(6) . . ? C14 C13 H13A 126.2 . . ? C12 C13 H13A 126.2 . . ? C13 C14 N6 108.1(6) . . ? C13 C14 C15 129.2(6) . . ? N6 C14 C15 122.7(6) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N4 B1 N2 109.6(6) . . ? N4 B1 N6 108.5(5) . . ? N2 B1 N6 108.0(6) . . ? N4 B1 H1 110.2 . . ? N2 B1 H1 110.2 . . ? N6 B1 H1 110.2 . . ? C17 C16 C24 140.7(6) . . ? C17 C16 W1 70.7(4) . . ? C24 C16 W1 148.6(5) . . ? C16 C17 C18 141.3(7) . . ? C16 C17 W1 72.2(4) . . ? C18 C17 W1 146.2(5) . . ? C19 C18 C23 118.4(6) . . ? C19 C18 C17 122.6(6) . . ? C23 C18 C17 119.0(6) . . ? C20 C19 C18 119.6(7) . . ? C20 C19 H19A 120.2 . . ? C18 C19 H19A 120.2 . . ? C21 C20 C19 121.2(7) . . ? C21 C20 H20A 119.4 . . ? C19 C20 H20A 119.4 . . ? C20 C21 C22 119.3(7) . . ? C20 C21 H21A 120.4 . . ? C22 C21 H21A 120.4 . . ? C23 C22 C21 120.6(7) . . ? C23 C22 H22A 119.7 . . ? C21 C22 H22A 119.7 . . ? C22 C23 C18 120.9(7) . . ? C22 C23 H23A 119.5 . . ? C18 C23 H23A 119.5 . . ? C25 C24 C29 118.9(6) . . ? C25 C24 C16 119.9(6) . . ? C29 C24 C16 121.2(6) . . ? C26 C25 C24 120.2(7) . . ? C26 C25 H25A 119.9 . . ? C24 C25 H25A 119.9 . . ? C25 C26 C27 119.2(6) . . ? C25 C26 H26A 120.4 . . ? C27 C26 H26A 120.4 . . ? C28 C27 C26 121.9(7) . . ? C28 C27 H27A 119.1 . . ? C26 C27 H27A 119.1 . . ? C27 C28 C29 119.5(7) . . ? C27 C28 H28A 120.3 . . ? C29 C28 H28A 120.3 . . ? C28 C29 C24 120.3(6) . . ? C28 C29 H29A 119.9 . . ? C24 C29 H29A 119.9 . . ? _diffrn_measured_fraction_theta_max 0.849 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.849 _refine_diff_density_max 2.162 _refine_diff_density_min -1.029 _refine_diff_density_rms 0.147 #===END data_7 _database_code_depnum_ccdc_archive 'CCDC 697675' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H32 B F2 Mo N6' _chemical_formula_sum 'C29 H32 B F2 Mo N6' _chemical_formula_weight 609.36 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' F F 0.0171 0.0103 '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 9.718(3) _cell_length_b 32.315(11) _cell_length_c 9.779(3) _cell_angle_alpha 90.00 _cell_angle_beta 113.270(5) _cell_angle_gamma 90.00 _cell_volume 2821.1(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 128 _cell_measurement_theta_min 2.5805 _cell_measurement_theta_max 27.275 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.435 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1252 _exptl_absorpt_coefficient_mu 0.508 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.879 _exptl_absorpt_correction_T_max 0.9 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 29496 _diffrn_reflns_av_R_equivalents 0.0932 _diffrn_reflns_av_sigmaI/netI 0.3434 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 27.54 _reflns_number_total 6472 _reflns_number_gt 2099 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 1998)' _computing_cell_refinement 'Bruker SMART (Bruker, 1998)' _computing_data_reduction 'Bruker SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1998)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1998)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6472 _refine_ls_number_parameters 358 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0651 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.0715 _refine_ls_wR_factor_gt 0.0666 _refine_ls_goodness_of_fit_ref 0.340 _refine_ls_restrained_S_all 0.340 _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 Mo1 Mo 1.08528(4) 0.126049(11) 0.61673(4) 0.02304(9) Uani 1 1 d . . . F1 F 1.1547(2) 0.16270(6) 0.7926(2) 0.0295(5) Uani 1 1 d . . . F2 F 1.2685(2) 0.09533(6) 0.6855(2) 0.0346(6) Uani 1 1 d . . . N1 N 1.0246(3) 0.08588(9) 0.7725(3) 0.0220(7) Uani 1 1 d . . . N2 N 0.8818(3) 0.07035(9) 0.7271(3) 0.0238(8) Uani 1 1 d . . . C1 C 1.2555(4) 0.08817(11) 1.0039(4) 0.0356(11) Uani 1 1 d . . . H1A H 1.3126 0.0851 0.9414 0.053 Uiso 1 1 calc R . . H1B H 1.2981 0.0701 1.0912 0.053 Uiso 1 1 calc R . . H1C H 1.2605 0.1170 1.0365 0.053 Uiso 1 1 calc R . . C2 C 1.0960(4) 0.07647(11) 0.9167(4) 0.0255(9) Uani 1 1 d . . . C3 C 0.9968(4) 0.05495(12) 0.9621(4) 0.0319(10) Uani 1 1 d . . . H3A H 1.0182 0.0443 1.0590 0.038 Uiso 1 1 calc R . . C4 C 0.8646(4) 0.05198(11) 0.8432(4) 0.0273(10) Uani 1 1 d . . . C5 C 0.7176(4) 0.03454(12) 0.8332(4) 0.0402(12) Uani 1 1 d . . . H5A H 0.6810 0.0144 0.7518 0.060 Uiso 1 1 calc R . . H5B H 0.6445 0.0570 0.8140 0.060 Uiso 1 1 calc R . . H5C H 0.7314 0.0209 0.9272 0.060 Uiso 1 1 calc R . . N3 N 0.9809(3) 0.07361(9) 0.4727(3) 0.0241(8) Uani 1 1 d . . . N4 N 0.8413(3) 0.05974(9) 0.4591(3) 0.0237(8) Uani 1 1 d . . . C6 C 1.1671(4) 0.05798(11) 0.3662(4) 0.0316(10) Uani 1 1 d . . . H6A H 1.2440 0.0646 0.4644 0.047 Uiso 1 1 calc R . . H6B H 1.1573 0.0810 0.2978 0.047 Uiso 1 1 calc R . . H6C H 1.1959 0.0329 0.3278 0.047 Uiso 1 1 calc R . . C7 C 1.0203(4) 0.05100(11) 0.3790(4) 0.0222(9) Uani 1 1 d . . . C8 C 0.9088(4) 0.02242(11) 0.3075(4) 0.0297(10) Uani 1 1 d . . . H8A H 0.9093 0.0023 0.2368 0.036 Uiso 1 1 calc R . . C9 C 0.7991(4) 0.02851(11) 0.3576(4) 0.0250(9) Uani 1 1 d . . . C10 C 0.6492(4) 0.00730(11) 0.3104(4) 0.0373(11) Uani 1 1 d . . . H10A H 0.6542 -0.0199 0.2680 0.056 Uiso 1 1 calc R . . H10B H 0.5724 0.0242 0.2356 0.056 Uiso 1 1 calc R . . H10C H 0.6236 0.0037 0.3972 0.056 Uiso 1 1 calc R . . N5 N 0.8619(3) 0.14951(9) 0.5749(3) 0.0230(8) Uani 1 1 d . . . N6 N 0.7427(3) 0.12346(10) 0.5376(3) 0.0231(7) Uani 1 1 d . . . C11 C 0.9047(4) 0.22599(11) 0.5911(5) 0.0417(12) Uani 1 1 d . . . H11A H 1.0038 0.2198 0.6679 0.063 Uiso 1 1 calc R . . H11B H 0.8589 0.2487 0.6251 0.063 Uiso 1 1 calc R . . H11C H 0.9148 0.2341 0.4990 0.063 Uiso 1 1 calc R . . C12 C 0.8080(4) 0.18847(12) 0.5630(4) 0.0265(10) Uani 1 1 d . . . C13 C 0.6516(4) 0.18617(12) 0.5179(4) 0.0268(10) Uani 1 1 d . . . H13A H 0.5843 0.2088 0.5009 0.032 Uiso 1 1 calc R . . C14 C 0.6156(4) 0.14508(12) 0.5034(4) 0.0246(9) Uani 1 1 d . . . C15 C 0.4650(4) 0.12530(13) 0.4583(4) 0.0413(11) Uani 1 1 d . . . H15A H 0.4614 0.1001 0.4009 0.062 Uiso 1 1 calc R . . H15B H 0.3876 0.1446 0.3969 0.062 Uiso 1 1 calc R . . H15C H 0.4474 0.1181 0.5474 0.062 Uiso 1 1 calc R . . B1 B 0.7714(5) 0.07647(13) 0.5631(5) 0.0245(11) Uani 1 1 d . . . H1 H 0.6751 0.0618 0.5446 0.029 Uiso 1 1 calc R . . C16 C 1.0600(4) 0.15377(11) 0.4189(4) 0.0241(9) Uani 1 1 d . . . C17 C 1.1659(4) 0.17178(11) 0.5273(4) 0.0259(9) Uani 1 1 d . . . C18 C 1.2774(4) 0.20501(11) 0.5761(4) 0.0238(9) Uani 1 1 d . . . C19 C 1.4052(4) 0.20130(12) 0.7076(4) 0.0284(10) Uani 1 1 d . . . H19A H 1.4214 0.1769 0.7660 0.034 Uiso 1 1 calc R . . C20 C 1.5072(4) 0.23294(12) 0.7525(4) 0.0328(11) Uani 1 1 d . . . H20A H 1.5952 0.2299 0.8408 0.039 Uiso 1 1 calc R . . C21 C 1.4844(4) 0.26909(12) 0.6718(5) 0.0375(11) Uani 1 1 d . . . H21A H 1.5561 0.2907 0.7055 0.045 Uiso 1 1 calc R . . C22 C 1.3592(5) 0.27407(12) 0.5433(5) 0.0373(11) Uani 1 1 d . . . H22A H 1.3423 0.2992 0.4885 0.045 Uiso 1 1 calc R . . C23 C 1.2578(4) 0.24179(12) 0.4949(4) 0.0326(10) Uani 1 1 d . . . H23A H 1.1725 0.2447 0.4041 0.039 Uiso 1 1 calc R . . C24 C 0.9732(4) 0.15391(11) 0.2586(4) 0.0234(9) Uani 1 1 d . . . C25 C 1.0344(4) 0.16737(11) 0.1618(4) 0.0299(10) Uani 1 1 d . . . H25A H 1.1341 0.1777 0.2016 0.036 Uiso 1 1 calc R . . C26 C 0.9577(5) 0.16658(12) 0.0093(5) 0.0356(11) Uani 1 1 d . . . H26A H 1.0042 0.1751 -0.0552 0.043 Uiso 1 1 calc R . . C27 C 0.8088(5) 0.15274(12) -0.0474(5) 0.0448(12) Uani 1 1 d . . . H27A H 0.7529 0.1523 -0.1520 0.054 Uiso 1 1 calc R . . C28 C 0.7431(5) 0.13990(12) 0.0449(5) 0.0394(11) Uani 1 1 d . . . H28A H 0.6420 0.1307 0.0049 0.047 Uiso 1 1 calc R . . C29 C 0.8251(4) 0.14030(11) 0.1993(4) 0.0343(11) Uani 1 1 d . . . H29A H 0.7794 0.1313 0.2639 0.041 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 Mo1 0.02339(17) 0.02374(18) 0.01986(18) -0.00215(19) 0.00625(14) -0.00562(19) F1 0.0313(13) 0.0293(14) 0.0271(14) -0.0043(11) 0.0107(11) -0.0083(10) F2 0.0266(13) 0.0395(15) 0.0339(15) -0.0002(11) 0.0079(11) 0.0032(11) N1 0.0200(18) 0.0197(19) 0.025(2) -0.0019(15) 0.0071(16) -0.0034(14) N2 0.0258(19) 0.0184(19) 0.026(2) -0.0020(15) 0.0086(17) -0.0026(15) C1 0.036(3) 0.033(3) 0.026(3) 0.005(2) 0.000(2) -0.004(2) C2 0.036(3) 0.018(2) 0.019(2) -0.0011(18) 0.008(2) -0.0043(19) C3 0.040(3) 0.031(3) 0.023(3) 0.006(2) 0.010(2) -0.001(2) C4 0.034(3) 0.022(2) 0.026(3) -0.0043(19) 0.013(2) -0.0041(19) C5 0.046(3) 0.041(3) 0.042(3) 0.004(2) 0.026(2) -0.008(2) N3 0.0216(18) 0.0213(19) 0.026(2) 0.0023(15) 0.0049(16) -0.0016(15) N4 0.0212(18) 0.023(2) 0.023(2) 0.0016(15) 0.0040(16) -0.0057(15) C6 0.030(2) 0.038(3) 0.025(3) -0.007(2) 0.008(2) 0.000(2) C7 0.027(2) 0.020(2) 0.018(2) 0.0002(17) 0.0072(19) 0.0020(18) C8 0.038(3) 0.023(2) 0.027(2) -0.0027(19) 0.011(2) -0.002(2) C9 0.025(2) 0.019(2) 0.024(2) -0.0033(18) 0.002(2) -0.0038(18) C10 0.039(3) 0.030(3) 0.036(3) -0.007(2) 0.006(2) -0.011(2) N5 0.0220(18) 0.0212(19) 0.024(2) -0.0021(15) 0.0074(16) -0.0050(15) N6 0.0177(16) 0.0219(18) 0.0284(19) -0.0013(17) 0.0076(15) -0.0036(16) C11 0.037(3) 0.030(3) 0.051(3) -0.002(2) 0.010(2) -0.003(2) C12 0.034(3) 0.018(2) 0.029(3) 0.0041(19) 0.013(2) 0.000(2) C13 0.024(2) 0.027(2) 0.028(3) 0.0044(19) 0.009(2) 0.0071(19) C14 0.020(2) 0.033(3) 0.020(2) 0.0033(19) 0.0071(19) 0.0034(19) C15 0.028(2) 0.045(3) 0.044(3) -0.004(3) 0.008(2) 0.003(2) B1 0.019(2) 0.024(3) 0.027(3) -0.004(2) 0.005(2) -0.009(2) C16 0.021(2) 0.019(2) 0.033(3) -0.0032(19) 0.012(2) 0.0052(18) C17 0.022(2) 0.024(2) 0.029(3) 0.0071(19) 0.007(2) 0.0061(18) C18 0.026(2) 0.023(2) 0.018(2) 0.0005(18) 0.004(2) -0.0032(19) C19 0.029(2) 0.026(2) 0.030(3) 0.002(2) 0.011(2) -0.0020(19) C20 0.025(2) 0.036(3) 0.030(3) -0.006(2) 0.003(2) -0.008(2) C21 0.040(3) 0.029(3) 0.041(3) -0.003(2) 0.014(2) -0.019(2) C22 0.045(3) 0.030(3) 0.032(3) 0.008(2) 0.011(2) -0.008(2) C23 0.031(3) 0.034(3) 0.028(3) 0.007(2) 0.006(2) -0.007(2) C24 0.028(2) 0.019(2) 0.021(2) -0.0023(18) 0.007(2) 0.0030(18) C25 0.037(3) 0.026(3) 0.025(3) 0.000(2) 0.010(2) 0.004(2) C26 0.049(3) 0.028(3) 0.031(3) 0.004(2) 0.017(2) 0.008(2) C27 0.065(4) 0.035(3) 0.022(3) -0.004(2) 0.004(3) 0.016(2) C28 0.038(3) 0.039(3) 0.029(3) 0.006(2) 0.000(2) 0.002(2) C29 0.038(3) 0.030(3) 0.031(3) 0.000(2) 0.009(2) -0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 F2 1.914(2) . ? Mo1 F1 1.974(2) . ? Mo1 C17 2.026(4) . ? Mo1 C16 2.057(4) . ? Mo1 N5 2.180(3) . ? Mo1 N3 2.181(3) . ? Mo1 N1 2.250(3) . ? N1 C2 1.338(4) . ? N1 N2 1.374(3) . ? N2 C4 1.348(4) . ? N2 B1 1.551(5) . ? C1 C2 1.493(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.396(5) . ? C3 C4 1.353(5) . ? C3 H3A 0.9500 . ? C4 C5 1.503(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? N3 C7 1.341(4) . ? N3 N4 1.384(3) . ? N4 C9 1.360(4) . ? N4 B1 1.528(5) . ? C6 C7 1.498(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.385(5) . ? C8 C9 1.351(5) . ? C8 H8A 0.9500 . ? C9 C10 1.508(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? N5 C12 1.351(4) . ? N5 N6 1.360(4) . ? N6 C14 1.341(4) . ? N6 B1 1.546(5) . ? C11 C12 1.491(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.407(5) . ? C13 C14 1.366(5) . ? C13 H13A 0.9500 . ? C14 C15 1.495(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? B1 H1 1.0000 . ? C16 C17 1.288(5) . ? C16 C24 1.458(5) . ? C17 C18 1.464(5) . ? C18 C19 1.396(5) . ? C18 C23 1.400(5) . ? C19 C20 1.370(5) . ? C19 H19A 0.9500 . ? C20 C21 1.378(5) . ? C20 H20A 0.9500 . ? C21 C22 1.370(5) . ? C21 H21A 0.9500 . ? C22 C23 1.384(5) . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? C24 C25 1.372(5) . ? C24 C29 1.394(5) . ? C25 C26 1.379(5) . ? C25 H25A 0.9500 . ? C26 C27 1.403(5) . ? C26 H26A 0.9500 . ? C27 C28 1.361(5) . ? C27 H27A 0.9500 . ? C28 C29 1.401(5) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? 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 F2 Mo1 F1 93.15(9) . . ? F2 Mo1 C17 93.72(12) . . ? F1 Mo1 C17 83.17(13) . . ? F2 Mo1 C16 107.76(11) . . ? F1 Mo1 C16 115.51(12) . . ? C17 Mo1 C16 36.78(13) . . ? F2 Mo1 N5 164.95(10) . . ? F1 Mo1 N5 85.82(10) . . ? C17 Mo1 N5 101.05(13) . . ? C16 Mo1 N5 86.10(12) . . ? F2 Mo1 N3 87.41(10) . . ? F1 Mo1 N3 160.11(9) . . ? C17 Mo1 N3 116.66(14) . . ? C16 Mo1 N3 83.04(13) . . ? N5 Mo1 N3 88.52(11) . . ? F2 Mo1 N1 85.37(10) . . ? F1 Mo1 N1 81.22(9) . . ? C17 Mo1 N1 164.28(13) . . ? C16 Mo1 N1 157.25(13) . . ? N5 Mo1 N1 79.63(10) . . ? N3 Mo1 N1 79.01(11) . . ? C2 N1 N2 107.1(3) . . ? C2 N1 Mo1 132.8(2) . . ? N2 N1 Mo1 119.6(2) . . ? C4 N2 N1 109.5(3) . . ? C4 N2 B1 131.5(3) . . ? N1 N2 B1 119.0(3) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 108.3(3) . . ? N1 C2 C1 122.2(3) . . ? C3 C2 C1 129.5(4) . . ? C4 C3 C2 107.6(4) . . ? C4 C3 H3A 126.2 . . ? C2 C3 H3A 126.2 . . ? N2 C4 C3 107.5(3) . . ? N2 C4 C5 122.7(4) . . ? C3 C4 C5 129.6(4) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 N3 N4 106.9(3) . . ? C7 N3 Mo1 132.8(2) . . ? N4 N3 Mo1 120.1(2) . . ? C9 N4 N3 108.2(3) . . ? C9 N4 B1 131.6(3) . . ? N3 N4 B1 119.9(3) . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N3 C7 C8 109.3(3) . . ? N3 C7 C6 120.9(3) . . ? C8 C7 C6 129.7(3) . . ? C9 C8 C7 107.0(3) . . ? C9 C8 H8A 126.5 . . ? C7 C8 H8A 126.5 . . ? C8 C9 N4 108.6(3) . . ? C8 C9 C10 128.9(4) . . ? N4 C9 C10 122.4(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 N5 N6 107.1(3) . . ? C12 N5 Mo1 131.6(2) . . ? N6 N5 Mo1 121.0(2) . . ? C14 N6 N5 110.3(3) . . ? C14 N6 B1 129.9(3) . . ? N5 N6 B1 119.0(3) . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N5 C12 C13 108.2(3) . . ? N5 C12 C11 123.2(3) . . ? C13 C12 C11 128.6(4) . . ? C14 C13 C12 106.5(3) . . ? C14 C13 H13A 126.7 . . ? C12 C13 H13A 126.7 . . ? N6 C14 C13 107.9(3) . . ? N6 C14 C15 123.3(3) . . ? C13 C14 C15 128.8(3) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N4 B1 N6 109.8(3) . . ? N4 B1 N2 109.6(3) . . ? N6 B1 N2 107.4(3) . . ? N4 B1 H1 110.0 . . ? N6 B1 H1 110.0 . . ? N2 B1 H1 110.0 . . ? C17 C16 C24 144.9(4) . . ? C17 C16 Mo1 70.3(2) . . ? C24 C16 Mo1 144.7(3) . . ? C16 C17 C18 147.9(4) . . ? C16 C17 Mo1 72.9(2) . . ? C18 C17 Mo1 139.2(3) . . ? C19 C18 C23 117.9(4) . . ? C19 C18 C17 120.8(3) . . ? C23 C18 C17 121.4(3) . . ? C20 C19 C18 119.9(4) . . ? C20 C19 H19A 120.0 . . ? C18 C19 H19A 120.0 . . ? C19 C20 C21 121.1(4) . . ? C19 C20 H20A 119.4 . . ? C21 C20 H20A 119.4 . . ? C22 C21 C20 120.6(4) . . ? C22 C21 H21A 119.7 . . ? C20 C21 H21A 119.7 . . ? C21 C22 C23 118.6(4) . . ? C21 C22 H22A 120.7 . . ? C23 C22 H22A 120.7 . . ? C22 C23 C18 121.8(4) . . ? C22 C23 H23A 119.1 . . ? C18 C23 H23A 119.1 . . ? C25 C24 C29 118.1(4) . . ? C25 C24 C16 121.2(4) . . ? C29 C24 C16 120.6(3) . . ? C24 C25 C26 122.9(4) . . ? C24 C25 H25A 118.5 . . ? C26 C25 H25A 118.5 . . ? C25 C26 C27 117.8(4) . . ? C25 C26 H26A 121.1 . . ? C27 C26 H26A 121.1 . . ? C28 C27 C26 121.1(4) . . ? C28 C27 H27A 119.5 . . ? C26 C27 H27A 119.5 . . ? C27 C28 C29 119.7(4) . . ? C27 C28 H28A 120.1 . . ? C29 C28 H28A 120.1 . . ? C24 C29 C28 120.3(4) . . ? C24 C29 H29A 119.8 . . ? C28 C29 H29A 119.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag F2 Mo1 N1 C2 51.4(3) . . . . ? F1 Mo1 N1 C2 -42.5(3) . . . . ? C17 Mo1 N1 C2 -35.9(6) . . . . ? C16 Mo1 N1 C2 178.2(3) . . . . ? N5 Mo1 N1 C2 -129.8(3) . . . . ? N3 Mo1 N1 C2 139.7(3) . . . . ? F2 Mo1 N1 N2 -138.1(2) . . . . ? F1 Mo1 N1 N2 128.0(2) . . . . ? C17 Mo1 N1 N2 134.6(4) . . . . ? C16 Mo1 N1 N2 -11.3(4) . . . . ? N5 Mo1 N1 N2 40.7(2) . . . . ? N3 Mo1 N1 N2 -49.8(2) . . . . ? C2 N1 N2 C4 0.8(4) . . . . ? Mo1 N1 N2 C4 -171.9(2) . . . . ? C2 N1 N2 B1 -179.9(3) . . . . ? Mo1 N1 N2 B1 7.4(4) . . . . ? N2 N1 C2 C3 -0.2(4) . . . . ? Mo1 N1 C2 C3 171.2(2) . . . . ? N2 N1 C2 C1 179.4(3) . . . . ? Mo1 N1 C2 C1 -9.2(5) . . . . ? N1 C2 C3 C4 -0.6(5) . . . . ? C1 C2 C3 C4 179.9(4) . . . . ? N1 N2 C4 C3 -1.2(4) . . . . ? B1 N2 C4 C3 179.7(4) . . . . ? N1 N2 C4 C5 175.5(3) . . . . ? B1 N2 C4 C5 -3.6(6) . . . . ? C2 C3 C4 N2 1.1(5) . . . . ? C2 C3 C4 C5 -175.3(4) . . . . ? F2 Mo1 N3 C7 -48.1(3) . . . . ? F1 Mo1 N3 C7 -140.2(3) . . . . ? C17 Mo1 N3 C7 44.7(4) . . . . ? C16 Mo1 N3 C7 60.1(3) . . . . ? N5 Mo1 N3 C7 146.4(3) . . . . ? N1 Mo1 N3 C7 -133.9(3) . . . . ? F2 Mo1 N3 N4 136.7(2) . . . . ? F1 Mo1 N3 N4 44.7(4) . . . . ? C17 Mo1 N3 N4 -130.4(2) . . . . ? C16 Mo1 N3 N4 -115.0(2) . . . . ? N5 Mo1 N3 N4 -28.8(2) . . . . ? N1 Mo1 N3 N4 50.9(2) . . . . ? C7 N3 N4 C9 0.5(4) . . . . ? Mo1 N3 N4 C9 176.8(2) . . . . ? C7 N3 N4 B1 173.9(3) . . . . ? Mo1 N3 N4 B1 -9.8(4) . . . . ? N4 N3 C7 C8 -1.0(4) . . . . ? Mo1 N3 C7 C8 -176.6(2) . . . . ? N4 N3 C7 C6 -179.8(3) . . . . ? Mo1 N3 C7 C6 4.6(5) . . . . ? N3 C7 C8 C9 1.0(5) . . . . ? C6 C7 C8 C9 179.7(4) . . . . ? C7 C8 C9 N4 -0.7(5) . . . . ? C7 C8 C9 C10 176.6(4) . . . . ? N3 N4 C9 C8 0.1(4) . . . . ? B1 N4 C9 C8 -172.2(4) . . . . ? N3 N4 C9 C10 -177.4(3) . . . . ? B1 N4 C9 C10 10.3(6) . . . . ? F2 Mo1 N5 C12 139.7(4) . . . . ? F1 Mo1 N5 C12 53.1(3) . . . . ? C17 Mo1 N5 C12 -29.1(4) . . . . ? C16 Mo1 N5 C12 -62.9(3) . . . . ? N3 Mo1 N5 C12 -146.0(3) . . . . ? N1 Mo1 N5 C12 134.9(3) . . . . ? F2 Mo1 N5 N6 -48.4(5) . . . . ? F1 Mo1 N5 N6 -134.9(2) . . . . ? C17 Mo1 N5 N6 142.9(3) . . . . ? C16 Mo1 N5 N6 109.1(3) . . . . ? N3 Mo1 N5 N6 26.0(2) . . . . ? N1 Mo1 N5 N6 -53.1(2) . . . . ? C12 N5 N6 C14 -0.3(4) . . . . ? Mo1 N5 N6 C14 -174.0(2) . . . . ? C12 N5 N6 B1 -171.0(3) . . . . ? Mo1 N5 N6 B1 15.2(4) . . . . ? N6 N5 C12 C13 0.3(4) . . . . ? Mo1 N5 C12 C13 173.1(2) . . . . ? N6 N5 C12 C11 -178.4(3) . . . . ? Mo1 N5 C12 C11 -5.6(6) . . . . ? N5 C12 C13 C14 -0.2(4) . . . . ? C11 C12 C13 C14 178.4(4) . . . . ? N5 N6 C14 C13 0.2(4) . . . . ? B1 N6 C14 C13 169.6(3) . . . . ? N5 N6 C14 C15 -179.8(3) . . . . ? B1 N6 C14 C15 -10.3(6) . . . . ? C12 C13 C14 N6 0.0(4) . . . . ? C12 C13 C14 C15 179.9(4) . . . . ? C9 N4 B1 N6 -124.9(4) . . . . ? N3 N4 B1 N6 63.5(4) . . . . ? C9 N4 B1 N2 117.3(4) . . . . ? N3 N4 B1 N2 -54.3(4) . . . . ? C14 N6 B1 N4 124.4(4) . . . . ? N5 N6 B1 N4 -66.9(4) . . . . ? C14 N6 B1 N2 -116.4(4) . . . . ? N5 N6 B1 N2 52.2(4) . . . . ? C4 N2 B1 N4 -126.3(4) . . . . ? N1 N2 B1 N4 54.6(4) . . . . ? C4 N2 B1 N6 114.4(4) . . . . ? N1 N2 B1 N6 -64.7(4) . . . . ? F2 Mo1 C16 C17 -71.7(2) . . . . ? F1 Mo1 C16 C17 30.9(2) . . . . ? N5 Mo1 C16 C17 114.3(2) . . . . ? N3 Mo1 C16 C17 -156.7(2) . . . . ? N1 Mo1 C16 C17 165.3(3) . . . . ? F2 Mo1 C16 C24 110.5(4) . . . . ? F1 Mo1 C16 C24 -147.0(4) . . . . ? C17 Mo1 C16 C24 -177.8(6) . . . . ? N5 Mo1 C16 C24 -63.5(4) . . . . ? N3 Mo1 C16 C24 25.5(4) . . . . ? N1 Mo1 C16 C24 -12.5(7) . . . . ? C24 C16 C17 C18 1.1(11) . . . . ? Mo1 C16 C17 C18 -176.7(7) . . . . ? C24 C16 C17 Mo1 177.8(6) . . . . ? F2 Mo1 C17 C16 115.1(2) . . . . ? F1 Mo1 C17 C16 -152.2(2) . . . . ? N5 Mo1 C17 C16 -67.8(2) . . . . ? N3 Mo1 C17 C16 26.1(3) . . . . ? N1 Mo1 C17 C16 -158.8(4) . . . . ? F2 Mo1 C17 C18 -67.6(4) . . . . ? F1 Mo1 C17 C18 25.1(4) . . . . ? C16 Mo1 C17 C18 177.3(5) . . . . ? N5 Mo1 C17 C18 109.5(4) . . . . ? N3 Mo1 C17 C18 -156.6(4) . . . . ? N1 Mo1 C17 C18 18.5(8) . . . . ? C16 C17 C18 C19 -155.9(6) . . . . ? Mo1 C17 C18 C19 28.9(6) . . . . ? C16 C17 C18 C23 25.7(8) . . . . ? Mo1 C17 C18 C23 -149.5(3) . . . . ? C23 C18 C19 C20 -0.7(5) . . . . ? C17 C18 C19 C20 -179.1(3) . . . . ? C18 C19 C20 C21 1.6(6) . . . . ? C19 C20 C21 C22 -0.7(6) . . . . ? C20 C21 C22 C23 -1.2(6) . . . . ? C21 C22 C23 C18 2.2(6) . . . . ? C19 C18 C23 C22 -1.2(6) . . . . ? C17 C18 C23 C22 177.2(3) . . . . ? C17 C16 C24 C25 30.5(8) . . . . ? Mo1 C16 C24 C25 -153.1(3) . . . . ? C17 C16 C24 C29 -149.4(5) . . . . ? Mo1 C16 C24 C29 27.0(6) . . . . ? C29 C24 C25 C26 -2.4(6) . . . . ? C16 C24 C25 C26 177.6(3) . . . . ? C24 C25 C26 C27 2.4(6) . . . . ? C25 C26 C27 C28 -1.0(6) . . . . ? C26 C27 C28 C29 -0.2(6) . . . . ? C25 C24 C29 C28 1.1(6) . . . . ? C16 C24 C29 C28 -179.0(3) . . . . ? C27 C28 C29 C24 0.2(6) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.618 _refine_diff_density_min -0.358 _refine_diff_density_rms 0.063 #===END data_8 _database_code_depnum_ccdc_archive 'CCDC 697676' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H32 B Cl2 Mo N6' _chemical_formula_sum 'C29 H32 B Cl2 Mo N6' _chemical_formula_weight 642.26 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' Cl Cl 0.1484 0.1585 '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 16.483(5) _cell_length_b 12.527(4) _cell_length_c 17.014(5) _cell_angle_alpha 90.00 _cell_angle_beta 113.115(7) _cell_angle_gamma 90.00 _cell_volume 3231.1(17) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 62 _cell_measurement_theta_min 2.4155 _cell_measurement_theta_max 20.71 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.320 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1316 _exptl_absorpt_coefficient_mu 0.598 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.847674 _exptl_absorpt_correction_T_max 0.976562 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 20476 _diffrn_reflns_av_R_equivalents 0.1393 _diffrn_reflns_av_sigmaI/netI 0.2659 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 27.54 _reflns_number_total 7417 _reflns_number_gt 2926 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'Bruker SMART (Bruker, 1998)' _computing_data_reduction 'Bruker SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1998)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1998)' _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^)+(0.0494P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7417 _refine_ls_number_parameters 359 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1666 _refine_ls_R_factor_gt 0.0639 _refine_ls_wR_factor_ref 0.1385 _refine_ls_wR_factor_gt 0.1194 _refine_ls_goodness_of_fit_ref 0.789 _refine_ls_restrained_S_all 0.789 _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 Mo1 Mo 0.70459(3) 0.95500(4) 0.81776(3) 0.02241(15) Uani 1 1 d . . . Cl1 Cl 0.57935(10) 1.06414(11) 0.73445(9) 0.0319(4) Uani 1 1 d . . . Cl2 Cl 0.77751(10) 0.98204(13) 0.72134(10) 0.0347(4) Uani 1 1 d . . . N1 N 0.7648(3) 1.1166(4) 0.8756(3) 0.0266(12) Uani 1 1 d . . . N2 N 0.7984(3) 1.1247(4) 0.9630(3) 0.0243(12) Uani 1 1 d . . . C1 C 0.7326(4) 1.2425(5) 0.7517(4) 0.046(2) Uani 1 1 d . . . H1A H 0.7543 1.1883 0.7231 0.069 Uiso 1 1 calc R . . H1B H 0.7557 1.3126 0.7453 0.069 Uiso 1 1 calc R . . H1C H 0.6680 1.2440 0.7258 0.069 Uiso 1 1 calc R . . C2 C 0.7631(4) 1.2158(5) 0.8448(4) 0.0303(16) Uani 1 1 d . . . C3 C 0.7973(4) 1.2865(5) 0.9128(4) 0.0403(19) Uani 1 1 d . . . H3A H 0.8058 1.3611 0.9091 0.048 Uiso 1 1 calc R . . C4 C 0.8165(4) 1.2285(5) 0.9859(4) 0.0295(16) Uani 1 1 d . . . C5 C 0.8522(4) 1.2650(5) 1.0777(4) 0.047(2) Uani 1 1 d . . . H5A H 0.9107 1.2337 1.1084 0.071 Uiso 1 1 calc R . . H5B H 0.8123 1.2420 1.1045 0.071 Uiso 1 1 calc R . . H5C H 0.8569 1.3430 1.0798 0.071 Uiso 1 1 calc R . . N3 N 0.6613(3) 0.9592(4) 0.9229(3) 0.0291(12) Uani 1 1 d . . . N4 N 0.7231(3) 0.9784(4) 1.0052(3) 0.0240(12) Uani 1 1 d . . . C6 C 0.5047(4) 0.8951(5) 0.8577(4) 0.0375(17) Uani 1 1 d . . . H6A H 0.4998 0.9387 0.8082 0.056 Uiso 1 1 calc R . . H6B H 0.4535 0.9080 0.8720 0.056 Uiso 1 1 calc R . . H6C H 0.5069 0.8194 0.8440 0.056 Uiso 1 1 calc R . . C7 C 0.5877(4) 0.9245(4) 0.9326(4) 0.0281(15) Uani 1 1 d . . . C8 C 0.6019(4) 0.9203(4) 1.0185(4) 0.0277(15) Uani 1 1 d . . . H8A H 0.5610 0.8988 1.0422 0.033 Uiso 1 1 calc R . . C9 C 0.6885(4) 0.9543(5) 1.0628(4) 0.0313(15) Uani 1 1 d . . . C10 C 0.7384(4) 0.9624(6) 1.1577(4) 0.0463(18) Uani 1 1 d . . . H10A H 0.7599 1.0356 1.1727 0.070 Uiso 1 1 calc R . . H10B H 0.7885 0.9131 1.1758 0.070 Uiso 1 1 calc R . . H10C H 0.6992 0.9438 1.1866 0.070 Uiso 1 1 calc R . . N5 N 0.8301(3) 0.8987(4) 0.9099(3) 0.0238(12) Uani 1 1 d . . . N6 N 0.8658(3) 0.9419(4) 0.9907(3) 0.0232(11) Uani 1 1 d . . . C11 C 0.8712(5) 0.7521(6) 0.8305(4) 0.056(2) Uani 1 1 d . . . H11A H 0.8171 0.7106 0.8173 0.085 Uiso 1 1 calc R . . H11B H 0.9213 0.7035 0.8429 0.085 Uiso 1 1 calc R . . H11C H 0.8654 0.7970 0.7813 0.085 Uiso 1 1 calc R . . C12 C 0.8866(4) 0.8223(5) 0.9077(4) 0.0311(16) Uani 1 1 d . . . C13 C 0.9597(4) 0.8210(5) 0.9846(4) 0.0403(18) Uani 1 1 d . . . H13A H 1.0104 0.7769 0.9987 0.048 Uiso 1 1 calc R . . C14 C 0.9446(4) 0.8958(5) 1.0366(4) 0.0308(16) Uani 1 1 d . . . C15 C 1.0023(4) 0.9287(5) 1.1247(4) 0.0438(19) Uani 1 1 d . . . H15A H 1.0092 1.0065 1.1268 0.066 Uiso 1 1 calc R . . H15B H 1.0602 0.8948 1.1410 0.066 Uiso 1 1 calc R . . H15C H 0.9755 0.9066 1.1643 0.066 Uiso 1 1 calc R . . B1 B 0.8138(5) 1.0256(5) 1.0194(5) 0.0315(19) Uani 1 1 d . . . H1 H 0.8466 1.0447 1.0809 0.038 Uiso 1 1 calc R . . C16 C 0.6695(4) 0.8001(5) 0.8155(4) 0.0256(15) Uani 1 1 d . . . C17 C 0.6285(4) 0.8382(4) 0.7391(4) 0.0236(14) Uani 1 1 d . . . C18 C 0.5603(4) 0.8188(4) 0.6540(4) 0.0251(15) Uani 1 1 d . . . C19 C 0.4915(4) 0.7479(4) 0.6442(4) 0.0269(15) Uani 1 1 d . . . H19A H 0.4903 0.7106 0.6923 0.032 Uiso 1 1 calc R . . C20 C 0.4254(4) 0.7323(5) 0.5648(4) 0.0315(16) Uani 1 1 d . . . H20A H 0.3778 0.6857 0.5586 0.038 Uiso 1 1 calc R . . C21 C 0.4279(4) 0.7846(5) 0.4934(4) 0.0367(18) Uani 1 1 d . . . H21A H 0.3829 0.7721 0.4386 0.044 Uiso 1 1 calc R . . C22 C 0.4964(4) 0.8553(5) 0.5025(4) 0.0385(18) Uani 1 1 d . . . H22A H 0.4986 0.8904 0.4539 0.046 Uiso 1 1 calc R . . C23 C 0.5610(4) 0.8738(4) 0.5828(4) 0.0254(15) Uani 1 1 d . . . H23A H 0.6062 0.9243 0.5896 0.030 Uiso 1 1 calc R . . C24 C 0.6811(4) 0.7048(4) 0.8695(4) 0.0240(14) Uani 1 1 d . . . C25 C 0.7256(4) 0.7107(5) 0.9587(4) 0.0347(17) Uani 1 1 d . . . H25A H 0.7507 0.7763 0.9851 0.042 Uiso 1 1 calc R . . C26 C 0.7327(4) 0.6195(5) 1.0083(4) 0.0420(18) Uani 1 1 d . . . H26A H 0.7624 0.6237 1.0687 0.050 Uiso 1 1 calc R . . C27 C 0.6972(4) 0.5238(5) 0.9710(4) 0.0378(17) Uani 1 1 d . . . H27A H 0.7031 0.4621 1.0053 0.045 Uiso 1 1 calc R . . C28 C 0.6529(4) 0.5178(5) 0.8831(5) 0.0416(19) Uani 1 1 d . . . H28A H 0.6288 0.4518 0.8569 0.050 Uiso 1 1 calc R . . C29 C 0.6437(4) 0.6074(4) 0.8337(4) 0.0290(16) Uani 1 1 d . . . H29A H 0.6111 0.6029 0.7738 0.035 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 Mo1 0.0189(3) 0.0224(3) 0.0234(3) -0.0004(3) 0.0056(2) 0.0000(3) Cl1 0.0292(8) 0.0296(9) 0.0312(9) 0.0019(7) 0.0059(7) 0.0061(7) Cl2 0.0282(9) 0.0470(11) 0.0295(9) -0.0047(7) 0.0122(7) -0.0095(7) N1 0.028(3) 0.024(3) 0.023(3) 0.007(2) 0.005(2) 0.002(2) N2 0.019(3) 0.021(3) 0.026(3) 0.000(2) 0.002(2) -0.003(2) C1 0.050(5) 0.042(4) 0.039(5) 0.008(3) 0.010(4) -0.010(4) C2 0.030(4) 0.018(3) 0.041(4) -0.003(3) 0.010(3) 0.002(3) C3 0.029(4) 0.025(4) 0.057(5) 0.002(4) 0.006(4) 0.000(3) C4 0.024(4) 0.027(4) 0.036(4) 0.000(3) 0.010(3) 0.007(3) C5 0.055(5) 0.028(4) 0.054(5) -0.014(4) 0.017(4) 0.001(3) N3 0.029(3) 0.021(3) 0.031(3) 0.002(3) 0.005(2) 0.003(2) N4 0.022(3) 0.030(3) 0.015(3) -0.001(2) 0.002(2) -0.001(2) C6 0.019(4) 0.045(4) 0.041(4) -0.003(3) 0.003(3) 0.002(3) C7 0.016(3) 0.022(3) 0.045(4) 0.002(3) 0.011(3) -0.004(3) C8 0.029(4) 0.030(4) 0.030(4) -0.003(3) 0.018(3) -0.006(3) C9 0.039(4) 0.029(3) 0.027(4) -0.003(3) 0.014(3) 0.007(3) C10 0.051(4) 0.056(5) 0.033(4) -0.003(4) 0.018(4) -0.008(4) N5 0.018(3) 0.028(3) 0.023(3) 0.000(2) 0.005(2) 0.000(2) N6 0.020(3) 0.026(3) 0.021(3) -0.006(2) 0.005(2) 0.001(2) C11 0.044(5) 0.066(5) 0.053(5) -0.023(4) 0.012(4) 0.015(4) C12 0.023(4) 0.034(4) 0.038(4) -0.001(3) 0.014(3) 0.005(3) C13 0.020(4) 0.042(4) 0.051(5) 0.001(4) 0.005(3) 0.013(3) C14 0.016(3) 0.041(4) 0.028(4) 0.003(3) 0.000(3) 0.008(3) C15 0.026(4) 0.049(5) 0.043(4) 0.003(4) -0.001(3) 0.001(3) B1 0.031(4) 0.031(5) 0.028(4) -0.009(3) 0.006(3) -0.012(4) C16 0.025(3) 0.035(4) 0.019(4) -0.006(3) 0.011(3) -0.003(3) C17 0.018(3) 0.021(3) 0.032(4) 0.003(3) 0.010(3) 0.000(3) C18 0.023(3) 0.024(3) 0.024(4) 0.000(3) 0.005(3) -0.006(3) C19 0.032(4) 0.021(3) 0.023(4) 0.001(3) 0.006(3) 0.006(3) C20 0.027(4) 0.023(3) 0.035(4) -0.004(3) 0.002(3) 0.001(3) C21 0.036(4) 0.028(4) 0.030(4) -0.011(3) -0.005(3) 0.001(3) C22 0.056(5) 0.028(3) 0.025(4) 0.007(3) 0.009(4) 0.007(3) C23 0.028(4) 0.024(3) 0.024(4) 0.000(3) 0.010(3) -0.003(3) C24 0.015(3) 0.027(3) 0.030(4) 0.002(3) 0.008(3) 0.002(3) C25 0.053(5) 0.019(3) 0.024(4) -0.001(3) 0.008(3) 0.007(3) C26 0.051(5) 0.038(4) 0.037(4) 0.011(3) 0.016(4) 0.010(4) C27 0.041(4) 0.025(4) 0.053(5) 0.010(3) 0.025(4) 0.011(3) C28 0.033(4) 0.025(4) 0.057(5) 0.007(3) 0.007(4) 0.002(3) C29 0.033(4) 0.022(3) 0.035(4) 0.001(3) 0.016(3) -0.005(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 Mo1 C16 2.021(6) . ? Mo1 C17 2.047(6) . ? Mo1 N5 2.165(4) . ? Mo1 N3 2.171(5) . ? Mo1 N1 2.299(5) . ? Mo1 Cl2 2.4082(18) . ? Mo1 Cl1 2.4171(16) . ? N1 C2 1.345(7) . ? N1 N2 1.371(6) . ? N2 C4 1.357(7) . ? N2 B1 1.528(8) . ? C1 C2 1.500(8) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.389(8) . ? C3 C4 1.366(8) . ? C3 H3A 0.9500 . ? C4 C5 1.508(8) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? N3 C7 1.360(7) . ? N3 N4 1.391(6) . ? N4 C9 1.348(7) . ? N4 B1 1.535(8) . ? C6 C7 1.504(7) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.387(8) . ? C8 C9 1.395(8) . ? C8 H8A 0.9500 . ? C9 C10 1.499(8) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? N5 C12 1.346(7) . ? N5 N6 1.377(6) . ? N6 C14 1.355(7) . ? N6 B1 1.550(8) . ? C11 C12 1.517(8) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.388(8) . ? C13 C14 1.377(8) . ? C13 H13A 0.9500 . ? C14 C15 1.483(8) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? B1 H1 1.0000 . ? C16 C17 1.297(7) . ? C16 C24 1.473(8) . ? C17 C18 1.463(7) . ? C18 C19 1.398(8) . ? C18 C23 1.399(8) . ? C19 C20 1.376(7) . ? C19 H19A 0.9500 . ? C20 C21 1.395(8) . ? C20 H20A 0.9500 . ? C21 C22 1.395(8) . ? C21 H21A 0.9500 . ? C22 C23 1.383(7) . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? C24 C29 1.394(7) . ? C24 C25 1.404(7) . ? C25 C26 1.398(8) . ? C25 H25A 0.9500 . ? C26 C27 1.376(8) . ? C26 H26A 0.9500 . ? C27 C28 1.385(8) . ? C27 H27A 0.9500 . ? C28 C29 1.374(8) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? 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 C16 Mo1 C17 37.2(2) . . ? C16 Mo1 N5 83.5(2) . . ? C17 Mo1 N5 114.0(2) . . ? C16 Mo1 N3 81.7(2) . . ? C17 Mo1 N3 103.9(2) . . ? N5 Mo1 N3 86.64(18) . . ? C16 Mo1 N1 157.8(2) . . ? C17 Mo1 N1 163.85(19) . . ? N5 Mo1 N1 81.23(16) . . ? N3 Mo1 N1 81.48(18) . . ? C16 Mo1 Cl2 109.73(17) . . ? C17 Mo1 Cl2 89.82(17) . . ? N5 Mo1 Cl2 87.03(14) . . ? N3 Mo1 Cl2 166.22(13) . . ? N1 Mo1 Cl2 85.47(13) . . ? C16 Mo1 Cl1 111.07(17) . . ? C17 Mo1 Cl1 81.84(16) . . ? N5 Mo1 Cl1 164.17(13) . . ? N3 Mo1 Cl1 89.32(13) . . ? N1 Mo1 Cl1 83.04(12) . . ? Cl2 Mo1 Cl1 93.48(6) . . ? C2 N1 N2 107.1(5) . . ? C2 N1 Mo1 135.0(4) . . ? N2 N1 Mo1 116.9(3) . . ? C4 N2 N1 109.3(5) . . ? C4 N2 B1 129.4(5) . . ? N1 N2 B1 121.2(5) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 108.9(6) . . ? N1 C2 C1 124.5(6) . . ? C3 C2 C1 126.6(6) . . ? C4 C3 C2 107.0(6) . . ? C4 C3 H3A 126.5 . . ? C2 C3 H3A 126.5 . . ? N2 C4 C3 107.6(6) . . ? N2 C4 C5 122.7(6) . . ? C3 C4 C5 129.7(6) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 N3 N4 105.6(5) . . ? C7 N3 Mo1 133.7(4) . . ? N4 N3 Mo1 119.1(4) . . ? C9 N4 N3 110.0(5) . . ? C9 N4 B1 129.4(5) . . ? N3 N4 B1 120.5(5) . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N3 C7 C8 110.6(5) . . ? N3 C7 C6 122.2(6) . . ? C8 C7 C6 127.3(6) . . ? C7 C8 C9 105.7(5) . . ? C7 C8 H8A 127.1 . . ? C9 C8 H8A 127.1 . . ? N4 C9 C8 108.1(5) . . ? N4 C9 C10 124.0(6) . . ? C8 C9 C10 127.9(6) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 N5 N6 106.2(5) . . ? C12 N5 Mo1 133.3(4) . . ? N6 N5 Mo1 120.5(3) . . ? C14 N6 N5 110.2(5) . . ? C14 N6 B1 129.1(5) . . ? N5 N6 B1 120.6(4) . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N5 C12 C13 109.7(6) . . ? N5 C12 C11 123.6(5) . . ? C13 C12 C11 126.7(6) . . ? C14 C13 C12 106.8(5) . . ? C14 C13 H13A 126.6 . . ? C12 C13 H13A 126.6 . . ? N6 C14 C13 107.1(5) . . ? N6 C14 C15 123.6(6) . . ? C13 C14 C15 129.2(5) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N2 B1 N4 107.6(5) . . ? N2 B1 N6 109.1(5) . . ? N4 B1 N6 108.3(5) . . ? N2 B1 H1 110.6 . . ? N4 B1 H1 110.6 . . ? N6 B1 H1 110.6 . . ? C17 C16 C24 144.4(5) . . ? C17 C16 Mo1 72.5(4) . . ? C24 C16 Mo1 143.1(4) . . ? C16 C17 C18 145.6(6) . . ? C16 C17 Mo1 70.4(4) . . ? C18 C17 Mo1 143.2(4) . . ? C19 C18 C23 119.4(5) . . ? C19 C18 C17 119.7(5) . . ? C23 C18 C17 120.8(5) . . ? C20 C19 C18 120.0(6) . . ? C20 C19 H19A 120.0 . . ? C18 C19 H19A 120.0 . . ? C19 C20 C21 120.3(6) . . ? C19 C20 H20A 119.8 . . ? C21 C20 H20A 119.8 . . ? C22 C21 C20 120.1(6) . . ? C22 C21 H21A 120.0 . . ? C20 C21 H21A 120.0 . . ? C23 C22 C21 119.4(6) . . ? C23 C22 H22A 120.3 . . ? C21 C22 H22A 120.3 . . ? C22 C23 C18 120.6(6) . . ? C22 C23 H23A 119.7 . . ? C18 C23 H23A 119.7 . . ? C29 C24 C25 118.2(5) . . ? C29 C24 C16 120.6(5) . . ? C25 C24 C16 121.1(5) . . ? C26 C25 C24 119.6(6) . . ? C26 C25 H25A 120.2 . . ? C24 C25 H25A 120.2 . . ? C27 C26 C25 120.9(6) . . ? C27 C26 H26A 119.5 . . ? C25 C26 H26A 119.5 . . ? C26 C27 C28 119.6(6) . . ? C26 C27 H27A 120.2 . . ? C28 C27 H27A 120.2 . . ? C29 C28 C27 120.1(6) . . ? C29 C28 H28A 120.0 . . ? C27 C28 H28A 120.0 . . ? C28 C29 C24 121.6(6) . . ? C28 C29 H29A 119.2 . . ? C24 C29 H29A 119.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C16 Mo1 N1 C2 -170.0(6) . . . . ? C17 Mo1 N1 C2 -18.1(11) . . . . ? N5 Mo1 N1 C2 143.0(6) . . . . ? N3 Mo1 N1 C2 -129.1(6) . . . . ? Cl2 Mo1 N1 C2 55.4(6) . . . . ? Cl1 Mo1 N1 C2 -38.7(6) . . . . ? C16 Mo1 N1 N2 -3.9(7) . . . . ? C17 Mo1 N1 N2 148.0(7) . . . . ? N5 Mo1 N1 N2 -50.8(4) . . . . ? N3 Mo1 N1 N2 37.0(4) . . . . ? Cl2 Mo1 N1 N2 -138.5(4) . . . . ? Cl1 Mo1 N1 N2 127.4(4) . . . . ? C2 N1 N2 C4 0.6(6) . . . . ? Mo1 N1 N2 C4 -169.1(4) . . . . ? C2 N1 N2 B1 -177.1(5) . . . . ? Mo1 N1 N2 B1 13.1(6) . . . . ? N2 N1 C2 C3 1.1(7) . . . . ? Mo1 N1 C2 C3 168.2(4) . . . . ? N2 N1 C2 C1 178.6(6) . . . . ? Mo1 N1 C2 C1 -14.4(10) . . . . ? N1 C2 C3 C4 -2.5(7) . . . . ? C1 C2 C3 C4 -179.8(6) . . . . ? N1 N2 C4 C3 -2.2(7) . . . . ? B1 N2 C4 C3 175.3(6) . . . . ? N1 N2 C4 C5 178.4(5) . . . . ? B1 N2 C4 C5 -4.1(10) . . . . ? C2 C3 C4 N2 2.8(7) . . . . ? C2 C3 C4 C5 -177.8(6) . . . . ? C16 Mo1 N3 C7 -49.3(5) . . . . ? C17 Mo1 N3 C7 -19.2(5) . . . . ? N5 Mo1 N3 C7 -133.1(5) . . . . ? N1 Mo1 N3 C7 145.2(5) . . . . ? Cl2 Mo1 N3 C7 164.1(4) . . . . ? Cl1 Mo1 N3 C7 62.2(5) . . . . ? C16 Mo1 N3 N4 113.6(4) . . . . ? C17 Mo1 N3 N4 143.6(4) . . . . ? N5 Mo1 N3 N4 29.7(4) . . . . ? N1 Mo1 N3 N4 -51.9(4) . . . . ? Cl2 Mo1 N3 N4 -33.0(8) . . . . ? Cl1 Mo1 N3 N4 -135.0(4) . . . . ? C7 N3 N4 C9 1.1(6) . . . . ? Mo1 N3 N4 C9 -166.2(4) . . . . ? C7 N3 N4 B1 -176.2(5) . . . . ? Mo1 N3 N4 B1 16.6(6) . . . . ? N4 N3 C7 C8 -0.7(6) . . . . ? Mo1 N3 C7 C8 163.9(4) . . . . ? N4 N3 C7 C6 179.9(5) . . . . ? Mo1 N3 C7 C6 -15.6(8) . . . . ? N3 C7 C8 C9 0.0(7) . . . . ? C6 C7 C8 C9 179.4(5) . . . . ? N3 N4 C9 C8 -1.1(7) . . . . ? B1 N4 C9 C8 175.9(5) . . . . ? N3 N4 C9 C10 178.0(5) . . . . ? B1 N4 C9 C10 -5.1(10) . . . . ? C7 C8 C9 N4 0.6(7) . . . . ? C7 C8 C9 C10 -178.4(6) . . . . ? C16 Mo1 N5 C12 55.5(6) . . . . ? C17 Mo1 N5 C12 33.7(6) . . . . ? N3 Mo1 N5 C12 137.5(6) . . . . ? N1 Mo1 N5 C12 -140.6(6) . . . . ? Cl2 Mo1 N5 C12 -54.8(5) . . . . ? Cl1 Mo1 N5 C12 -147.0(5) . . . . ? C16 Mo1 N5 N6 -122.6(4) . . . . ? C17 Mo1 N5 N6 -144.4(4) . . . . ? N3 Mo1 N5 N6 -40.6(4) . . . . ? N1 Mo1 N5 N6 41.3(4) . . . . ? Cl2 Mo1 N5 N6 127.2(4) . . . . ? Cl1 Mo1 N5 N6 34.9(8) . . . . ? C12 N5 N6 C14 2.3(6) . . . . ? Mo1 N5 N6 C14 -179.2(4) . . . . ? C12 N5 N6 B1 -174.1(5) . . . . ? Mo1 N5 N6 B1 4.5(6) . . . . ? N6 N5 C12 C13 -3.2(7) . . . . ? Mo1 N5 C12 C13 178.5(4) . . . . ? N6 N5 C12 C11 178.3(6) . . . . ? Mo1 N5 C12 C11 0.0(9) . . . . ? N5 C12 C13 C14 3.0(8) . . . . ? C11 C12 C13 C14 -178.6(6) . . . . ? N5 N6 C14 C13 -0.4(7) . . . . ? B1 N6 C14 C13 175.5(6) . . . . ? N5 N6 C14 C15 176.5(6) . . . . ? B1 N6 C14 C15 -7.5(10) . . . . ? C12 C13 C14 N6 -1.6(7) . . . . ? C12 C13 C14 C15 -178.3(6) . . . . ? C4 N2 B1 N4 115.2(6) . . . . ? N1 N2 B1 N4 -67.6(7) . . . . ? C4 N2 B1 N6 -127.5(6) . . . . ? N1 N2 B1 N6 49.7(7) . . . . ? C9 N4 B1 N2 -126.1(6) . . . . ? N3 N4 B1 N2 50.5(7) . . . . ? C9 N4 B1 N6 116.1(6) . . . . ? N3 N4 B1 N6 -67.2(6) . . . . ? C14 N6 B1 N2 121.9(6) . . . . ? N5 N6 B1 N2 -62.5(6) . . . . ? C14 N6 B1 N4 -121.2(6) . . . . ? N5 N6 B1 N4 54.3(7) . . . . ? N5 Mo1 C16 C17 -145.9(4) . . . . ? N3 Mo1 C16 C17 126.6(4) . . . . ? N1 Mo1 C16 C17 167.5(5) . . . . ? Cl2 Mo1 C16 C17 -61.4(4) . . . . ? Cl1 Mo1 C16 C17 40.5(4) . . . . ? C17 Mo1 C16 C24 -177.5(9) . . . . ? N5 Mo1 C16 C24 36.6(7) . . . . ? N3 Mo1 C16 C24 -50.9(7) . . . . ? N1 Mo1 C16 C24 -10.0(11) . . . . ? Cl2 Mo1 C16 C24 121.1(7) . . . . ? Cl1 Mo1 C16 C24 -137.0(7) . . . . ? C24 C16 C17 C18 7.2(17) . . . . ? Mo1 C16 C17 C18 -170.2(10) . . . . ? C24 C16 C17 Mo1 177.4(10) . . . . ? N5 Mo1 C17 C16 37.6(4) . . . . ? N3 Mo1 C17 C16 -55.0(4) . . . . ? N1 Mo1 C17 C16 -162.9(6) . . . . ? Cl2 Mo1 C17 C16 124.3(3) . . . . ? Cl1 Mo1 C17 C16 -142.2(4) . . . . ? C16 Mo1 C17 C18 170.8(9) . . . . ? N5 Mo1 C17 C18 -151.6(7) . . . . ? N3 Mo1 C17 C18 115.8(7) . . . . ? N1 Mo1 C17 C18 7.9(13) . . . . ? Cl2 Mo1 C17 C18 -65.0(7) . . . . ? Cl1 Mo1 C17 C18 28.6(7) . . . . ? C16 C17 C18 C19 25.0(13) . . . . ? Mo1 C17 C18 C19 -139.5(6) . . . . ? C16 C17 C18 C23 -157.8(9) . . . . ? Mo1 C17 C18 C23 37.7(10) . . . . ? C23 C18 C19 C20 0.4(9) . . . . ? C17 C18 C19 C20 177.6(5) . . . . ? C18 C19 C20 C21 1.8(9) . . . . ? C19 C20 C21 C22 -1.6(9) . . . . ? C20 C21 C22 C23 -0.7(9) . . . . ? C21 C22 C23 C18 2.9(9) . . . . ? C19 C18 C23 C22 -2.8(9) . . . . ? C17 C18 C23 C22 -180.0(5) . . . . ? C17 C16 C24 C29 8.0(13) . . . . ? Mo1 C16 C24 C29 -176.1(5) . . . . ? C17 C16 C24 C25 -168.2(8) . . . . ? Mo1 C16 C24 C25 7.7(10) . . . . ? C29 C24 C25 C26 1.3(9) . . . . ? C16 C24 C25 C26 177.7(6) . . . . ? C24 C25 C26 C27 0.5(10) . . . . ? C25 C26 C27 C28 -0.8(10) . . . . ? C26 C27 C28 C29 -0.7(10) . . . . ? C27 C28 C29 C24 2.6(10) . . . . ? C25 C24 C29 C28 -2.9(9) . . . . ? C16 C24 C29 C28 -179.2(6) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.891 _refine_diff_density_min -1.119 _refine_diff_density_rms 0.126 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.500 248.6 50.6 2 0.000 0.500 1.000 248.6 50.6 _platon_squeeze_details ; ; #===END data_9.CH2Cl2 _database_code_depnum_ccdc_archive 'CCDC 697677' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H34 B1 Cl7 Mo1 N6 Sb' _chemical_formula_weight 955.29 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' Cl Cl 0.1484 0.1585 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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 9.9217(9) _cell_length_b 10.4480(10) _cell_length_c 18.8067(14) _cell_angle_alpha 75.940(6) _cell_angle_beta 83.241(9) _cell_angle_gamma 79.431(7) _cell_volume 1853.6(3) _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 Red _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.712 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 946 _exptl_absorpt_coefficient_mu 1.603 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.538 _exptl_absorpt_correction_T_max 0.923 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'omega scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 19763 _diffrn_reflns_av_R_equivalents 0.0262 _diffrn_reflns_av_sigmaI/netI 0.0355 _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 -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8425 _reflns_number_gt 7054 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0301P)^2^+1.2731P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8425 _refine_ls_number_parameters 448 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0380 _refine_ls_R_factor_gt 0.0281 _refine_ls_wR_factor_ref 0.0709 _refine_ls_wR_factor_gt 0.0671 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.003 _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 0.798809(19) 0.797431(19) 0.330282(10) 0.01703(5) Uani 1 1 d . . . Cl1 Cl 0.90008(6) 1.00246(6) 0.28866(4) 0.02811(13) Uani 1 1 d . . . Cl2 Cl 0.69964(6) 0.83795(6) 0.44655(3) 0.02669(13) Uani 1 1 d . . . N1 N 0.6082(2) 0.93673(19) 0.28660(11) 0.0211(4) Uani 1 1 d . . . N2 N 0.5412(2) 0.9026(2) 0.23536(11) 0.0216(4) Uani 1 1 d . . . N3 N 0.8387(2) 0.77607(19) 0.21679(11) 0.0211(4) Uani 1 1 d . . . N4 N 0.7329(2) 0.7629(2) 0.17855(11) 0.0229(4) Uani 1 1 d . . . N5 N 0.66609(19) 0.65014(19) 0.34319(11) 0.0194(4) Uani 1 1 d . . . N6 N 0.5878(2) 0.65358(19) 0.28630(11) 0.0201(4) Uani 1 1 d . . . C1 C 0.5852(3) 1.1366(3) 0.34279(16) 0.0356(6) Uani 1 1 d . . . H1A H 0.6748 1.0943 0.3612 0.053 Uiso 1 1 calc R . . H1B H 0.5150 1.1347 0.3841 0.053 Uiso 1 1 calc R . . H1C H 0.5894 1.2295 0.3170 0.053 Uiso 1 1 calc R . . C2 C 0.5492(3) 1.0626(2) 0.29107(14) 0.0259(5) Uani 1 1 d . . . C3 C 0.4491(3) 1.1084(3) 0.24141(16) 0.0320(6) Uani 1 1 d . . . H3A H 0.3934 1.1941 0.2326 0.038 Uiso 1 1 calc R . . C4 C 0.4451(3) 1.0070(3) 0.20702(15) 0.0311(6) Uani 1 1 d . . . C5 C 0.3576(4) 1.0051(3) 0.1481(2) 0.0504(9) Uani 1 1 d . . . H5A H 0.2887 1.0864 0.1400 0.076 Uiso 1 1 calc R . . H5B H 0.3112 0.9265 0.1630 0.076 Uiso 1 1 calc R . . H5C H 0.4154 1.0011 0.1024 0.076 Uiso 1 1 calc R . . C6 C 1.0924(3) 0.7750(3) 0.19137(15) 0.0345(6) Uani 1 1 d . . . H6A H 1.0868 0.8445 0.2189 0.052 Uiso 1 1 calc R . . H6B H 1.1546 0.7941 0.1470 0.052 Uiso 1 1 calc R . . H6C H 1.1273 0.6879 0.2222 0.052 Uiso 1 1 calc R . . C7 C 0.9528(3) 0.7729(3) 0.17007(14) 0.0269(5) Uani 1 1 d . . . C8 C 0.9195(3) 0.7623(3) 0.10232(15) 0.0374(7) Uani 1 1 d . . . H8A H 0.9802 0.7601 0.0595 0.045 Uiso 1 1 calc R . . C9 C 0.7806(3) 0.7555(3) 0.10959(14) 0.0331(6) Uani 1 1 d . . . C10 C 0.6906(4) 0.7427(4) 0.05369(17) 0.0492(8) Uani 1 1 d . . . H10A H 0.6609 0.6549 0.0681 0.074 Uiso 1 1 calc R . . H10B H 0.7424 0.7518 0.0055 0.074 Uiso 1 1 calc R . . H10C H 0.6098 0.8130 0.0509 0.074 Uiso 1 1 calc R . . C11 C 0.7139(3) 0.5011(3) 0.46631(14) 0.0306(6) Uani 1 1 d . . . H11A H 0.7504 0.5773 0.4740 0.046 Uiso 1 1 calc R . . H11B H 0.7894 0.4269 0.4639 0.046 Uiso 1 1 calc R . . H11C H 0.6470 0.4730 0.5072 0.046 Uiso 1 1 calc R . . C12 C 0.6453(2) 0.5409(2) 0.39615(13) 0.0229(5) Uani 1 1 d . . . C13 C 0.5549(3) 0.4747(2) 0.37320(15) 0.0270(5) Uani 1 1 d . . . H13A H 0.5228 0.3951 0.4000 0.032 Uiso 1 1 calc R . . C14 C 0.5209(2) 0.5465(2) 0.30434(14) 0.0246(5) Uani 1 1 d . . . C15 C 0.4308(3) 0.5182(3) 0.25319(16) 0.0326(6) Uani 1 1 d . . . H15A H 0.3664 0.5994 0.2345 0.049 Uiso 1 1 calc R . . H15B H 0.3791 0.4472 0.2797 0.049 Uiso 1 1 calc R . . H15C H 0.4879 0.4894 0.2119 0.049 Uiso 1 1 calc R . . C16 C 0.9523(2) 0.6371(2) 0.34901(12) 0.0204(5) Uani 1 1 d . . . C17 C 0.9844(2) 0.7323(2) 0.37412(12) 0.0199(5) Uani 1 1 d . . . C18 C 1.0893(2) 0.7779(2) 0.40559(13) 0.0217(5) Uani 1 1 d . . . C19 C 1.0576(3) 0.8346(3) 0.46614(15) 0.0308(6) Uani 1 1 d . . . H19A H 0.9659 0.8445 0.4877 0.037 Uiso 1 1 calc R . . C20 C 1.1596(3) 0.8770(3) 0.49548(17) 0.0365(7) Uani 1 1 d . . . H20A H 1.1383 0.9116 0.5385 0.044 Uiso 1 1 calc R . . C21 C 1.2921(3) 0.8689(3) 0.46215(16) 0.0317(6) Uani 1 1 d . . . H21A H 1.3605 0.9013 0.4811 0.038 Uiso 1 1 calc R . . C22 C 1.3247(3) 0.8137(3) 0.40119(15) 0.0294(6) Uani 1 1 d . . . H22A H 1.4156 0.8079 0.3784 0.035 Uiso 1 1 calc R . . C23 C 1.2244(2) 0.7668(3) 0.37352(14) 0.0252(5) Uani 1 1 d . . . H23A H 1.2475 0.7269 0.3325 0.030 Uiso 1 1 calc R . . C24 C 1.0003(2) 0.5013(2) 0.33961(13) 0.0219(5) Uani 1 1 d . . . C25 C 1.1149(3) 0.4264(3) 0.37567(14) 0.0272(5) Uani 1 1 d . . . H25A H 1.1616 0.4657 0.4040 0.033 Uiso 1 1 calc R . . C26 C 1.1605(3) 0.2951(3) 0.37017(15) 0.0315(6) Uani 1 1 d . . . H26A H 1.2378 0.2444 0.3951 0.038 Uiso 1 1 calc R . . C27 C 1.0933(3) 0.2384(3) 0.32842(16) 0.0348(6) Uani 1 1 d . . . H27A H 1.1243 0.1485 0.3247 0.042 Uiso 1 1 calc R . . C28 C 0.9812(3) 0.3120(3) 0.29199(16) 0.0336(6) Uani 1 1 d . . . H28A H 0.9360 0.2724 0.2631 0.040 Uiso 1 1 calc R . . C29 C 0.9340(3) 0.4426(3) 0.29701(14) 0.0270(5) Uani 1 1 d . . . H29A H 0.8569 0.4925 0.2717 0.032 Uiso 1 1 calc R . . B1 B 0.5866(3) 0.7658(3) 0.21609(15) 0.0230(6) Uani 1 1 d . . . H1 H 0.5228 0.7529 0.1819 0.028 Uiso 1 1 calc R . . Sb1 Sb 0.776489(19) 1.100867(19) 0.136334(10) 0.03410(6) Uani 1 1 d . . . Cl3 Cl 0.72987(9) 1.32272(8) 0.15130(5) 0.0523(2) Uani 1 1 d . . . Cl4 Cl 1.00599(8) 1.11403(9) 0.09177(5) 0.0559(2) Uani 1 1 d . . . Cl5 Cl 0.69399(11) 1.15283(11) 0.01641(5) 0.0676(3) Uani 1 1 d . . . C99 C 0.0783(9) 1.4367(8) 0.1029(4) 0.061(2) Uani 0.50 1 d P A 1 H99A H 0.0562 1.3448 0.1180 0.073 Uiso 0.50 1 calc PR A 1 H99B H 0.0177 1.4914 0.1338 0.073 Uiso 0.50 1 calc PR A 1 Cl6 Cl 0.0464(2) 1.5002(2) 0.01446(11) 0.0659(5) Uani 0.50 1 d P . 1 Cl7 Cl 0.2524(5) 1.4324(5) 0.1185(3) 0.1130(16) Uani 0.50 1 d P A 1 C99A C 0.2682(9) 1.5220(8) 0.0625(5) 0.068(2) Uani 0.50 1 d P B 2 H99C H 0.2628 1.6132 0.0704 0.082 Uiso 0.50 1 calc PR B 2 H99D H 0.2215 1.5297 0.0176 0.082 Uiso 0.50 1 calc PR B 2 Cl7A Cl 0.1841(4) 1.4275(4) 0.1366(2) 0.0781(10) Uani 0.50 1 d P B 2 Cl6A Cl 0.4422(2) 1.4516(3) 0.04929(15) 0.0816(7) Uani 0.50 1 d P . 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 Mo1 0.01785(10) 0.01587(10) 0.01774(10) -0.00296(7) -0.00420(7) -0.00298(7) Cl1 0.0285(3) 0.0205(3) 0.0362(3) -0.0016(2) -0.0082(3) -0.0089(2) Cl2 0.0269(3) 0.0321(3) 0.0223(3) -0.0099(2) -0.0026(2) -0.0025(2) N1 0.0229(10) 0.0196(10) 0.0216(10) -0.0048(8) -0.0051(8) -0.0028(8) N2 0.0202(10) 0.0213(10) 0.0236(10) -0.0027(8) -0.0081(8) -0.0033(8) N3 0.0213(10) 0.0226(10) 0.0196(10) -0.0039(8) -0.0053(8) -0.0026(8) N4 0.0267(11) 0.0240(10) 0.0187(10) -0.0037(8) -0.0073(8) -0.0039(8) N5 0.0194(9) 0.0197(9) 0.0198(10) -0.0036(8) -0.0049(8) -0.0036(8) N6 0.0205(10) 0.0190(9) 0.0231(10) -0.0061(8) -0.0061(8) -0.0043(8) C1 0.0421(16) 0.0262(13) 0.0397(16) -0.0143(12) -0.0098(13) 0.0045(12) C2 0.0253(12) 0.0193(12) 0.0311(14) -0.0040(10) -0.0031(10) -0.0001(10) C3 0.0278(13) 0.0219(13) 0.0425(16) -0.0036(11) -0.0093(12) 0.0049(11) C4 0.0267(13) 0.0268(13) 0.0370(15) -0.0008(11) -0.0118(11) 0.0002(11) C5 0.0504(19) 0.0395(17) 0.062(2) -0.0035(15) -0.0392(17) 0.0014(15) C6 0.0239(13) 0.0460(17) 0.0296(14) -0.0045(12) 0.0024(11) -0.0033(12) C7 0.0264(13) 0.0290(13) 0.0221(12) -0.0027(10) -0.0003(10) -0.0011(10) C8 0.0357(15) 0.0511(18) 0.0208(13) -0.0074(12) 0.0009(11) 0.0016(13) C9 0.0385(15) 0.0383(15) 0.0217(13) -0.0077(11) -0.0062(11) -0.0006(12) C10 0.053(2) 0.072(2) 0.0266(15) -0.0183(15) -0.0123(14) -0.0047(17) C11 0.0380(15) 0.0278(13) 0.0241(13) 0.0022(10) -0.0075(11) -0.0078(11) C12 0.0238(12) 0.0206(11) 0.0229(12) -0.0037(9) 0.0007(10) -0.0034(9) C13 0.0258(13) 0.0215(12) 0.0336(14) -0.0053(10) 0.0019(11) -0.0077(10) C14 0.0199(11) 0.0216(12) 0.0361(14) -0.0130(10) -0.0030(10) -0.0038(9) C15 0.0272(13) 0.0307(14) 0.0454(17) -0.0145(12) -0.0069(12) -0.0079(11) C16 0.0198(11) 0.0223(11) 0.0181(11) -0.0016(9) -0.0013(9) -0.0049(9) C17 0.0197(11) 0.0226(11) 0.0164(11) -0.0021(9) -0.0026(9) -0.0035(9) C18 0.0217(11) 0.0185(11) 0.0259(12) -0.0046(9) -0.0071(10) -0.0033(9) C19 0.0224(12) 0.0386(15) 0.0358(15) -0.0168(12) -0.0014(11) -0.0054(11) C20 0.0335(15) 0.0450(17) 0.0402(16) -0.0261(14) -0.0064(12) -0.0051(13) C21 0.0291(14) 0.0306(14) 0.0402(16) -0.0091(12) -0.0117(12) -0.0101(11) C22 0.0222(12) 0.0344(14) 0.0323(14) -0.0055(11) -0.0026(11) -0.0086(11) C23 0.0247(12) 0.0319(13) 0.0217(12) -0.0107(10) -0.0035(10) -0.0044(10) C24 0.0246(12) 0.0201(11) 0.0220(12) -0.0042(9) -0.0026(10) -0.0061(9) C25 0.0272(13) 0.0283(13) 0.0264(13) -0.0066(10) -0.0059(10) -0.0025(10) C26 0.0305(14) 0.0262(13) 0.0341(15) -0.0038(11) -0.0063(11) 0.0030(11) C27 0.0424(16) 0.0201(12) 0.0404(16) -0.0076(11) -0.0014(13) -0.0013(11) C28 0.0418(16) 0.0281(14) 0.0368(15) -0.0139(12) -0.0082(12) -0.0088(12) C29 0.0278(13) 0.0254(12) 0.0293(13) -0.0070(10) -0.0086(11) -0.0030(10) B1 0.0255(14) 0.0236(13) 0.0220(14) -0.0053(11) -0.0095(11) -0.0043(11) Sb1 0.03287(11) 0.03683(11) 0.02777(10) 0.00367(8) -0.00716(8) -0.00495(8) Cl3 0.0551(5) 0.0359(4) 0.0597(5) -0.0014(4) -0.0074(4) -0.0020(4) Cl4 0.0378(4) 0.0620(5) 0.0489(5) 0.0166(4) 0.0043(4) -0.0038(4) Cl5 0.0724(6) 0.0869(7) 0.0354(4) -0.0037(4) -0.0238(4) 0.0070(5) C99 0.070(5) 0.049(4) 0.061(5) -0.007(4) -0.011(4) -0.007(4) Cl6 0.0758(14) 0.0681(12) 0.0553(12) -0.0219(10) -0.0193(9) 0.0044(11) Cl7 0.135(4) 0.120(3) 0.096(3) -0.009(3) -0.068(3) -0.033(3) C99A 0.074(5) 0.055(5) 0.059(5) 0.004(4) -0.005(4) 0.009(4) Cl7A 0.094(3) 0.0602(14) 0.0662(16) 0.0061(11) -0.0036(18) -0.0064(17) Cl6A 0.0529(12) 0.1006(18) 0.0986(17) -0.0387(14) -0.0233(11) 0.0019(11) _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 C16 2.038(2) . ? Mo1 C17 2.039(2) . ? Mo1 N5 2.1558(19) . ? Mo1 N3 2.182(2) . ? Mo1 N1 2.2684(19) . ? Mo1 Cl2 2.3915(7) . ? Mo1 Cl1 2.4497(7) . ? Cl1 Sb1 3.1146(7) . ? N1 C2 1.355(3) . ? N1 N2 1.379(3) . ? N2 C4 1.356(3) . ? N2 B1 1.535(3) . ? N3 C7 1.349(3) . ? N3 N4 1.384(3) . ? N4 C9 1.343(3) . ? N4 B1 1.537(4) . ? N5 C12 1.350(3) . ? N5 N6 1.384(3) . ? N6 C14 1.357(3) . ? N6 B1 1.538(3) . ? C1 C2 1.490(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.384(4) . ? C3 C4 1.378(4) . ? C3 H3A 0.9500 . ? C4 C5 1.492(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.492(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.388(4) . ? C8 C9 1.382(4) . ? C8 H8A 0.9500 . ? C9 C10 1.501(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.489(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.390(3) . ? C13 C14 1.375(4) . ? C13 H13A 0.9500 . ? C14 C15 1.501(3) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.301(3) . ? C16 C24 1.458(3) . ? C17 C18 1.458(3) . ? C18 C19 1.386(4) . ? C18 C23 1.400(3) . ? C19 C20 1.393(4) . ? C19 H19A 0.9500 . ? C20 C21 1.385(4) . ? C20 H20A 0.9500 . ? C21 C22 1.385(4) . ? C21 H21A 0.9500 . ? C22 C23 1.388(3) . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? C24 C29 1.400(3) . ? C24 C25 1.401(3) . ? C25 C26 1.389(4) . ? C25 H25A 0.9500 . ? C26 C27 1.380(4) . ? C26 H26A 0.9500 . ? C27 C28 1.381(4) . ? C27 H27A 0.9500 . ? C28 C29 1.381(4) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? B1 H1 1.0000 . ? Sb1 Cl4 2.3486(9) . ? Sb1 Cl3 2.3578(9) . ? Sb1 Cl5 2.3933(9) . ? C99 Cl6 1.679(8) . ? C99 Cl7 1.777(9) . ? C99 H99A 0.9900 . ? C99 H99B 0.9900 . ? Cl6 Cl6 1.125(4) 2_585 ? C99A Cl7A 1.725(9) . ? C99A Cl6A 1.762(8) . ? C99A H99C 0.9900 . ? C99A H99D 0.9900 . ? Cl6A Cl6A 2.189(6) 2_685 ? 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 C16 Mo1 C17 37.21(9) . . ? C16 Mo1 N5 84.90(8) . . ? C17 Mo1 N5 116.41(8) . . ? C16 Mo1 N3 83.24(8) . . ? C17 Mo1 N3 104.58(8) . . ? N5 Mo1 N3 85.44(7) . . ? C16 Mo1 N1 161.63(8) . . ? C17 Mo1 N1 160.39(8) . . ? N5 Mo1 N1 81.77(7) . . ? N3 Mo1 N1 83.15(7) . . ? C16 Mo1 Cl2 108.16(7) . . ? C17 Mo1 Cl2 89.18(7) . . ? N5 Mo1 Cl2 87.88(6) . . ? N3 Mo1 Cl2 166.24(5) . . ? N1 Mo1 Cl2 83.99(5) . . ? C16 Mo1 Cl1 109.18(7) . . ? C17 Mo1 Cl1 80.43(7) . . ? N5 Mo1 Cl1 162.68(5) . . ? N3 Mo1 Cl1 86.28(5) . . ? N1 Mo1 Cl1 82.16(5) . . ? Cl2 Mo1 Cl1 96.82(2) . . ? Mo1 Cl1 Sb1 97.60(2) . . ? C2 N1 N2 106.73(19) . . ? C2 N1 Mo1 134.19(16) . . ? N2 N1 Mo1 118.36(14) . . ? C4 N2 N1 109.7(2) . . ? C4 N2 B1 130.6(2) . . ? N1 N2 B1 119.67(18) . . ? C7 N3 N4 106.36(19) . . ? C7 N3 Mo1 133.34(16) . . ? N4 N3 Mo1 120.30(14) . . ? C9 N4 N3 109.7(2) . . ? C9 N4 B1 130.6(2) . . ? N3 N4 B1 119.59(19) . . ? C12 N5 N6 106.95(19) . . ? C12 N5 Mo1 133.51(16) . . ? N6 N5 Mo1 119.38(14) . . ? C14 N6 N5 109.06(19) . . ? C14 N6 B1 129.7(2) . . ? N5 N6 B1 121.25(18) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 108.9(2) . . ? N1 C2 C1 124.9(2) . . ? C3 C2 C1 126.2(2) . . ? C4 C3 C2 107.4(2) . . ? C4 C3 H3A 126.3 . . ? C2 C3 H3A 126.3 . . ? N2 C4 C3 107.3(2) . . ? N2 C4 C5 123.4(3) . . ? C3 C4 C5 129.3(2) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N3 C7 C8 109.5(2) . . ? N3 C7 C6 123.6(2) . . ? C8 C7 C6 126.8(2) . . ? C9 C8 C7 106.4(2) . . ? C9 C8 H8A 126.8 . . ? C7 C8 H8A 126.8 . . ? N4 C9 C8 107.9(2) . . ? N4 C9 C10 122.9(3) . . ? C8 C9 C10 129.2(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N5 C12 C13 109.2(2) . . ? N5 C12 C11 123.2(2) . . ? C13 C12 C11 127.6(2) . . ? C14 C13 C12 106.9(2) . . ? C14 C13 H13A 126.6 . . ? C12 C13 H13A 126.6 . . ? N6 C14 C13 108.0(2) . . ? N6 C14 C15 122.5(2) . . ? C13 C14 C15 129.5(2) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C24 143.5(2) . . ? C17 C16 Mo1 71.46(14) . . ? C24 C16 Mo1 145.05(17) . . ? C16 C17 C18 146.4(2) . . ? C16 C17 Mo1 71.34(14) . . ? C18 C17 Mo1 141.85(18) . . ? C19 C18 C23 119.0(2) . . ? C19 C18 C17 121.3(2) . . ? C23 C18 C17 119.7(2) . . ? C18 C19 C20 120.3(2) . . ? C18 C19 H19A 119.8 . . ? C20 C19 H19A 119.8 . . ? C21 C20 C19 120.2(3) . . ? C21 C20 H20A 119.9 . . ? C19 C20 H20A 119.9 . . ? C22 C21 C20 120.0(2) . . ? C22 C21 H21A 120.0 . . ? C20 C21 H21A 120.0 . . ? C21 C22 C23 119.9(2) . . ? C21 C22 H22A 120.1 . . ? C23 C22 H22A 120.1 . . ? C22 C23 C18 120.5(2) . . ? C22 C23 H23A 119.7 . . ? C18 C23 H23A 119.7 . . ? C29 C24 C25 119.1(2) . . ? C29 C24 C16 122.2(2) . . ? C25 C24 C16 118.7(2) . . ? C26 C25 C24 120.4(2) . . ? C26 C25 H25A 119.8 . . ? C24 C25 H25A 119.8 . . ? C27 C26 C25 119.8(2) . . ? C27 C26 H26A 120.1 . . ? C25 C26 H26A 120.1 . . ? C26 C27 C28 120.2(2) . . ? C26 C27 H27A 119.9 . . ? C28 C27 H27A 119.9 . . ? C27 C28 C29 120.8(2) . . ? C27 C28 H28A 119.6 . . ? C29 C28 H28A 119.6 . . ? C28 C29 C24 119.7(2) . . ? C28 C29 H29A 120.1 . . ? C24 C29 H29A 120.1 . . ? N2 B1 N4 107.7(2) . . ? N2 B1 N6 110.2(2) . . ? N4 B1 N6 109.15(19) . . ? N2 B1 H1 109.9 . . ? N4 B1 H1 109.9 . . ? N6 B1 H1 109.9 . . ? Cl4 Sb1 Cl3 93.68(3) . . ? Cl4 Sb1 Cl5 94.10(4) . . ? Cl3 Sb1 Cl5 95.38(4) . . ? Cl4 Sb1 Cl1 83.70(3) . . ? Cl3 Sb1 Cl1 90.84(3) . . ? Cl5 Sb1 Cl1 173.53(3) . . ? Cl6 C99 Cl7 112.3(5) . . ? Cl6 C99 H99A 109.1 . . ? Cl7 C99 H99A 109.1 . . ? Cl6 C99 H99B 109.1 . . ? Cl7 C99 H99B 109.1 . . ? H99A C99 H99B 107.9 . . ? Cl6 Cl6 C99 129.3(4) 2_585 . ? Cl7A C99A Cl6A 112.1(4) . . ? Cl7A C99A H99C 109.2 . . ? Cl6A C99A H99C 109.2 . . ? Cl7A C99A H99D 109.2 . . ? Cl6A C99A H99D 109.2 . . ? H99C C99A H99D 107.9 . . ? C99A Cl6A Cl6A 116.5(3) . 2_685 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.663 _refine_diff_density_min -0.725 _refine_diff_density_rms 0.077