# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email j.mcmaster@nottingham.ac.uk _publ_contact_author_name 'Jonathan McMaster' loop_ _publ_author_name 'Jonathan McMaster' C.Garner E.Davies D.Collison M.Helliwell F.Mabbs C.Wilson A.Blake A.Whalley H.Disley data_1 _database_code_depnum_ccdc_archive 'CCDC 822493' #TrackingRef '- combined.cif' #CPMOSS _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H16 Mo S2' _chemical_formula_sum 'C18 H16 Mo S2' _chemical_formula_weight 392.37 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' S S 0.1246 0.1234 '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 8.8648(8) _cell_length_b 15.5930(10) _cell_length_c 10.8010(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.990(2) _cell_angle_gamma 90.00 _cell_volume 1492.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4050 _cell_measurement_theta_min 4.6 _cell_measurement_theta_max 56.5 _exptl_crystal_description 'rectangular plate' _exptl_crystal_colour red _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.746 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 1.147 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.687 _exptl_absorpt_correction_T_max 0.815 _exptl_absorpt_process_details 'XPREP (Bruker, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker SMART CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 9524 _diffrn_reflns_av_R_equivalents 0.055 _diffrn_reflns_av_sigmaI/netI 0.041 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 28.75 _reflns_number_total 3612 _reflns_number_gt 2774 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART version 5.054 (Bruker, 1998)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT version 6.01 (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC version 5.03 (Sheldrick, 1994)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.033P)^2^] 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 3471 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0395 _refine_ls_R_factor_gt 0.0279 _refine_ls_wR_factor_ref 0.0650 _refine_ls_wR_factor_gt 0.0619 _refine_ls_goodness_of_fit_ref 0.964 _refine_ls_restrained_S_all 0.964 _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 Mo Mo 0.44185(2) 0.125299(13) 0.76484(2) 0.01838(7) Uani 1 1 d . . . C1C C 0.2170(3) 0.1301(2) 0.6471(3) 0.0403(7) Uani 1 1 d . . . H1CA H 0.1695 0.1829 0.6112 0.048 Uiso 1 1 calc R . . C2C C 0.3113(3) 0.0743(2) 0.5854(3) 0.0361(7) Uani 1 1 d . . . H2CA H 0.3452 0.0806 0.4980 0.043 Uiso 1 1 calc R . . C3C C 0.3443(3) 0.00587(18) 0.6640(3) 0.0370(7) Uani 1 1 d . . . H3CA H 0.4026 -0.0466 0.6413 0.044 Uiso 1 1 calc R . . C4C C 0.2674(3) 0.01829(19) 0.7759(3) 0.0363(7) Uani 1 1 d . . . H4CA H 0.2579 -0.0243 0.8444 0.044 Uiso 1 1 calc R . . C5C C 0.1861(3) 0.0948(2) 0.7630(3) 0.0386(7) Uani 1 1 d . . . H5CA H 0.1112 0.1174 0.8229 0.046 Uiso 1 1 calc R . . C6C C 0.3822(4) 0.26784(19) 0.8157(4) 0.0478(9) Uani 1 1 d . . . H6CA H 0.3111 0.3059 0.7684 0.057 Uiso 1 1 calc R . . C7C C 0.5342(3) 0.26512(16) 0.8027(3) 0.0322(7) Uani 1 1 d . . . H7CA H 0.5930 0.3004 0.7430 0.039 Uiso 1 1 calc R . . C8C C 0.5953(4) 0.20848(18) 0.8877(3) 0.0422(8) Uani 1 1 d . . . H8CA H 0.7054 0.1988 0.9038 0.051 Uiso 1 1 calc R . . C9C C 0.4767(6) 0.1767(2) 0.9604(3) 0.0690(14) Uani 1 1 d . . . H9CA H 0.4873 0.1420 1.0379 0.083 Uiso 1 1 calc R . . C10C C 0.3444(5) 0.2149(2) 0.9143(4) 0.0713(14) Uani 1 1 d . . . H10A H 0.2422 0.2099 0.9513 0.086 Uiso 1 1 calc R . . S1 S 0.63408(7) 0.13720(4) 0.60675(6) 0.02197(14) Uani 1 1 d . . . S2 S 0.61201(7) 0.01460(4) 0.84457(6) 0.02495(15) Uani 1 1 d . . . C1 C 0.7733(3) 0.06239(15) 0.6464(2) 0.0218(5) Uani 1 1 d . . . H1A H 0.8599 0.0593 0.5960 0.026 Uiso 1 1 calc R . . C2 C 0.7659(3) 0.00953(15) 0.7424(2) 0.0220(5) Uani 1 1 d . . . C1P C 0.8803(3) -0.05728(15) 0.7689(3) 0.0248(6) Uani 1 1 d . . . C2P C 0.9113(3) -0.08461(19) 0.8885(3) 0.0383(7) Uani 1 1 d . . . H2PA H 0.8615 -0.0584 0.9559 0.046 Uiso 1 1 calc R . . C3P C 1.0146(3) -0.1502(2) 0.9111(3) 0.0500(9) Uani 1 1 d . . . H3PA H 1.0354 -0.1679 0.9938 0.060 Uiso 1 1 calc R . . C4P C 1.0864(3) -0.18927(18) 0.8156(4) 0.0488(9) Uani 1 1 d . . . H4PA H 1.1543 -0.2353 0.8315 0.059 Uiso 1 1 calc R . . C5P C 1.0599(3) -0.16175(19) 0.6960(3) 0.0431(8) Uani 1 1 d . . . H5PA H 1.1125 -0.1873 0.6296 0.052 Uiso 1 1 calc R . . C6P C 0.9573(3) -0.09709(17) 0.6727(3) 0.0321(7) Uani 1 1 d . . . H6PA H 0.9385 -0.0792 0.5898 0.039 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo 0.02069(12) 0.01557(11) 0.01887(12) -0.00182(8) 0.00009(8) -0.00011(8) C1C 0.0356(16) 0.0462(18) 0.0386(18) 0.0009(15) -0.0166(14) 0.0067(14) C2C 0.0295(15) 0.0560(19) 0.0223(15) -0.0101(14) -0.0074(12) -0.0101(14) C3C 0.0354(16) 0.0286(15) 0.0467(19) -0.0174(14) -0.0074(14) -0.0092(12) C4C 0.0297(15) 0.0388(16) 0.0403(18) 0.0044(14) -0.0023(13) -0.0182(13) C5C 0.0193(14) 0.061(2) 0.0355(18) -0.0117(15) -0.0004(12) 0.0023(13) C6C 0.0427(19) 0.0234(15) 0.077(3) -0.0210(16) -0.0082(18) 0.0098(14) C7C 0.0456(18) 0.0162(13) 0.0352(17) -0.0061(11) 0.0098(13) -0.0042(12) C8C 0.0462(18) 0.0240(15) 0.055(2) -0.0139(14) -0.0241(16) -0.0049(13) C9C 0.165(5) 0.0273(18) 0.0150(16) -0.0069(13) 0.011(2) -0.028(2) C10C 0.071(3) 0.046(2) 0.099(3) -0.048(2) 0.058(3) -0.028(2) S1 0.0252(3) 0.0203(3) 0.0205(3) 0.0017(2) 0.0013(2) -0.0001(2) S2 0.0232(3) 0.0253(3) 0.0264(4) 0.0079(3) 0.0034(3) 0.0032(3) C1 0.0183(12) 0.0233(12) 0.0238(14) -0.0019(10) 0.0006(10) -0.0007(10) C2 0.0174(12) 0.0222(12) 0.0264(14) -0.0040(11) -0.0021(10) -0.0016(10) C1P 0.0175(12) 0.0205(12) 0.0364(16) 0.0027(11) -0.0014(11) -0.0040(10) C2P 0.0227(14) 0.0458(18) 0.047(2) 0.0184(15) 0.0088(13) 0.0061(13) C3P 0.0300(16) 0.055(2) 0.065(2) 0.0374(18) 0.0114(16) 0.0124(15) C4P 0.0253(16) 0.0279(16) 0.093(3) 0.0171(18) 0.0076(17) 0.0065(13) C5P 0.0249(15) 0.0299(16) 0.075(3) -0.0117(16) 0.0008(15) 0.0029(12) C6P 0.0213(14) 0.0310(14) 0.0440(18) -0.0092(13) -0.0043(12) -0.0013(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 Mo C9C 2.276(3) . ? Mo C4C 2.280(3) . ? Mo C8C 2.287(3) . ? Mo C10C 2.313(3) . ? Mo C5C 2.316(3) . ? Mo C3C 2.317(3) . ? Mo C1C 2.347(3) . ? Mo C6C 2.352(3) . ? Mo C7C 2.362(3) . ? Mo C2C 2.377(3) . ? Mo S1 2.4402(7) . Yes Mo S2 2.4397(7) . Yes C1C C2C 1.385(4) . ? C1C C5C 1.399(4) . ? C2C C3C 1.392(4) . ? C3C C4C 1.411(4) . ? C4C C5C 1.399(4) . ? C6C C7C 1.358(4) . ? C6C C10C 1.393(5) . ? C7C C8C 1.378(4) . ? C8C C9C 1.413(5) . ? C9C C10C 1.398(6) . ? S1 C1 1.746(2) . Yes S2 C2 1.771(3) . Yes C1 C2 1.327(3) . Yes C2 C1P 1.478(3) . ? C1P C2P 1.384(4) . ? C1P C6P 1.398(4) . ? C2P C3P 1.392(4) . ? C3P C4P 1.365(5) . ? C4P C5P 1.377(5) . ? C5P C6P 1.378(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C9C Mo C4C 106.91(13) . . ? C9C Mo C8C 36.07(13) . . ? C4C Mo C8C 141.44(12) . . ? C9C Mo C10C 35.47(15) . . ? C4C Mo C10C 98.26(12) . . ? C8C Mo C10C 58.54(13) . . ? C9C Mo C5C 101.40(15) . . ? C4C Mo C5C 35.43(11) . . ? C8C Mo C5C 133.93(12) . . ? C10C Mo C5C 75.70(13) . . ? C9C Mo C3C 139.74(11) . . ? C4C Mo C3C 35.73(10) . . ? C8C Mo C3C 160.37(11) . . ? C10C Mo C3C 132.25(12) . . ? C5C Mo C3C 58.22(11) . . ? C9C Mo C1C 126.30(16) . . ? C4C Mo C1C 58.73(11) . . ? C8C Mo C1C 141.94(11) . . ? C10C Mo C1C 92.01(15) . . ? C5C Mo C1C 34.90(11) . . ? C3C Mo C1C 57.60(11) . . ? C9C Mo C6C 58.50(13) . . ? C4C Mo C6C 121.61(11) . . ? C8C Mo C6C 57.48(11) . . ? C10C Mo C6C 34.74(13) . . ? C5C Mo C6C 88.41(11) . . ? C3C Mo C6C 141.78(11) . . ? C1C Mo C6C 84.51(11) . . ? C9C Mo C7C 58.20(11) . . ? C4C Mo C7C 154.16(11) . . ? C8C Mo C7C 34.44(10) . . ? C10C Mo C7C 56.94(11) . . ? C5C Mo C7C 121.83(10) . . ? C3C Mo C7C 161.54(11) . . ? C1C Mo C7C 110.67(10) . . ? C6C Mo C7C 33.48(10) . . ? C9C Mo C2C 158.61(15) . . ? C4C Mo C2C 58.45(11) . . ? C8C Mo C2C 159.88(12) . . ? C10C Mo C2C 126.05(15) . . ? C5C Mo C2C 57.42(10) . . ? C3C Mo C2C 34.47(10) . . ? C1C Mo C2C 34.09(10) . . ? C6C Mo C2C 113.46(11) . . ? C7C Mo C2C 127.74(11) . . ? C9C Mo S2 81.29(12) . . ? C4C Mo S2 83.09(8) . . ? C8C Mo S2 80.71(8) . . ? C10C Mo S2 114.64(14) . . ? C5C Mo S2 117.19(8) . . ? C3C Mo S2 79.68(8) . . ? C1C Mo S2 136.71(8) . . ? C6C Mo S2 136.58(9) . . ? C7C Mo S2 112.44(7) . . ? C2C Mo S2 109.92(8) . . ? C9C Mo S1 122.52(12) . . ? C4C Mo S1 125.09(8) . . ? C8C Mo S1 86.98(9) . . ? C10C Mo S1 135.73(9) . . ? C5C Mo S1 134.81(8) . . ? C3C Mo S1 89.53(8) . . ? C1C Mo S1 102.43(8) . . ? C6C Mo S1 104.71(10) . . ? C7C Mo S1 78.85(7) . . ? C2C Mo S1 77.93(7) . . ? S1 Mo S2 82.29(2) . . Yes C2C C1C C5C 108.2(3) . . ? C2C C1C Mo 74.14(15) . . ? C5C C1C Mo 71.32(16) . . ? C1C C2C C3C 108.0(3) . . ? C1C C2C Mo 71.77(16) . . ? C3C C2C Mo 70.41(15) . . ? C2C C3C C4C 108.5(3) . . ? C2C C3C Mo 75.13(16) . . ? C4C C3C Mo 70.68(15) . . ? C5C C4C C3C 106.7(3) . . ? C5C C4C Mo 73.70(16) . . ? C3C C4C Mo 73.59(15) . . ? C4C C5C C1C 108.5(3) . . ? C4C C5C Mo 70.87(15) . . ? C1C C5C Mo 73.78(17) . . ? C7C C6C C10C 108.2(3) . . ? C7C C6C Mo 73.68(15) . . ? C10C C6C Mo 71.11(18) . . ? C6C C7C C8C 109.3(3) . . ? C6C C7C Mo 72.85(16) . . ? C8C C7C Mo 69.81(15) . . ? C7C C8C C9C 107.9(3) . . ? C7C C8C Mo 75.75(16) . . ? C9C C8C Mo 71.51(17) . . ? C10C C9C C8C 106.3(3) . . ? C10C C9C Mo 73.7(2) . . ? C8C C9C Mo 72.42(17) . . ? C6C C10C C9C 108.2(3) . . ? C6C C10C Mo 74.15(19) . . ? C9C C10C Mo 70.80(18) . . ? Mo S1 C1 106.06(9) . . Yes Mo S2 C2 106.85(8) . . Yes S1 C1 C2 124.2(2) . . Yes C1 C2 C1P 123.1(2) . . ? C1 C2 S2 120.55(19) . . Yes C1P C2 S2 116.38(19) . . ? C2P C1P C6P 117.7(3) . . ? C2P C1P C2 121.5(2) . . ? C6P C1P C2 120.8(2) . . ? C1P C2P C3P 120.6(3) . . ? C4P C3P C2P 120.7(3) . . ? C3P C4P C5P 119.7(3) . . ? C4P C5P C6P 120.0(3) . . ? C5P C6P C1P 121.2(3) . . ? _diffrn_measured_fraction_theta_max 0.898 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.65 _refine_diff_density_min -0.54 _refine_diff_density_rms 0.08 #=== END of CIF data_2 _database_code_depnum_ccdc_archive 'CCDC 822494' #TrackingRef '- combined.cif' #_CPMOBF _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H16 Mo S2 +, B F4 -' _chemical_formula_sum 'C18 H16 B F4 Mo S2' _chemical_formula_weight 479.20 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 'P 21/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 6.7275(5) _cell_length_b 14.586(1) _cell_length_c 18.307(10) _cell_angle_alpha 90.00 _cell_angle_beta 98.2730(1) _cell_angle_gamma 90.00 _cell_volume 1777.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6065 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 27.74 _exptl_crystal_description Sphenoid _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.790 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 956 _exptl_absorpt_coefficient_mu 1.011 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.638 _exptl_absorpt_correction_T_max 0.878 _exptl_absorpt_process_details 'SADABS, Bruker 1999' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 15612 _diffrn_reflns_av_R_equivalents 0.101 _diffrn_reflns_av_sigmaI/netI 0.033 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 28.74 _reflns_number_total 4343 _reflns_number_gt 3265 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL(Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; ; _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^)+(0.081P)^2^+1.457P] 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 4176 _refine_ls_number_parameters 217 _refine_ls_number_restraints 135 _refine_ls_R_factor_all 0.0633 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_ref 0.138 _refine_ls_wR_factor_gt 0.129 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.166 _refine_ls_shift/su_max 0.007 _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 Mo Mo 0.10207(5) 0.66008(2) 0.35097(2) 0.03255(15) Uani 1 1 d U . . S1 S 0.44975(18) 0.70533(9) 0.35963(10) 0.0562(4) Uani 1 1 d U . . S2 S 0.05784(19) 0.82372(9) 0.36571(10) 0.0592(4) Uani 1 1 d U . . C1 C 0.4571(7) 0.8166(3) 0.3804(3) 0.0409(10) Uani 1 1 d U . . C2 C 0.2929(7) 0.8710(3) 0.3843(2) 0.0370(9) Uani 1 1 d U . . H2A H 0.5856 0.8447 0.3902 0.049 Uiso 1 1 calc R . . C2P C 0.3090(7) 0.9696(3) 0.4018(2) 0.0373(9) Uani 1 1 d U . . C1P C 0.4829(8) 1.0183(4) 0.3938(3) 0.0466(11) Uani 1 1 d U . . H2PA H 0.5927 0.9875 0.3774 0.056 Uiso 1 1 calc R . . C3P C 0.4975(9) 1.1111(4) 0.4094(3) 0.0524(12) Uani 1 1 d U . . H3PA H 0.6166 1.1435 0.4033 0.063 Uiso 1 1 calc R . . C4P C 0.3408(10) 1.1563(3) 0.4335(3) 0.0525(13) Uani 1 1 d U . . H4PA H 0.3508 1.2201 0.4441 0.063 Uiso 1 1 calc R . . C5P C 0.1704(9) 1.1094(4) 0.4424(3) 0.0534(13) Uani 1 1 d U . . H5PA H 0.0629 1.1407 0.4599 0.064 Uiso 1 1 calc R . . C6P C 0.1517(8) 1.0167(3) 0.4262(3) 0.0441(10) Uani 1 1 d U . . H6PA H 0.0310 0.9853 0.4318 0.053 Uiso 1 1 calc R . . C6C C 0.2422(9) 0.5777(5) 0.4538(3) 0.0646(15) Uani 1 1 d U A . H6CA H 0.3857 0.5581 0.4654 0.078 Uiso 1 1 calc R . . C7C C 0.0856(10) 0.5252(4) 0.4184(3) 0.0602(13) Uani 1 1 d U A . H7CA H 0.0973 0.4616 0.3991 0.072 Uiso 1 1 calc R . . C8C C -0.0949(9) 0.5737(4) 0.4199(3) 0.0530(12) Uani 1 1 d U A . H8CA H -0.2330 0.5501 0.4021 0.064 Uiso 1 1 calc R . . C9C C -0.0499(8) 0.6566(4) 0.4554(3) 0.0534(12) Uani 1 1 d U A . H9CA H -0.1497 0.7021 0.4688 0.064 Uiso 1 1 calc R . . C20C C 0.1606(9) 0.6616(5) 0.4753(3) 0.0638(15) Uani 1 1 d U A . H10A H 0.2353 0.7102 0.5067 0.077 Uiso 1 1 calc R . . B B 0.5093(8) 0.3903(3) 0.3341(3) 0.0642(17) Uani 1 1 d DU . . F1 F 0.4243(13) 0.3735(6) 0.3963(4) 0.110(3) Uani 0.60 1 d PDU A 1 F2 F 0.4043(13) 0.3604(7) 0.2734(4) 0.179(6) Uani 0.60 1 d PDU A 1 F3 F 0.5208(10) 0.4840(4) 0.3301(6) 0.127(4) Uani 0.60 1 d PDU A 1 F4 F 0.7001(11) 0.3592(7) 0.3436(5) 0.178(6) Uani 0.60 1 d PDU A 1 F1A F 0.4953(18) 0.4284(7) 0.3973(5) 0.106(4) Uiso 0.40 1 d PDU A 2 F2A F 0.3224(14) 0.3864(7) 0.2919(6) 0.110(5) Uiso 0.40 1 d PDU A 2 F3A F 0.6307(19) 0.4360(8) 0.2953(8) 0.197(9) Uiso 0.40 1 d PDU A 2 F4A F 0.5675(5) 0.3015(2) 0.33933(14) 0.097(4) Uiso 0.40 1 d PDU A 2 C2C C 0.0211(5) 0.5491(2) 0.25925(14) 0.0412(16) Uiso 0.65 1 d PRU A 1 H1CA H 0.0285 0.4812 0.2666 0.049 Uiso 0.65 1 calc PR A 1 C1C C -0.1517(5) 0.6046(2) 0.26076(14) 0.0375(14) Uiso 0.65 1 d PRU A 1 H2CA H -0.2870 0.5826 0.2695 0.045 Uiso 0.65 1 calc PR A 1 C3C C -0.1022(5) 0.6957(2) 0.24284(14) 0.0436(16) Uiso 0.65 1 d PRU A 1 H3CA H -0.1977 0.7485 0.2353 0.052 Uiso 0.65 1 calc PR A 1 C4C C 0.1012(5) 0.6966(2) 0.23024(14) 0.0504(18) Uiso 0.65 1 d PRU A 1 H4CA H 0.1725 0.7497 0.2113 0.061 Uiso 0.65 1 calc PR A 1 C5C C 0.1774(5) 0.6060(2) 0.24038(14) 0.0422(16) Uiso 0.65 1 d PRU A 1 H5CA H 0.3124 0.5847 0.2306 0.051 Uiso 0.65 1 calc PR A 1 C2A C -0.0829(5) 0.5744(2) 0.25951(14) 0.049(3) Uiso 0.35 1 d PRU A 2 H1AA H -0.1715 0.5214 0.2674 0.059 Uiso 0.35 1 calc PR A 2 C1A C -0.1452(5) 0.6671(2) 0.24935(14) 0.042(3) Uiso 0.35 1 d PRU A 2 H2AA H -0.2850 0.6905 0.2491 0.050 Uiso 0.35 1 calc PR A 2 C3A C 0.0200(5) 0.7187(2) 0.23136(14) 0.049(3) Uiso 0.35 1 d PRU A 2 H3AA H 0.0173 0.7850 0.2173 0.059 Uiso 0.35 1 calc PR A 2 C4A C 0.1845(5) 0.6579(2) 0.23042(14) 0.052(4) Uiso 0.35 1 d PRU A 2 H4AA H 0.3179 0.6741 0.2160 0.062 Uiso 0.35 1 calc PR A 2 C5A C 0.1208(5) 0.5687(2) 0.24781(14) 0.045(3) Uiso 0.35 1 d PRU A 2 H5AA H 0.2010 0.5111 0.2469 0.054 Uiso 0.35 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo 0.0274(2) 0.0320(2) 0.0384(2) -0.00198(15) 0.00534(14) 0.00170(14) S2 0.0306(6) 0.0364(6) 0.1090(12) -0.0137(7) 0.0044(7) 0.0020(5) S1 0.0282(6) 0.0435(7) 0.0969(11) -0.0082(7) 0.0093(6) 0.0026(5) C2 0.040(2) 0.037(2) 0.033(2) 0.0007(18) 0.0035(17) -0.0047(18) C1 0.033(2) 0.046(2) 0.044(3) -0.001(2) 0.0055(18) -0.0046(19) C2P 0.046(2) 0.039(2) 0.026(2) 0.0008(17) 0.0021(17) -0.0034(18) C1P 0.050(3) 0.049(3) 0.041(3) -0.004(2) 0.006(2) -0.010(2) C3P 0.063(3) 0.049(3) 0.045(3) -0.003(2) 0.009(2) -0.020(2) C4P 0.082(4) 0.037(2) 0.037(3) -0.004(2) 0.005(2) -0.008(2) C5P 0.068(3) 0.046(3) 0.048(3) -0.008(2) 0.018(2) 0.001(2) C6P 0.049(3) 0.044(2) 0.041(3) -0.003(2) 0.010(2) -0.007(2) C6C 0.057(3) 0.089(4) 0.047(3) 0.022(3) 0.009(2) 0.029(3) C7C 0.085(4) 0.047(3) 0.053(3) 0.018(2) 0.026(3) 0.012(3) C8C 0.058(3) 0.057(3) 0.047(3) 0.013(2) 0.019(2) -0.003(2) C9C 0.048(3) 0.073(3) 0.042(3) -0.005(2) 0.016(2) 0.010(2) C20C 0.056(3) 0.092(4) 0.041(3) -0.014(3) 0.000(2) 0.003(3) B 0.073(4) 0.045(3) 0.072(4) -0.009(3) 0.002(3) 0.000(3) F1 0.149(8) 0.078(5) 0.110(6) 0.024(4) 0.040(6) 0.003(5) F2 0.116(7) 0.311(15) 0.114(7) -0.137(9) 0.027(5) -0.083(8) F3 0.054(4) 0.054(3) 0.274(12) 0.017(5) 0.033(5) -0.017(3) F4 0.135(7) 0.228(12) 0.159(9) -0.090(8) -0.021(6) 0.142(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo S1 2.413(2) . ? Mo S2 2.425(2) . ? Mo C20C 2.254(6) . ? Mo C4C 2.273(3) . ? Mo C9C 2.294(5) . ? Mo C5C 2.297(3) . ? Mo C3C 2.301(3) . ? Mo C2A 2.305(3) . ? Mo C1A 2.313(3) . ? Mo C6C 2.317(5) . ? Mo C8C 2.328(5) . ? Mo C5A 2.329(3) . ? Mo C7C 2.333(5) . ? Mo C2C 2.339(3) . ? S2 C2 1.714(5) . ? S1 C1 1.666(5) . ? C2 C1 1.370(7) . ? C2 C2P 1.474(6) . ? C2P C6P 1.389(7) . ? C2P C1P 1.395(7) . ? C1P C3P 1.383(7) . ? C3P C4P 1.370(8) . ? C4P C5P 1.366(8) . ? C5P C6P 1.385(7) . ? C6C C7C 1.386(9) . ? C6C C20C 1.420(9) . ? C7C C8C 1.409(8) . ? C8C C9C 1.385(8) . ? C9C C20C 1.413(8) . ? B F1A 1.299(7) . ? B F2 1.303(6) . ? B F3A 1.335(8) . ? B F4 1.349(6) . ? B F4A 1.352(5) . ? B F1 1.369(6) . ? B F3 1.372(6) . ? B F2A 1.379(7) . ? C2C C1C 1.4199 . ? C2C C5C 1.4200 . ? C1C C3C 1.4200 . ? C3C C4C 1.4200 . ? C4C C5C 1.4200 . ? C2A C1A 1.4199 . ? C2A C5A 1.4200 . ? C1A C3A 1.4201 . ? C3A C4A 1.4199 . ? C4A C5A 1.4200 . ? 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 S1 Mo S2 81.77(4) . . ? C20C Mo C4C 162.9(2) . . ? C20C Mo C9C 36.2(2) . . ? C4C Mo C9C 151.21(17) . . ? C20C Mo C5C 149.90(18) . . ? C4C Mo C5C 36.2 . . ? C9C Mo C5C 155.26(17) . . ? C20C Mo C3C 149.62(18) . . ? C4C Mo C3C 36.2 . . ? C9C Mo C3C 116.05(17) . . ? C5C Mo C3C 59.96(7) . . ? C20C Mo C2A 137.45(19) . . ? C4C Mo C2A 59.66(6) . . ? C9C Mo C2A 109.54(17) . . ? C5C Mo C2A 48.54(5) . . ? C3C Mo C2A 45.93(5) . . ? C20C Mo C1A 144.39(18) . . ? C4C Mo C1A 46.08(5) . . ? C9C Mo C1A 108.42(17) . . ? C5C Mo C1A 62.01(7) . . ? C3C Mo C1A 13.2 . . ? C2A Mo C1A 35.8 . . ? C20C Mo C6C 36.2(2) . . ? C4C Mo C6C 148.84(17) . . ? C9C Mo C6C 59.3(2) . . ? C5C Mo C6C 115.00(18) . . ? C3C Mo C6C 159.9(2) . . ? C2A Mo C6C 115.0(2) . . ? C1A Mo C6C 147.0(2) . . ? C20C Mo C8C 59.2(2) . . ? C4C Mo C8C 137.07(17) . . ? C9C Mo C8C 34.87(19) . . ? C5C Mo C8C 120.47(17) . . ? C3C Mo C8C 105.83(17) . . ? C2A Mo C8C 79.07(17) . . ? C1A Mo C8C 93.47(17) . . ? C6C Mo C8C 58.3(2) . . ? C20C Mo C5A 143.38(19) . . ? C4C Mo C5A 48.57(6) . . ? C9C Mo C5A 138.19(17) . . ? C5C Mo C5A 17.1 . . ? C3C Mo C5A 61.77(7) . . ? C2A Mo C5A 35.7 . . ? C1A Mo C5A 59.33(6) . . ? C6C Mo C5A 107.40(19) . . ? C8C Mo C5A 103.38(17) . . ? C20C Mo C7C 59.3(2) . . ? C4C Mo C7C 135.90(18) . . ? C9C Mo C7C 58.7(2) . . ? C5C Mo C7C 102.11(17) . . ? C3C Mo C7C 125.3(2) . . ? C2A Mo C7C 82.26(19) . . ? C1A Mo C7C 112.3(2) . . ? C6C Mo C7C 34.7(2) . . ? C8C Mo C7C 35.2(2) . . ? C5A Mo C7C 87.64(17) . . ? C20C Mo C2C 136.12(19) . . ? C4C Mo C2C 59.74(6) . . ? C9C Mo C2C 119.81(17) . . ? C5C Mo C2C 35.7 . . ? C3C Mo C2C 59.35(6) . . ? C2A Mo C2C 19.6 . . ? C1A Mo C2C 52.20(6) . . ? C6C Mo C2C 104.5(2) . . ? C8C Mo C2C 85.58(17) . . ? C5A Mo C2C 19.4 . . ? C7C Mo C2C 76.85(18) . . ? C2 S2 Mo 107.07(17) . . ? C1 S1 Mo 106.14(17) . . ? C1 C2 C2P 122.8(4) . . ? C1 C2 S2 119.0(4) . . ? C2P C2 S2 118.2(3) . . ? C2 C1 S1 125.3(4) . . ? C6P C2P C1P 118.1(4) . . ? C6P C2P C2 121.1(4) . . ? C1P C2P C2 120.8(4) . . ? C3P C1P C2P 120.8(5) . . ? C4P C3P C1P 120.2(5) . . ? C5P C4P C3P 119.6(5) . . ? C4P C5P C6P 121.1(5) . . ? C5P C6P C2P 120.1(5) . . ? C7C C6C C20C 107.9(5) . . ? C7C C6C Mo 73.3(3) . . ? C20C C6C Mo 69.5(3) . . ? C6C C7C C8C 108.3(5) . . ? C6C C7C Mo 72.0(3) . . ? C8C C7C Mo 72.2(3) . . ? C9C C8C C7C 108.4(5) . . ? C9C C8C Mo 71.2(3) . . ? C7C C8C Mo 72.6(3) . . ? C8C C9C C20C 108.1(5) . . ? C8C C9C Mo 73.9(3) . . ? C20C C9C Mo 70.4(3) . . ? C9C C20C C6C 107.2(6) . . ? C9C C20C Mo 73.4(3) . . ? C6C C20C Mo 74.3(3) . . ? F1A B F2 143.4(7) . . ? F1A B F3A 112.9(6) . . ? F2 B F3A 90.7(8) . . ? F1A B F4 102.6(6) . . ? F2 B F4 112.7(5) . . ? F3A B F4 66.0(7) . . ? F1A B F4A 113.8(6) . . ? F2 B F4A 81.7(6) . . ? F3A B F4A 108.8(6) . . ? F4 B F4A 53.7(5) . . ? F2 B F1 114.2(6) . . ? F3A B F1 153.3(7) . . ? F4 B F1 109.6(5) . . ? F4A B F1 85.4(4) . . ? F1A B F3 68.5(6) . . ? F2 B F3 108.4(6) . . ? F3A B F3 55.3(6) . . ? F4 B F3 106.4(5) . . ? F4A B F3 160.1(5) . . ? F1 B F3 104.9(5) . . ? F1A B F2A 109.9(6) . . ? F3A B F2A 107.5(6) . . ? F4 B F2A 146.3(6) . . ? F4A B F2A 103.4(5) . . ? F1 B F2A 90.1(7) . . ? F3 B F2A 93.8(6) . . ? C1C C2C C5C 108.0 . . ? C1C C2C Mo 72.45(8) . . ? C5C C2C Mo 70.54(8) . . ? C2C C1C C3C 108.0 . . ? C2C C1C Mo 72.23(8) . . ? C3C C1C Mo 70.63(8) . . ? C1C C3C C4C 108.0 . . ? C1C C3C Mo 73.77(8) . . ? C4C C3C Mo 70.83(8) . . ? C5C C4C C3C 108.0 . . ? C5C C4C Mo 72.81(8) . . ? C3C C4C Mo 73.00(8) . . ? C4C C5C C2C 108.0 . . ? C4C C5C Mo 70.98(8) . . ? C2C C5C Mo 73.80(9) . . ? C1A C2A C5A 108.0 . . ? C1A C2A Mo 72.39(8) . . ? C5A C2A Mo 73.09(8) . . ? C2A C1A C3A 108.0 . . ? C2A C1A Mo 71.80(8) . . ? C3A C1A Mo 73.36(9) . . ? C4A C3A C1A 108.0 . . ? C4A C3A Mo 72.77(8) . . ? C1A C3A Mo 71.13(8) . . ? C3A C4A C5A 108.0 . . ? C3A C4A Mo 72.01(8) . . ? C5A C4A Mo 71.48(8) . . ? C2A C5A C4A 108.0 . . ? C2A C5A Mo 71.23(8) . . ? C4A C5A Mo 73.20(8) . . ? _diffrn_measured_fraction_theta_max 0.906 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.04 _refine_diff_density_min -0.94 _refine_diff_density_rms 0.11 #=== END of CIF data_3 _database_code_depnum_ccdc_archive 'CCDC 822495' #TrackingRef '- combined.cif' #S715 #------------------------------------------------------------------------------ _audit_creation_date 19106-09-27 _audit_creation_method 'by teXsan v1.7' _audit_update_record ; ? ; _publ_section_exptl_refinement ; ; _publ_section_comment ; ; _publ_section_references ; Molecular Structure Corporation. (1995). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564. Beurskens, P.T., Admiraal, G., Beurskens, G., Bosman, W.P., Garcia-Granda, S., Gould, R.O., Smits, J.M.M. and Smykalla, C. (1992). The DIRDIF program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. ; _publ_section_acknowledgements ; ; _publ_section_table_legends ; ; _publ_section_figure_captions ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H15 Mo N S2' _chemical_formula_sum 'C17 H15 Mo N S2' _chemical_formula_weight 393.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/a ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 10.732(2) _cell_length_b 16.083(2) _cell_length_c 8.660(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.16(2) _cell_angle_gamma 90.00 _cell_volume 1494.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 33.5 _cell_measurement_theta_max 39.8 _exptl_crystal_description needle _exptl_crystal_colour purple _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.748 _exptl_crystal_density_meas ? _chemical_formula_analytical ? _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 792.00 _exptl_absorpt_coefficient_mu 9.815 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details 'North,Phillips & Matthews, 1968' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.748 _exptl_special_details ; The scan width was (0.94+0.30tan\q)\% with an \w scan speed of 16\% per minute (up to 4 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC5R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.69 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 -4 0 0 -1 5 2 -1 0 _diffrn_reflns_number 3158 _diffrn_reflns_av_R_equivalents 0.0713 _diffrn_reflns_av_sigmaI/netI 0.0425 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 4.95 _diffrn_reflns_theta_max 78.01 _reflns_number_total 2989 _reflns_number_gt 2411 _reflns_threshold_expression >2sigma(I) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1995)' _computing_structure_solution ; 'DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan (MSC, 1995)' _computing_publication_material 'teXsan (MSC, 1995)' _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^)+(0.0660P)^2^+2.7950P] 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 2989 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0654 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1287 _refine_ls_wR_factor_gt 0.1176 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 0.23404(4) 0.12635(2) 1.05849(5) 0.03454(16) Uani 1 1 d . . . S1 S 0.39336(14) 0.13402(8) 0.85681(17) 0.0430(3) Uani 1 1 d . . . S2 S 0.15198(14) 0.01705(9) 0.89187(16) 0.0433(3) Uani 1 1 d . . . N1 N 0.0764(7) -0.1515(4) 0.5080(7) 0.076(2) Uani 1 1 d . . . C1 C 0.3540(5) 0.0586(3) 0.7232(6) 0.0423(12) Uani 1 1 d . . . H1 H 0.4048 0.0532 0.6369 0.051 Uiso 1 1 calc R . . C2 C 0.2559(5) 0.0075(3) 0.7343(6) 0.0401(12) Uani 1 1 d . . . C3 C 0.2285(6) -0.0598(3) 0.6225(6) 0.0430(13) Uani 1 1 d . . . C4 C 0.3213(7) -0.0999(4) 0.5408(7) 0.0539(16) Uani 1 1 d . . . H4 H 0.4038 -0.0829 0.5500 0.065 Uiso 1 1 calc R . . C5 C 0.2902(9) -0.1652(5) 0.4455(7) 0.070(2) Uani 1 1 d . . . H5 H 0.3517 -0.1933 0.3910 0.084 Uiso 1 1 calc R . . C6 C 0.1664(9) -0.1888(5) 0.4316(8) 0.075(2) Uani 1 1 d . . . H6 H 0.1462 -0.2325 0.3658 0.089 Uiso 1 1 calc R . . C7 C 0.1086(7) -0.0882(4) 0.6001(8) 0.0613(18) Uani 1 1 d . . . H7 H 0.0451 -0.0612 0.6531 0.074 Uiso 1 1 calc R . . C8 C 0.2225(7) 0.0233(4) 1.2403(7) 0.0543(16) Uani 1 1 d . . . H8 H 0.1556 -0.0178 1.2502 0.065 Uiso 1 1 calc R . . C9 C 0.2325(7) 0.0975(5) 1.3219(7) 0.0569(16) Uani 1 1 d . . . H9 H 0.1712 0.1186 1.3959 0.068 Uiso 1 1 calc R . . C10 C 0.3496(7) 0.1337(5) 1.2918(8) 0.0641(19) Uani 1 1 d . . . H10 H 0.3830 0.1843 1.3395 0.077 Uiso 1 1 calc R . . C11 C 0.4136(6) 0.0802(5) 1.1936(8) 0.0635(19) Uani 1 1 d . . . H11 H 0.4998 0.0875 1.1592 0.076 Uiso 1 1 calc R . . C12 C 0.3370(7) 0.0122(4) 1.1579(8) 0.0600(18) Uani 1 1 d . . . H12 H 0.3618 -0.0375 1.1002 0.072 Uiso 1 1 calc R . . C13 C 0.1069(7) 0.2047(4) 0.9011(8) 0.0573(17) Uani 1 1 d . . . H13 H 0.0875 0.1924 0.7929 0.069 Uiso 1 1 calc R . . C14 C 0.0369(6) 0.1774(4) 1.0308(10) 0.065(2) Uani 1 1 d . . . H14 H -0.0405 0.1450 1.0284 0.078 Uiso 1 1 calc R . . C15 C 0.0889(7) 0.2173(4) 1.1591(9) 0.065(2) Uani 1 1 d . . . H15 H 0.0557 0.2153 1.2643 0.078 Uiso 1 1 calc R . . C16 C 0.1883(7) 0.2674(4) 1.1108(9) 0.0579(17) Uani 1 1 d . . . H16 H 0.2374 0.3049 1.1761 0.070 Uiso 1 1 calc R . . C17 C 0.1969(7) 0.2600(4) 0.9522(7) 0.0528(15) Uani 1 1 d . . . H17 H 0.2546 0.2909 0.8861 0.063 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 0.0383(3) 0.0320(2) 0.0333(2) 0.00104(15) 0.00660(16) 0.00244(17) S1 0.0417(8) 0.0414(7) 0.0458(7) 0.0024(5) 0.0115(6) -0.0031(6) S2 0.0482(8) 0.0448(7) 0.0371(6) -0.0062(5) 0.0153(6) -0.0089(6) N1 0.092(5) 0.081(4) 0.055(4) -0.025(3) 0.022(3) -0.038(4) C1 0.046(3) 0.045(3) 0.036(3) 0.005(2) 0.012(2) 0.009(2) C2 0.048(3) 0.039(3) 0.033(3) 0.003(2) 0.009(2) 0.005(2) C3 0.067(4) 0.037(3) 0.025(2) 0.002(2) 0.008(2) 0.003(3) C4 0.063(4) 0.063(4) 0.036(3) -0.004(3) 0.008(3) 0.013(3) C5 0.108(7) 0.067(5) 0.036(3) -0.014(3) 0.009(4) 0.018(4) C6 0.119(7) 0.060(4) 0.045(4) -0.014(3) 0.019(4) -0.025(4) C7 0.072(5) 0.062(4) 0.050(4) -0.016(3) 0.018(3) -0.016(3) C8 0.067(4) 0.055(4) 0.041(3) 0.020(3) 0.006(3) 0.001(3) C9 0.066(4) 0.074(4) 0.031(3) 0.004(3) 0.006(3) 0.007(3) C10 0.067(5) 0.080(5) 0.045(4) -0.003(3) -0.013(3) -0.001(4) C11 0.047(4) 0.096(6) 0.048(4) 0.013(4) -0.004(3) 0.015(4) C12 0.076(5) 0.056(4) 0.047(3) 0.011(3) -0.004(3) 0.024(4) C13 0.066(4) 0.049(3) 0.057(4) 0.009(3) -0.016(3) 0.016(3) C14 0.031(3) 0.045(3) 0.119(7) 0.015(4) 0.007(4) 0.010(3) C15 0.084(5) 0.045(3) 0.067(4) -0.001(3) 0.037(4) 0.020(3) C16 0.065(4) 0.041(3) 0.068(4) -0.010(3) 0.013(3) 0.004(3) C17 0.070(4) 0.036(3) 0.053(4) 0.011(2) 0.014(3) 0.006(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 C14 2.282(6) . ? Mo1 C8 2.290(6) . ? Mo1 C13 2.301(6) . ? Mo1 C12 2.308(6) . ? Mo1 C15 2.309(6) . ? Mo1 C9 2.328(6) . ? Mo1 C16 2.365(6) . ? Mo1 C11 2.370(6) . ? Mo1 C17 2.371(6) . ? Mo1 C10 2.371(7) . ? Mo1 S2 2.4375(15) . ? Mo1 S1 2.4506(15) . ? S1 C1 1.728(6) . ? S2 C2 1.771(5) . ? N1 C6 1.316(10) . ? N1 C7 1.339(8) . ? C1 C2 1.339(8) . ? C1 H1 0.9300 . ? C2 C3 1.481(8) . ? C3 C7 1.379(9) . ? C3 C4 1.383(8) . ? C4 C5 1.376(10) . ? C4 H4 0.9300 . ? C5 C6 1.387(11) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.391(10) . ? C8 C12 1.434(10) . ? C8 H8 0.9800 . ? C9 C10 1.410(11) . ? C9 H9 0.9800 . ? C10 C11 1.392(10) . ? C10 H10 0.9800 . ? C11 C12 1.401(11) . ? C11 H11 0.9800 . ? C12 H12 0.9800 . ? C13 C17 1.385(10) . ? C13 C14 1.422(10) . ? C13 H13 0.9800 . ? C14 C15 1.399(11) . ? C14 H14 0.9800 . ? C15 C16 1.401(10) . ? C15 H15 0.9800 . ? C16 C17 1.382(10) . ? C16 H16 0.9800 . ? C17 H17 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C14 Mo1 C8 106.3(3) . . ? C14 Mo1 C13 36.2(3) . . ? C8 Mo1 C13 140.4(3) . . ? C14 Mo1 C12 140.2(3) . . ? C8 Mo1 C12 36.3(2) . . ? C13 Mo1 C12 159.9(3) . . ? C14 Mo1 C15 35.5(3) . . ? C8 Mo1 C15 99.3(2) . . ? C13 Mo1 C15 58.5(3) . . ? C12 Mo1 C15 133.3(3) . . ? C14 Mo1 C9 99.5(3) . . ? C8 Mo1 C9 35.1(2) . . ? C13 Mo1 C9 133.1(3) . . ? C12 Mo1 C9 58.7(2) . . ? C15 Mo1 C9 75.5(3) . . ? C14 Mo1 C16 58.8(3) . . ? C8 Mo1 C16 123.5(3) . . ? C13 Mo1 C16 57.7(3) . . ? C12 Mo1 C16 142.3(3) . . ? C15 Mo1 C16 34.9(2) . . ? C9 Mo1 C16 90.1(3) . . ? C14 Mo1 C11 156.5(3) . . ? C8 Mo1 C11 58.6(3) . . ? C13 Mo1 C11 160.6(3) . . ? C12 Mo1 C11 34.8(3) . . ? C15 Mo1 C11 124.1(3) . . ? C9 Mo1 C11 57.5(2) . . ? C16 Mo1 C11 112.0(3) . . ? C14 Mo1 C17 58.6(2) . . ? C8 Mo1 C17 156.0(2) . . ? C13 Mo1 C17 34.4(2) . . ? C12 Mo1 C17 161.0(3) . . ? C15 Mo1 C17 57.3(2) . . ? C9 Mo1 C17 124.0(2) . . ? C16 Mo1 C17 33.9(2) . . ? C11 Mo1 C17 127.6(3) . . ? C14 Mo1 C10 123.7(3) . . ? C8 Mo1 C10 58.6(3) . . ? C13 Mo1 C10 141.8(3) . . ? C12 Mo1 C10 58.2(3) . . ? C15 Mo1 C10 89.9(3) . . ? C9 Mo1 C10 34.9(3) . . ? C16 Mo1 C10 84.1(3) . . ? C11 Mo1 C10 34.2(3) . . ? C17 Mo1 C10 111.9(3) . . ? C14 Mo1 S2 82.2(2) . . ? C8 Mo1 S2 82.22(18) . . ? C13 Mo1 S2 80.30(18) . . ? C12 Mo1 S2 79.6(2) . . ? C15 Mo1 S2 115.9(2) . . ? C9 Mo1 S2 115.64(19) . . ? C16 Mo1 S2 136.91(19) . . ? C11 Mo1 S2 111.0(2) . . ? C17 Mo1 S2 111.33(17) . . ? C10 Mo1 S2 136.69(19) . . ? C14 Mo1 S1 123.8(2) . . ? C8 Mo1 S1 124.43(18) . . ? C13 Mo1 S1 87.9(2) . . ? C12 Mo1 S1 88.37(19) . . ? C15 Mo1 S1 135.19(18) . . ? C9 Mo1 S1 135.67(18) . . ? C16 Mo1 S1 103.52(17) . . ? C11 Mo1 S1 78.44(18) . . ? C17 Mo1 S1 78.15(16) . . ? C10 Mo1 S1 103.9(2) . . ? S2 Mo1 S1 82.30(5) . . ? C1 S1 Mo1 105.80(19) . . ? C2 S2 Mo1 106.9(2) . . ? C6 N1 C7 117.2(7) . . ? C2 C1 S1 125.0(4) . . ? C2 C1 H1 117.5 . . ? S1 C1 H1 117.5 . . ? C1 C2 C3 123.8(5) . . ? C1 C2 S2 119.9(4) . . ? C3 C2 S2 116.3(4) . . ? C7 C3 C4 116.6(6) . . ? C7 C3 C2 121.1(5) . . ? C4 C3 C2 122.2(6) . . ? C5 C4 C3 119.3(7) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C4 C5 C6 119.5(7) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? N1 C6 C5 122.4(7) . . ? N1 C6 H6 118.8 . . ? C5 C6 H6 118.8 . . ? N1 C7 C3 125.1(7) . . ? N1 C7 H7 117.5 . . ? C3 C7 H7 117.5 . . ? C9 C8 C12 107.1(6) . . ? C9 C8 Mo1 74.0(4) . . ? C12 C8 Mo1 72.5(3) . . ? C9 C8 H8 126.1 . . ? C12 C8 H8 126.1 . . ? Mo1 C8 H8 126.1 . . ? C8 C9 C10 109.1(6) . . ? C8 C9 Mo1 71.0(3) . . ? C10 C9 Mo1 74.2(4) . . ? C8 C9 H9 125.3 . . ? C10 C9 H9 125.3 . . ? Mo1 C9 H9 125.3 . . ? C11 C10 C9 107.4(7) . . ? C11 C10 Mo1 72.9(4) . . ? C9 C10 Mo1 70.9(4) . . ? C11 C10 H10 126.2 . . ? C9 C10 H10 126.2 . . ? Mo1 C10 H10 126.2 . . ? C10 C11 C12 109.1(7) . . ? C10 C11 Mo1 72.9(4) . . ? C12 C11 Mo1 70.1(4) . . ? C10 C11 H11 125.4 . . ? C12 C11 H11 125.4 . . ? Mo1 C11 H11 125.4 . . ? C11 C12 C8 107.3(6) . . ? C11 C12 Mo1 75.0(4) . . ? C8 C12 Mo1 71.1(3) . . ? C11 C12 H12 126.1 . . ? C8 C12 H12 126.1 . . ? Mo1 C12 H12 126.1 . . ? C17 C13 C14 108.4(6) . . ? C17 C13 Mo1 75.6(4) . . ? C14 C13 Mo1 71.2(3) . . ? C17 C13 H13 125.5 . . ? C14 C13 H13 125.5 . . ? Mo1 C13 H13 125.5 . . ? C15 C14 C13 105.9(6) . . ? C15 C14 Mo1 73.3(4) . . ? C13 C14 Mo1 72.7(4) . . ? C15 C14 H14 126.7 . . ? C13 C14 H14 126.7 . . ? Mo1 C14 H14 126.7 . . ? C16 C15 C14 109.2(6) . . ? C16 C15 Mo1 74.7(4) . . ? C14 C15 Mo1 71.2(3) . . ? C16 C15 H15 125.2 . . ? C14 C15 H15 125.2 . . ? Mo1 C15 H15 125.2 . . ? C17 C16 C15 107.5(7) . . ? C17 C16 Mo1 73.3(3) . . ? C15 C16 Mo1 70.4(3) . . ? C17 C16 H16 126.1 . . ? C15 C16 H16 126.1 . . ? Mo1 C16 H16 126.1 . . ? C16 C17 C13 108.9(6) . . ? C16 C17 Mo1 72.8(3) . . ? C13 C17 Mo1 70.0(3) . . ? C16 C17 H17 125.5 . . ? C13 C17 H17 125.5 . . ? Mo1 C17 H17 125.5 . . ? 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 C14 Mo1 S1 C1 -75.9(3) . . . . ? C8 Mo1 S1 C1 74.3(3) . . . . ? C13 Mo1 S1 C1 -81.2(3) . . . . ? C12 Mo1 S1 C1 79.0(3) . . . . ? C15 Mo1 S1 C1 -120.1(4) . . . . ? C9 Mo1 S1 C1 118.3(3) . . . . ? C16 Mo1 S1 C1 -137.3(3) . . . . ? C11 Mo1 S1 C1 112.6(3) . . . . ? C17 Mo1 S1 C1 -114.6(3) . . . . ? C10 Mo1 S1 C1 135.5(3) . . . . ? S2 Mo1 S1 C1 -0.8(2) . . . . ? C14 Mo1 S2 C2 127.4(3) . . . . ? C8 Mo1 S2 C2 -124.8(3) . . . . ? C13 Mo1 S2 C2 90.8(3) . . . . ? C12 Mo1 S2 C2 -88.1(3) . . . . ? C15 Mo1 S2 C2 138.5(3) . . . . ? C9 Mo1 S2 C2 -135.8(3) . . . . ? C16 Mo1 S2 C2 103.2(3) . . . . ? C11 Mo1 S2 C2 -72.8(3) . . . . ? C17 Mo1 S2 C2 75.6(3) . . . . ? C10 Mo1 S2 C2 -100.5(3) . . . . ? S1 Mo1 S2 C2 1.62(19) . . . . ? Mo1 S1 C1 C2 -0.6(6) . . . . ? S1 C1 C2 C3 -176.3(4) . . . . ? S1 C1 C2 S2 2.3(7) . . . . ? Mo1 S2 C2 C1 -2.7(5) . . . . ? Mo1 S2 C2 C3 176.1(4) . . . . ? C1 C2 C3 C7 -153.9(6) . . . . ? S2 C2 C3 C7 27.4(7) . . . . ? C1 C2 C3 C4 29.1(8) . . . . ? S2 C2 C3 C4 -149.6(5) . . . . ? C7 C3 C4 C5 -1.0(9) . . . . ? C2 C3 C4 C5 176.2(6) . . . . ? C3 C4 C5 C6 0.9(11) . . . . ? C7 N1 C6 C5 0.8(12) . . . . ? C4 C5 C6 N1 -0.9(12) . . . . ? C6 N1 C7 C3 -0.9(12) . . . . ? C4 C3 C7 N1 1.0(11) . . . . ? C2 C3 C7 N1 -176.2(7) . . . . ? C14 Mo1 C8 C9 -83.3(5) . . . . ? C13 Mo1 C8 C9 -98.3(5) . . . . ? C12 Mo1 C8 C9 114.3(6) . . . . ? C15 Mo1 C8 C9 -47.6(5) . . . . ? C16 Mo1 C8 C9 -20.2(5) . . . . ? C11 Mo1 C8 C9 76.8(5) . . . . ? C17 Mo1 C8 C9 -36.1(8) . . . . ? C10 Mo1 C8 C9 36.6(4) . . . . ? S2 Mo1 C8 C9 -162.7(4) . . . . ? S1 Mo1 C8 C9 122.2(4) . . . . ? C14 Mo1 C8 C12 162.4(4) . . . . ? C13 Mo1 C8 C12 147.4(4) . . . . ? C15 Mo1 C8 C12 -161.9(5) . . . . ? C9 Mo1 C8 C12 -114.3(6) . . . . ? C16 Mo1 C8 C12 -134.5(4) . . . . ? C11 Mo1 C8 C12 -37.5(4) . . . . ? C17 Mo1 C8 C12 -150.4(6) . . . . ? C10 Mo1 C8 C12 -77.7(5) . . . . ? S2 Mo1 C8 C12 83.0(4) . . . . ? S1 Mo1 C8 C12 7.9(5) . . . . ? C12 C8 C9 C10 0.6(7) . . . . ? Mo1 C8 C9 C10 -64.9(5) . . . . ? C12 C8 C9 Mo1 65.5(4) . . . . ? C14 Mo1 C9 C8 104.9(4) . . . . ? C13 Mo1 C9 C8 120.2(5) . . . . ? C12 Mo1 C9 C8 -39.2(4) . . . . ? C15 Mo1 C9 C8 131.2(5) . . . . ? C16 Mo1 C9 C8 163.2(4) . . . . ? C11 Mo1 C9 C8 -80.5(5) . . . . ? C17 Mo1 C9 C8 163.2(4) . . . . ? C10 Mo1 C9 C8 -117.2(6) . . . . ? S2 Mo1 C9 C8 19.1(5) . . . . ? S1 Mo1 C9 C8 -87.1(5) . . . . ? C14 Mo1 C9 C10 -137.9(4) . . . . ? C8 Mo1 C9 C10 117.2(6) . . . . ? C13 Mo1 C9 C10 -122.6(5) . . . . ? C12 Mo1 C9 C10 78.0(5) . . . . ? C15 Mo1 C9 C10 -111.6(5) . . . . ? C16 Mo1 C9 C10 -79.6(5) . . . . ? C11 Mo1 C9 C10 36.8(4) . . . . ? C17 Mo1 C9 C10 -79.6(5) . . . . ? S2 Mo1 C9 C10 136.3(4) . . . . ? S1 Mo1 C9 C10 30.1(5) . . . . ? C8 C9 C10 C11 -1.4(8) . . . . ? Mo1 C9 C10 C11 -64.2(5) . . . . ? C8 C9 C10 Mo1 62.8(5) . . . . ? C14 Mo1 C10 C11 168.6(4) . . . . ? C8 Mo1 C10 C11 79.2(5) . . . . ? C13 Mo1 C10 C11 -147.6(5) . . . . ? C12 Mo1 C10 C11 36.3(5) . . . . ? C15 Mo1 C10 C11 -179.8(5) . . . . ? C9 Mo1 C10 C11 116.0(7) . . . . ? C16 Mo1 C10 C11 -145.4(5) . . . . ? C17 Mo1 C10 C11 -125.5(5) . . . . ? S2 Mo1 C10 C11 50.7(6) . . . . ? S1 Mo1 C10 C11 -42.9(5) . . . . ? C14 Mo1 C10 C9 52.6(5) . . . . ? C8 Mo1 C10 C9 -36.8(4) . . . . ? C13 Mo1 C10 C9 96.4(6) . . . . ? C12 Mo1 C10 C9 -79.7(5) . . . . ? C15 Mo1 C10 C9 64.2(5) . . . . ? C16 Mo1 C10 C9 98.7(5) . . . . ? C11 Mo1 C10 C9 -116.0(7) . . . . ? C17 Mo1 C10 C9 118.5(4) . . . . ? S2 Mo1 C10 C9 -65.3(5) . . . . ? S1 Mo1 C10 C9 -158.8(4) . . . . ? C9 C10 C11 C12 1.7(8) . . . . ? Mo1 C10 C11 C12 -61.2(5) . . . . ? C9 C10 C11 Mo1 62.9(5) . . . . ? C14 Mo1 C11 C10 -24.3(10) . . . . ? C8 Mo1 C11 C10 -79.2(5) . . . . ? C13 Mo1 C11 C10 91.5(9) . . . . ? C12 Mo1 C11 C10 -118.3(7) . . . . ? C15 Mo1 C11 C10 0.2(6) . . . . ? C9 Mo1 C11 C10 -37.6(5) . . . . ? C16 Mo1 C11 C10 37.6(5) . . . . ? C17 Mo1 C11 C10 72.6(5) . . . . ? S2 Mo1 C11 C10 -145.4(4) . . . . ? S1 Mo1 C11 C10 137.6(5) . . . . ? C14 Mo1 C11 C12 94.0(8) . . . . ? C8 Mo1 C11 C12 39.1(4) . . . . ? C13 Mo1 C11 C12 -150.2(7) . . . . ? C15 Mo1 C11 C12 118.5(4) . . . . ? C9 Mo1 C11 C12 80.7(5) . . . . ? C16 Mo1 C11 C12 155.9(4) . . . . ? C17 Mo1 C11 C12 -169.1(4) . . . . ? C10 Mo1 C11 C12 118.3(7) . . . . ? S2 Mo1 C11 C12 -27.1(4) . . . . ? S1 Mo1 C11 C12 -104.1(4) . . . . ? C10 C11 C12 C8 -1.4(7) . . . . ? Mo1 C11 C12 C8 -64.3(4) . . . . ? C10 C11 C12 Mo1 63.0(5) . . . . ? C9 C8 C12 C11 0.5(7) . . . . ? Mo1 C8 C12 C11 66.9(4) . . . . ? C9 C8 C12 Mo1 -66.4(4) . . . . ? C14 Mo1 C12 C11 -141.5(5) . . . . ? C8 Mo1 C12 C11 -114.6(6) . . . . ? C13 Mo1 C12 C11 151.4(7) . . . . ? C15 Mo1 C12 C11 -89.6(5) . . . . ? C9 Mo1 C12 C11 -76.8(5) . . . . ? C16 Mo1 C12 C11 -38.3(6) . . . . ? C17 Mo1 C12 C11 27.4(9) . . . . ? C10 Mo1 C12 C11 -35.6(4) . . . . ? S2 Mo1 C12 C11 154.4(4) . . . . ? S1 Mo1 C12 C11 71.9(4) . . . . ? C14 Mo1 C12 C8 -26.9(7) . . . . ? C13 Mo1 C12 C8 -94.0(8) . . . . ? C15 Mo1 C12 C8 25.0(6) . . . . ? C9 Mo1 C12 C8 37.8(4) . . . . ? C16 Mo1 C12 C8 76.3(6) . . . . ? C11 Mo1 C12 C8 114.6(6) . . . . ? C17 Mo1 C12 C8 142.0(7) . . . . ? C10 Mo1 C12 C8 79.0(5) . . . . ? S2 Mo1 C12 C8 -91.0(4) . . . . ? S1 Mo1 C12 C8 -173.5(4) . . . . ? C14 Mo1 C13 C17 115.6(6) . . . . ? C8 Mo1 C13 C17 140.5(4) . . . . ? C12 Mo1 C13 C17 -151.5(7) . . . . ? C15 Mo1 C13 C17 76.9(4) . . . . ? C9 Mo1 C13 C17 89.4(5) . . . . ? C16 Mo1 C13 C17 35.5(4) . . . . ? C11 Mo1 C13 C17 -26.9(10) . . . . ? C10 Mo1 C13 C17 38.2(7) . . . . ? S2 Mo1 C13 C17 -154.4(4) . . . . ? S1 Mo1 C13 C17 -71.9(4) . . . . ? C8 Mo1 C13 C14 24.9(6) . . . . ? C12 Mo1 C13 C14 92.9(9) . . . . ? C15 Mo1 C13 C14 -38.7(4) . . . . ? C9 Mo1 C13 C14 -26.2(6) . . . . ? C16 Mo1 C13 C14 -80.1(5) . . . . ? C11 Mo1 C13 C14 -142.5(8) . . . . ? C17 Mo1 C13 C14 -115.6(6) . . . . ? C10 Mo1 C13 C14 -77.4(6) . . . . ? S2 Mo1 C13 C14 90.0(4) . . . . ? S1 Mo1 C13 C14 172.5(4) . . . . ? C17 C13 C14 C15 -0.7(7) . . . . ? Mo1 C13 C14 C15 66.3(4) . . . . ? C17 C13 C14 Mo1 -67.0(4) . . . . ? C8 Mo1 C14 C15 83.1(4) . . . . ? C13 Mo1 C14 C15 -113.2(6) . . . . ? C12 Mo1 C14 C15 99.3(5) . . . . ? C9 Mo1 C14 C15 47.7(5) . . . . ? C16 Mo1 C14 C15 -36.5(4) . . . . ? C11 Mo1 C14 C15 36.4(9) . . . . ? C17 Mo1 C14 C15 -76.5(4) . . . . ? C10 Mo1 C14 C15 20.3(5) . . . . ? S2 Mo1 C14 C15 162.6(4) . . . . ? S1 Mo1 C14 C15 -122.2(4) . . . . ? C8 Mo1 C14 C13 -163.7(4) . . . . ? C12 Mo1 C14 C13 -147.5(4) . . . . ? C15 Mo1 C14 C13 113.2(6) . . . . ? C9 Mo1 C14 C13 160.9(4) . . . . ? C16 Mo1 C14 C13 76.6(4) . . . . ? C11 Mo1 C14 C13 149.6(6) . . . . ? C17 Mo1 C14 C13 36.7(4) . . . . ? C10 Mo1 C14 C13 133.5(4) . . . . ? S2 Mo1 C14 C13 -84.3(4) . . . . ? S1 Mo1 C14 C13 -9.0(5) . . . . ? C13 C14 C15 C16 -0.3(7) . . . . ? Mo1 C14 C15 C16 65.6(5) . . . . ? C13 C14 C15 Mo1 -65.9(4) . . . . ? C14 Mo1 C15 C16 -117.0(6) . . . . ? C8 Mo1 C15 C16 137.9(5) . . . . ? C13 Mo1 C15 C16 -77.5(5) . . . . ? C12 Mo1 C15 C16 123.2(5) . . . . ? C9 Mo1 C15 C16 111.9(5) . . . . ? C11 Mo1 C15 C16 79.7(5) . . . . ? C17 Mo1 C15 C16 -36.6(4) . . . . ? C10 Mo1 C15 C16 79.8(5) . . . . ? S2 Mo1 C15 C16 -136.3(4) . . . . ? S1 Mo1 C15 C16 -30.1(6) . . . . ? C8 Mo1 C15 C14 -105.1(4) . . . . ? C13 Mo1 C15 C14 39.5(4) . . . . ? C12 Mo1 C15 C14 -119.8(5) . . . . ? C9 Mo1 C15 C14 -131.1(5) . . . . ? C16 Mo1 C15 C14 117.0(6) . . . . ? C11 Mo1 C15 C14 -163.4(4) . . . . ? C17 Mo1 C15 C14 80.4(5) . . . . ? C10 Mo1 C15 C14 -163.2(4) . . . . ? S2 Mo1 C15 C14 -19.3(5) . . . . ? S1 Mo1 C15 C14 86.9(5) . . . . ? C14 C15 C16 C17 1.1(8) . . . . ? Mo1 C15 C16 C17 64.4(5) . . . . ? C14 C15 C16 Mo1 -63.3(4) . . . . ? C14 Mo1 C16 C17 -78.9(5) . . . . ? C8 Mo1 C16 C17 -168.5(4) . . . . ? C13 Mo1 C16 C17 -36.1(4) . . . . ? C12 Mo1 C16 C17 147.8(5) . . . . ? C15 Mo1 C16 C17 -116.1(7) . . . . ? C9 Mo1 C16 C17 -180.0(5) . . . . ? C11 Mo1 C16 C17 125.4(4) . . . . ? C10 Mo1 C16 C17 145.5(5) . . . . ? S2 Mo1 C16 C17 -50.6(5) . . . . ? S1 Mo1 C16 C17 42.6(4) . . . . ? C14 Mo1 C16 C15 37.2(5) . . . . ? C8 Mo1 C16 C15 -52.4(6) . . . . ? C13 Mo1 C16 C15 80.0(5) . . . . ? C12 Mo1 C16 C15 -96.1(6) . . . . ? C9 Mo1 C16 C15 -63.9(5) . . . . ? C11 Mo1 C16 C15 -118.5(5) . . . . ? C17 Mo1 C16 C15 116.1(7) . . . . ? C10 Mo1 C16 C15 -98.4(5) . . . . ? S2 Mo1 C16 C15 65.5(5) . . . . ? S1 Mo1 C16 C15 158.7(4) . . . . ? C15 C16 C17 C13 -1.5(7) . . . . ? Mo1 C16 C17 C13 61.0(4) . . . . ? C15 C16 C17 Mo1 -62.5(5) . . . . ? C14 C13 C17 C16 1.4(7) . . . . ? Mo1 C13 C17 C16 -62.7(5) . . . . ? C14 C13 C17 Mo1 64.1(4) . . . . ? C14 Mo1 C17 C16 79.7(5) . . . . ? C8 Mo1 C17 C16 24.1(9) . . . . ? C13 Mo1 C17 C16 118.3(6) . . . . ? C12 Mo1 C17 C16 -92.0(8) . . . . ? C15 Mo1 C17 C16 37.6(4) . . . . ? C9 Mo1 C17 C16 0.0(6) . . . . ? C11 Mo1 C17 C16 -72.6(5) . . . . ? C10 Mo1 C17 C16 -37.3(5) . . . . ? S2 Mo1 C17 C16 145.5(4) . . . . ? S1 Mo1 C17 C16 -137.7(4) . . . . ? C14 Mo1 C17 C13 -38.6(5) . . . . ? C8 Mo1 C17 C13 -94.2(7) . . . . ? C12 Mo1 C17 C13 149.7(7) . . . . ? C15 Mo1 C17 C13 -80.7(5) . . . . ? C9 Mo1 C17 C13 -118.3(5) . . . . ? C16 Mo1 C17 C13 -118.3(6) . . . . ? C11 Mo1 C17 C13 169.1(4) . . . . ? C10 Mo1 C17 C13 -155.6(4) . . . . ? S2 Mo1 C17 C13 27.2(4) . . . . ? S1 Mo1 C17 C13 103.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.936 _diffrn_reflns_theta_full 67.5 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.86 _refine_diff_density_min -1.53 _refine_diff_density_rms 0.13 #=== END of CIF data_3a _database_code_depnum_ccdc_archive 'CCDC 822496' #TrackingRef '- combined.cif' #CPMOSN _audit_creation_method SHELXL97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H15 Mo N S2 +, B F4 - ' _chemical_formula_sum 'C17 H15 B F4 Mo N S2' _chemical_formula_weight 480.19 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' S S 0.1246 0.1234 '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 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.9390(10) _cell_length_b 14.514(2) _cell_length_c 17.696(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.018(3) _cell_angle_gamma 90.00 _cell_volume 1749.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3473 _cell_measurement_theta_min 2.74 _cell_measurement_theta_max 28.75 _exptl_crystal_description Plate _exptl_crystal_colour 'Dark red' _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.827 _exptl_crystal_density_method ? _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 1.029 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.666 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details 'SADABS (Bruker, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 11124 _diffrn_reflns_av_R_equivalents 0.059 _diffrn_reflns_av_sigmaI/netI 0.053 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4270 _reflns_number_gt 2717 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART version 5.054 (Bruker, 1998)' _computing_cell_refinement 'SAINT version 6.02B (Bruker, 2000)' _computing_data_reduction 'SAINT; SHELXTL (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL/PC version 5.03 (Sheldrick, 2008)' _computing_publication_material 'SHELXL97; PLATON (Spek, 2009)' _refine_special_details ; ; _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^)+(0.078P)^2^P] 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 3920 _refine_ls_number_parameters 246 _refine_ls_number_restraints 102 _refine_ls_R_factor_all 0.0732 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_ref 0.124 _refine_ls_wR_factor_gt 0.111 _refine_ls_goodness_of_fit_ref 0.96 _refine_ls_restrained_S_all 0.99 _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 Mo Mo 0.22915(5) 0.30560(2) 0.12366(2) 0.02552(14) Uani 1 1 d U . . S1 S 0.55624(17) 0.27103(8) 0.10470(8) 0.0356(3) Uani 1 1 d U A . S2 S 0.17400(17) 0.14856(8) 0.07800(8) 0.0338(3) Uani 1 1 d U A . C1 C 0.5656(7) 0.1548(3) 0.1054(3) 0.0343(11) Uani 1 1 d U A . H1A H 0.6912 0.1265 0.1123 0.041 Uiso 1 1 calc R . . C2 C 0.4046(6) 0.0987(3) 0.0965(3) 0.0289(9) Uani 1 1 d U . . C1C C 0.1400(8) 0.4537(3) 0.0793(3) 0.0441(12) Uani 1 1 d U A . H1CA H 0.1608 0.5112 0.1109 0.053 Uiso 1 1 calc R . . C2C C 0.2681(7) 0.4186(4) 0.0360(3) 0.0425(12) Uani 1 1 d U A . H2CA H 0.3952 0.4470 0.0294 0.051 Uiso 1 1 calc R . . C3C C 0.1765(9) 0.3415(4) -0.0040(3) 0.0442(12) Uani 1 1 d U A . H3CA H 0.2256 0.3061 -0.0450 0.053 Uiso 1 1 calc R . . C4C C -0.0095(8) 0.3321(4) 0.0163(3) 0.0469(13) Uani 1 1 d U A . H4CA H -0.1147 0.2879 -0.0071 0.056 Uiso 1 1 calc R . . C5C C -0.0285(8) 0.4012(4) 0.0667(3) 0.0478(13) Uani 1 1 d U A . H5CA H -0.1492 0.4143 0.0879 0.057 Uiso 1 1 calc R . . C6C C 0.242(2) 0.3897(7) 0.2366(5) 0.031(2) Uiso 0.50 1 d PU A 1 H6CA H 0.2472 0.4584 0.2405 0.037 Uiso 0.50 1 calc PR A 1 C7C C 0.4047(18) 0.3319(10) 0.2454(6) 0.035(3) Uiso 0.50 1 d PU A 1 H7CA H 0.5453 0.3514 0.2588 0.042 Uiso 0.50 1 calc PR A 1 C8C C 0.334(2) 0.2390(8) 0.2404(6) 0.031(2) Uiso 0.50 1 d PU A 1 H8CA H 0.4155 0.1819 0.2509 0.038 Uiso 0.50 1 calc PR A 1 C9C C 0.1236(19) 0.2442(8) 0.2285(6) 0.030(2) Uiso 0.50 1 d PU A 1 H9CA H 0.0321 0.1908 0.2276 0.035 Uiso 0.50 1 calc PR A 1 C10C C 0.0710(16) 0.3366(9) 0.2257(5) 0.028(2) Uiso 0.50 1 d PU A 1 H10A H -0.0656 0.3610 0.2210 0.034 Uiso 0.50 1 calc PR A 1 C6A C 0.149(2) 0.3710(10) 0.2326(6) 0.042(3) Uiso 0.50 1 d PU A 2 H6AA H 0.0745 0.4298 0.2337 0.051 Uiso 0.50 1 calc PR A 2 C7A C 0.354(2) 0.3639(9) 0.2449(6) 0.034(3) Uiso 0.50 1 d PU A 2 H7AA H 0.4504 0.4156 0.2573 0.041 Uiso 0.50 1 calc PR A 2 C8A C 0.3972(19) 0.2700(10) 0.2507(6) 0.039(3) Uiso 0.50 1 d PU A 2 H8AA H 0.5325 0.2436 0.2638 0.046 Uiso 0.50 1 calc PR A 2 C9A C 0.227(2) 0.2192(9) 0.2393(7) 0.045(3) Uiso 0.50 1 d PU A 2 H9AA H 0.2169 0.1507 0.2435 0.054 Uiso 0.50 1 calc PR A 2 C10A C 0.067(2) 0.2836(13) 0.2264(7) 0.051(3) Uiso 0.50 1 d PU A 2 H10B H -0.0751 0.2686 0.2224 0.061 Uiso 0.50 1 calc PR A 2 C1P C 0.4229(7) -0.0031(3) 0.0942(3) 0.0315(10) Uani 1 1 d U A . C6P C 0.6043(8) -0.0472(3) 0.1132(3) 0.0399(12) Uani 1 1 d U . . H6PA H 0.7213 -0.0123 0.1279 0.048 Uiso 1 1 calc R A . C5P C 0.6119(8) -0.1417(3) 0.1105(3) 0.0451(13) Uani 1 1 d U A . H5PA H 0.7342 -0.1728 0.1231 0.054 Uiso 1 1 calc R . . C4P C 0.4397(9) -0.1910(3) 0.0892(3) 0.0437(13) Uani 1 1 d U . . H4PA H 0.4468 -0.2564 0.0883 0.052 Uiso 1 1 calc R A . N3P N 0.2644(7) -0.1513(3) 0.0698(3) 0.0473(11) Uani 1 1 d U A . C2P C 0.2603(8) -0.0589(3) 0.0725(3) 0.0400(12) Uani 1 1 d U . . H2PA H 0.1361 -0.0297 0.0583 0.048 Uiso 1 1 calc R A . B B 0.6724(8) 0.5678(4) 0.1885(3) 0.0533(16) Uani 1 1 d DU . . F1 F 0.5734(13) 0.5486(5) 0.2441(4) 0.066(3) Uani 0.60 1 d PDU B 1 F2 F 0.7219(7) 0.6630(3) 0.1908(3) 0.0467(13) Uani 0.60 1 d PDU B 1 F3 F 0.5916(12) 0.5450(7) 0.1174(3) 0.121(4) Uani 0.60 1 d PDU B 1 F4 F 0.8680(10) 0.5310(5) 0.2064(4) 0.107(3) Uani 0.60 1 d PDU B 1 F1' F 0.5928(19) 0.5665(9) 0.2557(5) 0.067(5) Uiso 0.40 1 d PDU B 2 F2' F 0.8070(17) 0.6305(9) 0.1915(9) 0.156(8) Uiso 0.40 1 d PDU B 2 F3' F 0.5093(12) 0.5839(6) 0.1275(5) 0.062(3) Uiso 0.40 1 d PDU B 2 F4' F 0.7241(17) 0.4775(6) 0.1769(7) 0.101(4) Uiso 0.40 1 d PDU B 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 Mo 0.0204(2) 0.0210(2) 0.0365(2) 0.00267(16) 0.00876(15) -0.00021(15) S1 0.0233(6) 0.0304(6) 0.0560(8) 0.0036(5) 0.0148(5) -0.0001(5) S2 0.0261(6) 0.0222(5) 0.0522(8) 0.0000(5) 0.0052(5) 0.0015(4) C2 0.029(2) 0.026(2) 0.033(2) 0.0047(19) 0.0085(19) 0.0084(17) C1 0.024(2) 0.034(2) 0.047(3) 0.001(2) 0.011(2) 0.0039(19) C1C 0.065(3) 0.023(2) 0.043(3) 0.0050(19) 0.005(3) 0.011(2) C2C 0.035(3) 0.040(3) 0.053(3) 0.022(2) 0.009(2) -0.002(2) C3C 0.060(3) 0.039(3) 0.035(3) 0.005(2) 0.011(2) 0.017(2) C4C 0.039(3) 0.033(2) 0.060(3) 0.018(2) -0.012(2) -0.005(2) C5C 0.039(3) 0.045(3) 0.063(4) 0.024(2) 0.017(2) 0.020(2) C1P 0.039(3) 0.027(2) 0.029(2) -0.0006(19) 0.008(2) 0.0048(18) C6P 0.046(3) 0.033(2) 0.040(3) -0.004(2) 0.005(2) 0.009(2) C5P 0.056(3) 0.032(3) 0.044(3) -0.005(2) 0.002(3) 0.018(2) C4P 0.065(3) 0.025(2) 0.038(3) -0.007(2) 0.001(3) 0.011(2) N3P 0.061(3) 0.024(2) 0.052(3) -0.002(2) -0.001(2) 0.004(2) C2P 0.041(3) 0.027(2) 0.050(3) 0.000(2) 0.003(2) 0.004(2) B 0.076(5) 0.034(3) 0.056(4) 0.000(3) 0.029(3) 0.005(3) F1 0.121(7) 0.034(3) 0.058(4) -0.005(3) 0.051(4) -0.012(4) F2 0.034(3) 0.031(2) 0.079(4) -0.001(2) 0.023(3) -0.004(2) F3 0.131(6) 0.183(10) 0.062(4) -0.066(5) 0.055(4) -0.104(7) F4 0.124(6) 0.104(6) 0.110(6) 0.017(5) 0.064(5) 0.084(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo C8C 2.271(10) . ? Mo C3C 2.278(5) . ? Mo C7C 2.295(11) . ? Mo C9C 2.301(10) . ? Mo C4C 2.302(5) . ? Mo C2C 2.308(5) . ? Mo C6A 2.310(11) . ? Mo C7A 2.316(11) . ? Mo C6C 2.329(10) . ? Mo C10C 2.329(9) . ? Mo C1C 2.332(5) . ? Mo C5C 2.334(5) . ? Mo C10A 2.335(13) . ? Mo C8A 2.383(11) . ? Mo C9A 2.402(12) . ? Mo S1 2.4097(12) . ? Mo S2 2.4240(12) . ? S1 C1 1.688(5) . ? S2 C2 1.730(4) . ? C1 C2 1.367(7) . ? C2 C1P 1.483(6) . ? C1C C2C 1.377(7) . ? C1C C5C 1.378(8) . ? C2C C3C 1.410(8) . ? C3C C4C 1.411(8) . ? C4C C5C 1.365(8) . ? C6C C7C 1.391(15) . ? C6C C10C 1.398(14) . ? C7C C8C 1.432(16) . ? C8C C9C 1.437(16) . ? C9C C10C 1.389(15) . ? C6A C10A 1.386(19) . ? C6A C7A 1.402(17) . ? C7A C8A 1.394(17) . ? C8A C9A 1.373(17) . ? C9A C10A 1.437(19) . ? C1P C2P 1.383(7) . ? C1P C6P 1.395(7) . ? C6P C5P 1.374(7) . ? C5P C4P 1.382(8) . ? C4P N3P 1.330(7) . ? N3P C2P 1.341(6) . ? B F2' 1.298(7) . ? B F3 1.318(6) . ? B F1 1.332(6) . ? B F4' 1.384(7) . ? B F1' 1.403(8) . ? B F2 1.423(6) . ? B F3' 1.427(7) . ? B F4 1.436(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 C8C Mo C3C 164.1(3) . . ? C8C Mo C7C 36.6(4) . . ? C3C Mo C7C 148.0(3) . . ? C8C Mo C9C 36.6(4) . . ? C3C Mo C9C 150.8(3) . . ? C7C Mo C9C 60.1(4) . . ? C8C Mo C4C 151.3(4) . . ? C3C Mo C4C 35.9(2) . . ? C7C Mo C4C 156.4(4) . . ? C9C Mo C4C 116.2(3) . . ? C8C Mo C2C 148.8(4) . . ? C3C Mo C2C 35.80(19) . . ? C7C Mo C2C 113.8(4) . . ? C9C Mo C2C 155.9(4) . . ? C4C Mo C2C 59.00(19) . . ? C8C Mo C6A 60.1(4) . . ? C3C Mo C6A 135.7(3) . . ? C7C Mo C6A 46.9(4) . . ? C9C Mo C6A 47.3(4) . . ? C4C Mo C6A 111.8(4) . . ? C2C Mo C6A 110.2(4) . . ? C8C Mo C7A 46.7(4) . . ? C3C Mo C7A 142.7(3) . . ? C7C Mo C7A 14.5(3) . . ? C9C Mo C7A 61.0(4) . . ? C4C Mo C7A 141.9(4) . . ? C2C Mo C7A 106.9(3) . . ? C6A Mo C7A 35.3(4) . . ? C8C Mo C6C 59.3(4) . . ? C3C Mo C6C 134.7(3) . . ? C7C Mo C6C 35.0(4) . . ? C9C Mo C6C 58.5(4) . . ? C4C Mo C6C 121.6(4) . . ? C2C Mo C6C 102.3(3) . . ? C6A Mo C6C 17.1(3) . . ? C7A Mo C6C 21.1(3) . . ? C8C Mo C10C 59.6(4) . . ? C3C Mo C10C 135.6(3) . . ? C7C Mo C10C 59.0(4) . . ? C9C Mo C10C 34.9(4) . . ? C4C Mo C10C 103.7(3) . . ? C2C Mo C10C 121.1(3) . . ? C6A Mo C10C 18.1(3) . . ? C7A Mo C10C 50.2(4) . . ? C6C Mo C10C 34.9(4) . . ? C8C Mo C1C 135.8(3) . . ? C3C Mo C1C 58.25(19) . . ? C7C Mo C1C 102.8(4) . . ? C9C Mo C1C 121.6(4) . . ? C4C Mo C1C 57.68(19) . . ? C2C Mo C1C 34.52(18) . . ? C6A Mo C1C 79.1(3) . . ? C7A Mo C1C 90.2(4) . . ? C6C Mo C1C 76.7(3) . . ? C10C Mo C1C 87.0(3) . . ? C8C Mo C5C 137.0(3) . . ? C3C Mo C5C 58.1(2) . . ? C7C Mo C5C 122.1(4) . . ? C9C Mo C5C 104.1(4) . . ? C4C Mo C5C 34.2(2) . . ? C2C Mo C5C 57.72(18) . . ? C6A Mo C5C 80.2(3) . . ? C7A Mo C5C 107.7(4) . . ? C6C Mo C5C 87.7(3) . . ? C10C Mo C5C 77.5(3) . . ? C1C Mo C5C 34.36(19) . . ? C8C Mo C10A 49.6(5) . . ? C3C Mo C10A 142.5(4) . . ? C7C Mo C10A 62.6(4) . . ? C9C Mo C10A 17.1(4) . . ? C4C Mo C10A 106.7(4) . . ? C2C Mo C10A 139.1(5) . . ? C6A Mo C10A 34.7(5) . . ? C7A Mo C10A 58.7(4) . . ? C6C Mo C10A 49.4(4) . . ? C10C Mo C10A 19.0(4) . . ? C1C Mo C10A 104.6(5) . . ? C5C Mo C10A 88.5(5) . . ? C8C Mo C8A 15.3(3) . . ? C3C Mo C8A 160.3(3) . . ? C7C Mo C8A 22.2(4) . . ? C9C Mo C8A 47.8(4) . . ? C4C Mo C8A 163.8(3) . . ? C2C Mo C8A 133.5(4) . . ? C6A Mo C8A 56.9(4) . . ? C7A Mo C8A 34.5(4) . . ? C6C Mo C8A 51.1(4) . . ? C10C Mo C8A 61.9(4) . . ? C1C Mo C8A 124.6(4) . . ? C5C Mo C8A 137.1(3) . . ? C10A Mo C8A 57.2(5) . . ? C8C Mo C9A 19.2(3) . . ? C3C Mo C9A 159.7(3) . . ? C7C Mo C9A 51.4(4) . . ? C9C Mo C9A 19.3(3) . . ? C4C Mo C9A 132.1(4) . . ? C2C Mo C9A 164.5(3) . . ? C6A Mo C9A 57.5(4) . . ? C7A Mo C9A 57.6(4) . . ? C6C Mo C9A 63.2(4) . . ? C10C Mo C9A 50.2(4) . . ? C1C Mo C9A 136.4(3) . . ? C5C Mo C9A 123.3(4) . . ? C10A Mo C9A 35.3(5) . . ? C8A Mo C9A 33.4(4) . . ? C8C Mo S1 83.8(3) . . ? C3C Mo S1 83.47(15) . . ? C7C Mo S1 79.6(3) . . ? C9C Mo S1 119.0(4) . . ? C4C Mo S1 117.90(17) . . ? C2C Mo S1 79.64(13) . . ? C6A Mo S1 125.8(4) . . ? C7A Mo S1 90.5(4) . . ? C6C Mo S1 110.2(4) . . ? C10C Mo S1 138.1(3) . . ? C1C Mo S1 109.98(15) . . ? C5C Mo S1 136.70(14) . . ? C10A Mo S1 133.4(4) . . ? C8A Mo S1 77.4(3) . . ? C9A Mo S1 99.7(4) . . ? C8C Mo S2 84.6(3) . . ? C3C Mo S2 84.21(15) . . ? C7C Mo S2 119.4(4) . . ? C9C Mo S2 81.4(3) . . ? C4C Mo S2 80.74(14) . . ? C2C Mo S2 118.41(15) . . ? C6A Mo S2 128.1(4) . . ? C7A Mo S2 131.3(3) . . ? C6C Mo S2 139.2(3) . . ? C10C Mo S2 111.9(3) . . ? C1C Mo S2 137.73(14) . . ? C5C Mo S2 110.84(16) . . ? C10A Mo S2 93.6(4) . . ? C8A Mo S2 97.4(4) . . ? C9A Mo S2 76.5(3) . . ? S1 Mo S2 81.41(4) . . ? C1 S1 Mo 104.08(16) . . ? C2 S2 Mo 104.42(16) . . ? C1 C2 C1P 121.6(4) . . ? C1 C2 S2 118.6(3) . . ? C1P C2 S2 119.5(3) . . ? C2 C1 S1 124.4(4) . . ? C2C C1C C5C 108.8(5) . . ? C2C C1C Mo 71.8(3) . . ? C5C C1C Mo 72.9(3) . . ? C1C C2C C3C 107.2(5) . . ? C1C C2C Mo 73.7(3) . . ? C3C C2C Mo 70.9(3) . . ? C2C C3C C4C 107.2(5) . . ? C2C C3C Mo 73.3(3) . . ? C4C C3C Mo 73.0(3) . . ? C5C C4C C3C 107.6(5) . . ? C5C C4C Mo 74.2(3) . . ? C3C C4C Mo 71.2(3) . . ? C4C C5C C1C 109.1(5) . . ? C4C C5C Mo 71.6(3) . . ? C1C C5C Mo 72.7(3) . . ? C7C C6C C10C 109.4(9) . . ? C7C C6C Mo 71.2(6) . . ? C10C C6C Mo 72.6(5) . . ? C6C C7C C8C 107.5(10) . . ? C6C C7C Mo 73.8(6) . . ? C8C C7C Mo 70.8(6) . . ? C7C C8C C9C 106.6(9) . . ? C7C C8C Mo 72.6(6) . . ? C9C C8C Mo 72.8(6) . . ? C10C C9C C8C 108.0(9) . . ? C10C C9C Mo 73.7(6) . . ? C8C C9C Mo 70.6(6) . . ? C9C C10C C6C 108.4(9) . . ? C9C C10C Mo 71.4(5) . . ? C6C C10C Mo 72.5(5) . . ? C10A C6A C7A 109.6(11) . . ? C10A C6A Mo 73.6(7) . . ? C7A C6A Mo 72.6(6) . . ? C6A C7A C8A 106.2(11) . . ? C6A C7A Mo 72.1(6) . . ? C8A C7A Mo 75.4(7) . . ? C9A C8A C7A 110.4(11) . . ? C9A C8A Mo 74.1(7) . . ? C7A C8A Mo 70.1(6) . . ? C8A C9A C10A 106.8(11) . . ? C8A C9A Mo 72.6(7) . . ? C10A C9A Mo 69.8(7) . . ? C6A C10A C9A 106.8(12) . . ? C6A C10A Mo 71.6(7) . . ? C9A C10A Mo 74.9(8) . . ? C2P C1P C6P 116.6(4) . . ? C2P C1P C2 121.5(4) . . ? C6P C1P C2 121.9(4) . . ? C5P C6P C1P 119.3(5) . . ? C6P C5P C4P 119.3(5) . . ? N3P C4P C5P 123.1(5) . . ? C4P N3P C2P 116.7(5) . . ? N3P C2P C1P 125.0(5) . . ? F3 B F4 109.2(6) . . ? F1 B F4 111.0(6) . . ? F2 B F4 98.2(5) . . ? F3 B F1 117.8(6) . . ? F3 B F2 109.1(5) . . ? F1 B F2 109.7(5) . . ? F2' B F4' 117.7(8) . . ? F2' B F1' 111.8(7) . . ? F4' B F1' 105.6(7) . . ? F2' B F3' 112.1(7) . . ? F4' B F3' 103.5(6) . . ? F1' B F3' 105.0(6) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.85 _refine_diff_density_min -1.03 _refine_diff_density_rms 0.12 #=== END of CIF data_9 _database_code_depnum_ccdc_archive 'CCDC 822497' #TrackingRef '- combined.cif' #wcptph _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H15 N S2 W' _chemical_formula_sum 'C17 H15 N S2 W' _chemical_formula_weight 481.27 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.5703(14) _cell_length_b 11.879(2) _cell_length_c 11.992(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.136(2) _cell_angle_gamma 90.00 _cell_volume 1494.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 987 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 28.60 _exptl_crystal_description column _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.140 _exptl_crystal_density_method ? _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 8.002 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.266 _exptl_absorpt_correction_T_max 0.397 _exptl_absorpt_process_details 'SADABS, Bruker' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2 _diffrn_reflns_number 15505 _diffrn_reflns_av_R_equivalents 0.031 _diffrn_reflns_av_sigmaI/netI 0.018 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 28.88 _reflns_number_total 3608 _reflns_number_gt 3275 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; ; _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^)+(0.0329P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 3608 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0215 _refine_ls_R_factor_gt 0.0185 _refine_ls_wR_factor_ref 0.0490 _refine_ls_wR_factor_gt 0.0480 _refine_ls_goodness_of_fit_ref 1.02 _refine_ls_restrained_S_all 1.02 _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 W W 0.786189(9) 0.837544(8) 0.621365(8) 0.01574(5) Uani 1 1 d . . . S1 S 0.72851(7) 1.02799(5) 0.55656(6) 0.02015(14) Uani 1 1 d . . . S2 S 0.80484(7) 0.80956(6) 0.42312(6) 0.02045(14) Uani 1 1 d . . . C1 C 0.7170(2) 1.0247(2) 0.4104(2) 0.0182(5) Uani 1 1 d . . . H1A H 0.6871 1.0901 0.3697 0.022 Uiso 1 1 calc R . . C2 C 0.7485(3) 0.9335(2) 0.3518(2) 0.0182(5) Uani 1 1 d . . . C1P C 0.7413(2) 0.9332(2) 0.2284(2) 0.0173(5) Uani 1 1 d . . . C2P C 0.6765(3) 1.0154(2) 0.1594(2) 0.0235(6) Uani 1 1 d . . . H2PA H 0.6358 1.0759 0.1925 0.028 Uiso 1 1 calc R . . C3P C 0.6713(3) 1.0095(2) 0.0447(2) 0.0269(6) Uani 1 1 d . . . H3PA H 0.6268 1.0674 0.0014 0.032 Uiso 1 1 calc R . . C5P C 0.7876(3) 0.8490(2) 0.0547(3) 0.0275(7) Uani 1 1 d . . . H5PA H 0.8273 0.7898 0.0188 0.033 Uiso 1 1 calc R . . C6P C 0.7985(3) 0.8482(2) 0.1710(3) 0.0227(6) Uani 1 1 d . . . H6PA H 0.8448 0.7898 0.2119 0.027 Uiso 1 1 calc R . . N N 0.7249(2) 0.9276(2) -0.0106(2) 0.0279(5) Uani 1 1 d . . . C1C C 0.6608(3) 0.7610(3) 0.7507(3) 0.0322(7) Uani 1 1 d . . . H1CA H 0.6845 0.7577 0.8340 0.039 Uiso 1 1 calc R . . C2C C 0.6792(3) 0.6731(2) 0.6733(3) 0.0310(7) Uani 1 1 d . . . H2CA H 0.7196 0.5984 0.6927 0.037 Uiso 1 1 calc R . . C3C C 0.6215(3) 0.7061(3) 0.5672(3) 0.0280(7) Uani 1 1 d . . . H3CA H 0.6136 0.6587 0.4978 0.034 Uiso 1 1 calc R . . C4C C 0.5713(3) 0.8149(3) 0.5753(3) 0.0270(7) Uani 1 1 d . . . H4CA H 0.5173 0.8556 0.5138 0.032 Uiso 1 1 calc R . . C5C C 0.5944(3) 0.8505(3) 0.6906(3) 0.0297(7) Uani 1 1 d . . . H5CA H 0.5587 0.9190 0.7237 0.036 Uiso 1 1 calc R . . C6C C 0.9825(3) 0.7555(3) 0.6583(3) 0.0336(8) Uani 1 1 d . . . H6CA H 1.0098 0.6826 0.6272 0.040 Uiso 1 1 calc R . . C7C C 1.0075(3) 0.8660(3) 0.6184(3) 0.0335(7) Uani 1 1 d . . . H7CA H 1.0495 0.8833 0.5501 0.040 Uiso 1 1 calc R . . C8C C 0.9716(3) 0.9449(3) 0.6941(3) 0.0272(6) Uani 1 1 d . . . H8CA H 0.9810 1.0283 0.6879 0.033 Uiso 1 1 calc R . . C9C C 0.9226(3) 0.8882(3) 0.7819(2) 0.0254(6) Uani 1 1 d . . . H9CA H 0.8966 0.9236 0.8513 0.030 Uiso 1 1 calc R . . C10C C 0.9337(3) 0.7711(3) 0.7621(3) 0.0302(7) Uani 1 1 d . . . H10A H 0.9187 0.7099 0.8163 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 W 0.01613(7) 0.01713(7) 0.01379(7) 0.00040(3) 0.00122(4) 0.00012(4) S1 0.0259(4) 0.0177(3) 0.0169(3) -0.0015(2) 0.0031(3) 0.0029(2) S2 0.0293(4) 0.0174(3) 0.0148(3) -0.0001(2) 0.0030(3) 0.0039(3) C1 0.0198(14) 0.0174(13) 0.0170(13) 0.0017(10) 0.0012(10) -0.0011(10) C2 0.0177(13) 0.0182(13) 0.0187(13) 0.0015(10) 0.0026(11) -0.0012(10) C1P 0.0177(13) 0.0165(12) 0.0177(13) 0.0007(10) 0.0018(11) -0.0021(10) C2P 0.0296(15) 0.0191(13) 0.0224(15) 0.0019(11) 0.0057(12) 0.0031(11) C3P 0.0362(17) 0.0225(14) 0.0222(15) 0.0054(11) 0.0044(13) 0.0036(12) C5P 0.0335(19) 0.0295(16) 0.0202(16) -0.0022(11) 0.0054(13) 0.0062(12) C6P 0.0253(16) 0.0241(15) 0.0183(15) -0.0028(11) 0.0018(12) 0.0056(11) N 0.0322(14) 0.0334(14) 0.0181(12) 0.0006(10) 0.0033(11) 0.0022(11) C1C 0.0339(18) 0.0399(18) 0.0238(16) 0.0059(13) 0.0074(14) -0.0127(14) C2C 0.0296(17) 0.0250(16) 0.0375(19) 0.0083(12) 0.0013(14) -0.0094(12) C3C 0.0279(16) 0.0295(15) 0.0267(16) -0.0022(13) 0.0044(13) -0.0137(12) C4C 0.0153(14) 0.0346(16) 0.0302(17) 0.0066(13) -0.0002(12) -0.0041(12) C5C 0.0207(16) 0.0360(17) 0.0354(19) -0.0025(13) 0.0156(14) -0.0031(12) C6C 0.0231(16) 0.0365(18) 0.0381(18) -0.0127(14) -0.0088(14) 0.0102(13) C7C 0.0184(16) 0.057(2) 0.0255(17) -0.0046(15) 0.0038(13) -0.0050(14) C8C 0.0187(14) 0.0304(15) 0.0305(17) 0.0023(12) -0.0044(12) -0.0072(11) C9C 0.0213(15) 0.0341(16) 0.0195(14) -0.0037(12) -0.0029(12) -0.0022(12) C10C 0.0291(17) 0.0322(16) 0.0261(16) 0.0068(12) -0.0095(13) -0.0002(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W C6C 2.285(3) . ? W C4C 2.286(3) . ? W C5C 2.289(3) . ? W C10C 2.291(3) . ? W C9C 2.337(3) . ? W C1C 2.345(3) . ? W C3C 2.368(3) . ? W C7C 2.369(3) . ? W C2C 2.378(3) . ? W C8C 2.409(3) . ? W S2 2.4326(8) . ? W S1 2.4446(7) . ? S1 C1 1.743(3) . ? S2 C2 1.769(3) . ? C1 C2 1.355(4) . ? C2 C1P 1.472(4) . ? C1P C6P 1.401(4) . ? C1P C2P 1.402(4) . ? C2P C3P 1.372(4) . ? C3P N 1.342(4) . ? C5P N 1.340(4) . ? C5P C6P 1.384(5) . ? C1C C5C 1.420(5) . ? C1C C2C 1.427(5) . ? C2C C3C 1.396(5) . ? C3C C4C 1.405(4) . ? C4C C5C 1.437(5) . ? C6C C10C 1.417(5) . ? C6C C7C 1.433(5) . ? C7C C8C 1.390(4) . ? C8C C9C 1.402(4) . ? C9C C10C 1.419(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6C W C4C 147.95(11) . . ? C6C W C5C 141.44(13) . . ? C4C W C5C 36.62(12) . . ? C6C W C10C 36.08(12) . . ? C4C W C10C 134.61(11) . . ? C5C W C10C 107.96(13) . . ? C6C W C9C 59.82(11) . . ? C4C W C9C 136.28(11) . . ? C5C W C9C 99.66(12) . . ? C10C W C9C 35.69(11) . . ? C6C W C1C 106.30(13) . . ? C4C W C1C 59.20(11) . . ? C5C W C1C 35.65(12) . . ? C10C W C1C 76.59(12) . . ? C9C W C1C 84.06(11) . . ? C6C W C3C 112.99(11) . . ? C4C W C3C 35.08(11) . . ? C5C W C3C 59.33(11) . . ? C10C W C3C 112.60(11) . . ? C9C W C3C 138.86(11) . . ? C1C W C3C 57.95(11) . . ? C6C W C7C 35.81(12) . . ? C4C W C7C 165.22(12) . . ? C5C W C7C 156.46(13) . . ? C10C W C7C 58.47(12) . . ? C9C W C7C 57.71(11) . . ? C1C W C7C 134.89(12) . . ? C3C W C7C 141.60(11) . . ? C6C W C2C 92.81(12) . . ? C4C W C2C 58.39(11) . . ? C5C W C2C 59.26(11) . . ? C10C W C2C 80.00(12) . . ? C9C W C2C 105.11(11) . . ? C1C W C2C 35.15(12) . . ? C3C W C2C 34.21(11) . . ? C7C W C2C 128.60(12) . . ? C6C W C8C 58.48(12) . . ? C4C W C8C 152.78(11) . . ? C5C W C8C 123.40(12) . . ? C10C W C8C 57.79(11) . . ? C9C W C8C 34.31(10) . . ? C1C W C8C 117.82(11) . . ? C3C W C8C 170.20(11) . . ? C7C W C8C 33.82(11) . . ? C2C W C8C 137.03(11) . . ? C6C W S2 87.10(9) . . ? C4C W S2 86.93(8) . . ? C5C W S2 123.12(10) . . ? C10C W S2 122.85(9) . . ? C9C W S2 136.37(8) . . ? C1C W S2 135.61(8) . . ? C3C W S2 77.76(8) . . ? C7C W S2 78.74(8) . . ? C2C W S2 104.04(9) . . ? C8C W S2 105.38(8) . . ? C6C W S1 129.85(9) . . ? C4C W S1 80.28(8) . . ? C5C W S1 81.72(8) . . ? C10C W S1 132.31(8) . . ? C9C W S1 97.33(8) . . ? C1C W S1 115.45(9) . . ? C3C W S1 112.17(8) . . ? C7C W S1 94.07(9) . . ? C2C W S1 137.33(9) . . ? C8C W S1 77.58(7) . . ? S2 W S1 82.13(2) . . ? C1 S1 W 106.42(9) . . ? C2 S2 W 107.19(10) . . ? C2 C1 S1 123.2(2) . . ? C1 C2 C1P 122.5(2) . . ? C1 C2 S2 120.3(2) . . ? C1P C2 S2 117.13(19) . . ? C6P C1P C2P 114.9(3) . . ? C6P C1P C2 121.6(3) . . ? C2P C1P C2 123.4(2) . . ? C3P C2P C1P 120.8(3) . . ? N C3P C2P 124.5(3) . . ? N C5P C6P 124.6(3) . . ? C5P C6P C1P 120.2(3) . . ? C5P N C3P 115.1(3) . . ? C5C C1C C2C 108.4(3) . . ? C5C C1C W 70.00(17) . . ? C2C C1C W 73.68(18) . . ? C3C C2C C1C 108.0(3) . . ? C3C C2C W 72.50(17) . . ? C1C C2C W 71.17(16) . . ? C2C C3C C4C 108.7(3) . . ? C2C C3C W 73.29(17) . . ? C4C C3C W 69.24(16) . . ? C3C C4C C5C 108.5(3) . . ? C3C C4C W 75.68(17) . . ? C5C C4C W 71.82(17) . . ? C1C C5C C4C 106.4(3) . . ? C1C C5C W 74.35(18) . . ? C4C C5C W 71.56(17) . . ? C10C C6C C7C 106.1(3) . . ? C10C C6C W 72.19(17) . . ? C7C C6C W 75.27(18) . . ? C8C C7C C6C 108.8(3) . . ? C8C C7C W 74.68(18) . . ? C6C C7C W 68.92(17) . . ? C7C C8C C9C 108.9(3) . . ? C7C C8C W 71.50(18) . . ? C9C C8C W 70.02(16) . . ? C8C C9C C10C 107.4(3) . . ? C8C C9C W 75.67(17) . . ? C10C C9C W 70.40(15) . . ? C6C C10C C9C 108.7(3) . . ? C6C C10C W 71.74(17) . . ? C9C C10C W 73.91(16) . . ? _diffrn_measured_fraction_theta_max 0.919 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.95 _refine_diff_density_min -0.91 _refine_diff_density_rms 0.12 #=== END of CIF data_8BF4 _database_code_depnum_ccdc_archive 'CCDC 822498' #TrackingRef '- combined.cif' # s752a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _publ_section_exptl_refinement ; The structure was solved by direct methods (SIR). H atoms were included in calculated positions. The Cp ring C13 to C17 was disordered over 2 sites, each at 0.5 occupancy. The two disordered fragments were constrained to be regular pentagons. The atoms F3 and F4 were also disordered over two sites, with occupancies of 0.5; the bond lengths of the F atoms to B1 were restrained to be equal. All non H atoms were refined anisotropically, with restraints on those of the disordered atoms. ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1995). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H15 N S2 W, B F4 ' _chemical_formula_sum 'C17 H15 B F4 N S2 W' _chemical_formula_weight 568.08 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' N N 0.0061 0.0033 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 'P 21/n' _symmetry_space_group_name_Hall -P2yn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.9700(9) _cell_length_b 14.514(2) _cell_length_c 17.689(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.907(10) _cell_angle_gamma 90.00 _cell_volume 1757.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description NEEDLE _exptl_crystal_colour BROWN _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.147 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1084 _exptl_absorpt_coefficient_mu 6.853 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.4101 _exptl_absorpt_correction_T_max 0.4587 _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 Number of psi-scan sets used was 3 Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 'Enraf Nonius CAD4' _diffrn_refln_scan_width 1.20 _diffrn_measurement_method omega-2theta _diffrn_refln_scan_mode_backgd MO _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _diffrn_reflns_number 3343 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0673 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 24.97 _reflns_number_total 3082 _reflns_number_gt 2147 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express (Enraf Nonius, 1992)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1992)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 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^)+(0.0275P)^2^+4.1796P] 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 3082 _refine_ls_number_parameters 284 _refine_ls_number_restraints 232 _refine_ls_R_factor_all 0.0776 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.0798 _refine_ls_wR_factor_gt 0.0686 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 0.999 _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 0.22726(5) 0.19756(3) 0.12010(2) 0.02852(12) Uani 1 1 d . . . S1 S 0.5508(4) 0.22955(17) 0.09954(16) 0.0402(6) Uani 1 1 d . . . S2 S 0.1746(4) 0.35202(17) 0.07148(15) 0.0369(6) Uani 1 1 d . . . C1 C 0.5635(15) 0.3460(7) 0.1042(6) 0.041(3) Uani 1 1 d . . . H1 H 0.6875 0.3738 0.1143 0.049 Uiso 1 1 calc R . . C2 C 0.4040(13) 0.4010(6) 0.0941(5) 0.033(2) Uani 1 1 d . . . C3 C 0.4183(14) 0.5037(6) 0.0942(5) 0.035(2) Uani 1 1 d . . . C4 C 0.5999(16) 0.5484(7) 0.1147(6) 0.048(3) Uani 1 1 d . . . H4 H 0.7148 0.5136 0.1291 0.057 Uiso 1 1 calc R . . C5 C 0.6092(17) 0.6431(7) 0.1136(6) 0.050(3) Uani 1 1 d . . . H5 H 0.7295 0.6738 0.1269 0.060 Uiso 1 1 calc R . . C6 C 0.4418(16) 0.6906(8) 0.0930(5) 0.047(3) Uani 1 1 d . . . H6 H 0.4494 0.7552 0.0925 0.057 Uiso 1 1 calc R . . N1 N 0.2647(14) 0.6519(6) 0.0731(5) 0.052(2) Uani 1 1 d . . . C7 C 0.2601(16) 0.5601(7) 0.0738(6) 0.048(3) Uani 1 1 d . . . H7 H 0.1375 0.5318 0.0590 0.058 Uiso 1 1 calc R . . C8 C 0.1702(17) 0.1571(7) -0.0074(5) 0.048(3) Uani 1 1 d . A . H8 H 0.2194 0.1937 -0.0432 0.058 Uiso 1 1 calc R . . C9 C -0.0113(15) 0.1676(7) 0.0145(6) 0.047(3) Uani 1 1 d . A . H9 H -0.1045 0.2132 -0.0035 0.056 Uiso 1 1 calc R . . C10 C -0.0294(14) 0.1003(8) 0.0663(6) 0.046(3) Uani 1 1 d . A . H10 H -0.1388 0.0911 0.0894 0.056 Uiso 1 1 calc R . . C11 C 0.1396(16) 0.0472(7) 0.0796(6) 0.045(3) Uani 1 1 d . A . H11 H 0.1653 -0.0033 0.1132 0.054 Uiso 1 1 calc R . . C12 C 0.2647(15) 0.0829(7) 0.0334(6) 0.048(3) Uani 1 1 d . A . H12 H 0.3899 0.0608 0.0306 0.057 Uiso 1 1 calc R . . C13A C 0.070(3) 0.2359(15) 0.2200(10) 0.032(4) Uani 0.50 1 d PGU A 3 H13A H -0.0580 0.2597 0.2100 0.038 Uiso 0.50 1 calc PR A 3 C14A C 0.122(3) 0.1401(14) 0.2252(11) 0.035(4) Uani 0.50 1 d PGU A 3 H14A H 0.0349 0.0901 0.2191 0.042 Uiso 0.50 1 calc PR A 3 C15A C 0.332(3) 0.1340(12) 0.2412(12) 0.040(4) Uani 0.50 1 d PGU A 3 H15A H 0.4056 0.0794 0.2475 0.048 Uiso 0.50 1 calc PR A 3 C16A C 0.409(2) 0.2261(18) 0.2460(12) 0.041(4) Uani 0.50 1 d PGU A 3 H16A H 0.5419 0.2423 0.2559 0.049 Uiso 0.50 1 calc PR A 3 C17A C 0.247(4) 0.2891(11) 0.2329(10) 0.041(4) Uani 0.50 1 d PGU A 3 H17A H 0.2553 0.3538 0.2328 0.050 Uiso 0.50 1 calc PR A 3 C13B C 0.067(3) 0.1841(19) 0.2245(11) 0.045(4) Uani 0.50 1 d PGU A 4 H13B H -0.0682 0.1724 0.2168 0.054 Uiso 0.50 1 calc PR A 4 C14B C 0.212(4) 0.1188(11) 0.2336(11) 0.045(4) Uani 0.50 1 d PGU A 4 H14B H 0.1945 0.0546 0.2333 0.054 Uiso 0.50 1 calc PR A 4 C15B C 0.389(3) 0.1640(17) 0.2433(13) 0.042(4) Uani 0.50 1 d PGU A 4 H15B H 0.5127 0.1361 0.2508 0.051 Uiso 0.50 1 calc PR A 4 C16B C 0.352(4) 0.2572(13) 0.2402(12) 0.037(4) Uani 0.50 1 d PGU A 4 H16B H 0.4468 0.3042 0.2451 0.045 Uiso 0.50 1 calc PR A 4 C17B C 0.153(3) 0.2696(16) 0.2285(11) 0.042(4) Uani 0.50 1 d PGU A 4 H17B H 0.0878 0.3266 0.2241 0.050 Uiso 0.50 1 calc PR A 4 F1 F 0.7688(13) 0.3461(6) 0.3073(5) 0.107(3) Uani 1 1 d DU B . F2 F 0.9245(12) 0.4492(5) 0.2526(4) 0.089(2) Uani 1 1 d DU B . F3A F 0.982(2) 0.4187(10) 0.3749(8) 0.071(4) Uani 0.50 1 d PDU B 1 F4A F 0.761(3) 0.5188(10) 0.3214(12) 0.110(5) Uani 0.50 1 d PDU B 1 F3B F 0.908(3) 0.4640(14) 0.3821(8) 0.094(5) Uani 0.50 1 d PDU B 2 F4B F 0.632(2) 0.4620(15) 0.2961(10) 0.109(5) Uani 0.50 1 d PDU B 2 B1 B 0.8299(17) 0.4342(7) 0.3118(6) 0.065(3) Uani 1 1 d DU . . 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 0.02597(18) 0.02438(18) 0.0358(2) -0.0023(2) 0.00737(13) 0.0004(2) S2 0.0347(14) 0.0269(13) 0.0468(15) -0.0007(12) 0.0017(12) 0.0017(11) S1 0.0280(13) 0.0383(14) 0.0555(16) -0.0033(12) 0.0108(12) 0.0005(11) C6 0.075(8) 0.031(5) 0.032(5) 0.000(5) 0.001(5) -0.022(7) C2 0.035(5) 0.030(5) 0.033(5) -0.005(4) -0.001(4) -0.008(4) C1 0.038(6) 0.043(6) 0.042(6) -0.002(5) 0.010(5) -0.007(5) C3 0.044(6) 0.032(5) 0.027(5) 0.003(4) 0.002(4) -0.012(5) C4 0.051(7) 0.045(7) 0.046(6) 0.009(5) 0.006(5) -0.005(5) C5 0.057(7) 0.045(7) 0.040(6) 0.000(5) -0.011(6) -0.017(6) N1 0.072(7) 0.028(5) 0.048(6) 0.004(4) -0.008(5) 0.000(5) C7 0.049(7) 0.041(7) 0.048(7) -0.003(5) -0.010(5) -0.003(5) C8 0.078(8) 0.043(6) 0.024(5) -0.007(5) 0.011(5) -0.023(6) C9 0.039(6) 0.036(6) 0.057(7) -0.015(5) -0.013(5) 0.013(5) C10 0.031(6) 0.055(7) 0.052(7) -0.017(6) 0.006(5) -0.023(5) C11 0.054(7) 0.030(6) 0.046(7) -0.007(5) -0.007(6) -0.005(5) C12 0.044(6) 0.039(6) 0.061(7) -0.031(6) 0.013(6) 0.001(5) C13A 0.042(7) 0.021(8) 0.036(8) -0.005(9) 0.020(7) -0.003(7) C14A 0.048(8) 0.026(8) 0.037(8) -0.002(8) 0.020(8) -0.002(7) C15A 0.047(9) 0.038(7) 0.036(8) 0.005(8) 0.009(9) 0.000(7) C16A 0.043(7) 0.044(10) 0.033(8) -0.004(9) 0.004(8) -0.004(7) C17A 0.043(10) 0.035(7) 0.044(8) -0.004(8) 0.002(9) -0.009(7) C13B 0.048(7) 0.050(10) 0.045(8) -0.001(10) 0.025(7) -0.006(7) C14B 0.051(10) 0.041(7) 0.044(8) 0.004(8) 0.011(10) -0.006(7) C15B 0.046(7) 0.044(9) 0.037(8) -0.004(9) 0.007(8) 0.001(7) C16B 0.043(8) 0.035(8) 0.034(8) -0.008(8) 0.008(8) -0.002(7) C17B 0.045(9) 0.041(8) 0.044(8) -0.001(8) 0.023(9) 0.002(7) F1 0.115(7) 0.084(5) 0.120(7) -0.010(5) 0.018(5) -0.043(5) F2 0.117(6) 0.081(5) 0.079(5) 0.013(4) 0.046(4) 0.010(5) F3A 0.090(10) 0.044(8) 0.075(7) -0.007(7) 0.003(7) -0.002(7) F4A 0.109(12) 0.087(8) 0.136(13) -0.020(10) 0.032(10) 0.056(9) F3B 0.104(8) 0.102(9) 0.079(6) -0.027(7) 0.023(6) -0.027(7) F4B 0.093(8) 0.149(13) 0.090(11) -0.033(11) 0.028(7) 0.030(10) B1 0.087(8) 0.050(6) 0.060(7) -0.009(7) 0.021(6) 0.005(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 S2 2.404(3) . ? W1 S1 2.397(3) . ? W1 C14A 2.280(18) . ? W1 C8 2.291(9) . ? W1 C9 2.295(10) . ? W1 C15B 2.31(2) . ? W1 C16B 2.31(2) . ? W1 C12 2.311(9) . ? W1 C13A 2.318(17) . ? W1 C15A 2.32(2) . ? W1 C14B 2.330(19) . ? W1 C17B 2.327(19) . ? W1 C10 2.336(9) . ? W1 C11 2.342(10) . ? S2 C2 1.726(9) . ? S1 C1 1.694(10) . ? C6 N1 1.341(12) . ? C6 C5 1.344(14) . ? C6 H6 0.9400 . ? C1 C2 1.353(13) . ? C2 C3 1.494(12) . ? C1 H1 0.9400 . ? C3 C7 1.366(13) . ? C3 C4 1.407(13) . ? C4 C5 1.376(14) . ? C4 H4 0.9400 . ? C5 H5 0.9400 . ? N1 C7 1.332(12) . ? C7 H7 0.9400 . ? C8 C12 1.390(14) . ? C8 C9 1.399(14) . ? C8 H8 0.9400 . ? C9 C10 1.362(14) . ? C9 H9 0.9400 . ? C10 C11 1.390(14) . ? C10 H10 0.9400 . ? C11 C12 1.402(14) . ? C11 H11 0.9400 . ? C12 H12 0.9400 . ? C13A C14A 1.437(15) . ? C13A C17A 1.438(15) . ? C13A H13A 0.9400 . ? C14A C15A 1.437(15) . ? C14A H14A 0.9400 . ? C15A C16A 1.437(15) . ? C15A H15A 0.9400 . ? C16A C17A 1.437(15) . ? C16A H16A 0.9400 . ? C17A H17A 0.9400 . ? C13B C17B 1.376(16) . ? C13B C14B 1.376(16) . ? C13B H13B 0.9400 . ? C14B C15B 1.376(16) . ? C14B H14B 0.9400 . ? C15B C16B 1.376(16) . ? C15B H15B 0.9400 . ? C16B C17B 1.376(16) . ? C16B H16B 0.9400 . ? C17B H17B 0.9400 . ? F1 B1 1.346(10) . ? F2 B1 1.355(10) . ? F3A B1 1.406(12) . ? F4A B1 1.340(12) . ? F3B B1 1.331(13) . ? F4B B1 1.411(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 S1 W1 S2 81.34(9) . . ? C14A W1 C8 133.3(5) . . ? C14A W1 C9 107.4(5) . . ? C8 W1 C9 35.5(4) . . ? C14A W1 C15B 47.8(5) . . ? C8 W1 C15B 147.0(6) . . ? C9 W1 C15B 151.4(7) . . ? C14A W1 C16B 60.7(5) . . ? C8 W1 C16B 165.4(5) . . ? C9 W1 C16B 155.5(7) . . ? C15B W1 C16B 34.7(4) . . ? C14A W1 C12 111.8(6) . . ? C8 W1 C12 35.2(4) . . ? C9 W1 C12 58.6(4) . . ? C15B W1 C12 112.2(6) . . ? C16B W1 C12 144.2(7) . . ? C14A W1 C13A 36.4(4) . . ? C8 W1 C13A 142.5(6) . . ? C9 W1 C13A 106.9(5) . . ? C15B W1 C13A 63.1(5) . . ? C16B W1 C13A 50.1(5) . . ? C12 W1 C13A 143.9(6) . . ? C14A W1 C15A 36.4(4) . . ? C8 W1 C15A 140.6(5) . . ? C9 W1 C15A 136.8(7) . . ? C15B W1 C15A 14.6(5) . . ? C16B W1 C15A 45.7(5) . . ? C12 W1 C15A 105.7(5) . . ? C13A W1 C15A 60.2(6) . . ? C14A W1 C14B 17.2(4) . . ? C8 W1 C14B 134.0(5) . . ? C9 W1 C14B 117.7(7) . . ? C15B W1 C14B 34.5(4) . . ? C16B W1 C14B 57.4(6) . . ? C12 W1 C14B 104.4(5) . . ? C13A W1 C14B 49.9(4) . . ? C15A W1 C14B 21.0(4) . . ? C14A W1 C17B 48.5(4) . . ? C8 W1 C17B 154.5(6) . . ? C9 W1 C17B 121.1(6) . . ? C15B W1 C17B 57.4(6) . . ? C16B W1 C17B 34.5(4) . . ? C12 W1 C17B 160.3(7) . . ? C13A W1 C17B 18.7(4) . . ? C15A W1 C17B 59.8(5) . . ? C14B W1 C17B 57.1(6) . . ? C14A W1 C10 76.8(5) . . ? C8 W1 C10 57.8(4) . . ? C9 W1 C10 34.2(3) . . ? C15B W1 C10 117.2(7) . . ? C16B W1 C10 136.8(5) . . ? C12 W1 C10 57.9(4) . . ? C13A W1 C10 91.1(6) . . ? C15A W1 C10 102.6(7) . . ? C14B W1 C10 84.2(6) . . ? C17B W1 C10 109.6(7) . . ? C14A W1 C11 78.6(5) . . ? C8 W1 C11 58.2(4) . . ? C9 W1 C11 57.8(4) . . ? C15B W1 C11 98.3(7) . . ? C16B W1 C11 131.5(6) . . ? C12 W1 C11 35.1(3) . . ? C13A W1 C11 108.9(6) . . ? C15A W1 C11 86.0(6) . . ? C14B W1 C11 75.8(5) . . ? C17B W1 C11 125.9(7) . . ? C10 W1 C11 34.6(3) . . ? C1 S1 W1 103.3(3) . . ? C2 S2 W1 103.2(4) . . ? N1 C6 C5 124.4(10) . . ? N1 C6 H6 117.8 . . ? C5 C6 H6 117.8 . . ? C1 C2 C3 122.4(9) . . ? C1 C2 S2 119.3(7) . . ? C3 C2 S2 118.1(7) . . ? C2 C1 S1 123.3(8) . . ? C2 C1 H1 118.4 . . ? S1 C1 H1 118.4 . . ? C7 C3 C4 115.7(9) . . ? C7 C3 C2 123.2(9) . . ? C4 C3 C2 121.1(9) . . ? C5 C4 C3 119.9(11) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C6 C5 C4 118.3(11) . . ? C6 C5 H5 120.8 . . ? C4 C5 H5 120.8 . . ? C7 N1 C6 116.0(10) . . ? N1 C7 C3 125.6(10) . . ? N1 C7 H7 117.2 . . ? C3 C7 H7 117.2 . . ? C12 C8 C9 107.8(9) . . ? C12 C8 W1 73.2(5) . . ? C9 C8 W1 72.4(6) . . ? C12 C8 H8 126.1 . . ? C9 C8 H8 126.1 . . ? W1 C8 H8 120.1 . . ? C10 C9 C8 108.2(9) . . ? C10 C9 W1 74.5(6) . . ? C8 C9 W1 72.1(6) . . ? C10 C9 H9 125.9 . . ? C8 C9 H9 125.9 . . ? W1 C9 H9 119.3 . . ? C9 C10 C11 109.1(9) . . ? C9 C10 W1 71.3(6) . . ? C11 C10 W1 73.0(5) . . ? C9 C10 H10 125.4 . . ? C11 C10 H10 125.4 . . ? W1 C10 H10 122.0 . . ? C10 C11 C12 107.3(10) . . ? C10 C11 W1 72.5(6) . . ? C12 C11 W1 71.2(5) . . ? C10 C11 H11 126.3 . . ? C12 C11 H11 126.3 . . ? W1 C11 H11 121.7 . . ? C8 C12 C11 107.6(9) . . ? C8 C12 W1 71.6(5) . . ? C11 C12 W1 73.7(6) . . ? C8 C12 H12 126.2 . . ? C11 C12 H12 126.2 . . ? W1 C12 H12 120.3 . . ? C14A C13A C17A 108.0 . . ? C14A C13A W1 70.4(7) . . ? C17A C13A W1 74.5(7) . . ? C14A C13A H13A 126.0 . . ? C17A C13A H13A 126.0 . . ? W1 C13A H13A 120.9 . . ? C13A C14A C15A 108.0 . . ? C13A C14A W1 73.2(6) . . ? C15A C14A W1 73.3(7) . . ? C13A C14A H14A 126.0 . . ? C15A C14A H14A 126.0 . . ? W1 C14A H14A 119.4 . . ? C14A C15A C16A 108.0 . . ? C14A C15A W1 70.3(7) . . ? C16A C15A W1 74.5(6) . . ? C14A C15A H15A 126.0 . . ? C16A C15A H15A 126.0 . . ? W1 C15A H15A 120.9 . . ? C15A C16A C17A 108.0 . . ? C15A C16A W1 69.9(6) . . ? C17A C16A W1 72.4(6) . . ? C15A C16A H16A 126.0 . . ? C17A C16A H16A 126.0 . . ? W1 C16A H16A 123.3 . . ? C16A C17A C13A 108.0 . . ? C16A C17A W1 72.4(7) . . ? C13A C17A W1 69.9(7) . . ? C16A C17A H17A 126.0 . . ? C13A C17A H17A 126.0 . . ? W1 C17A H17A 123.3 . . ? C17B C13B C14B 108.0 . . ? C17B C13B W1 72.3(7) . . ? C14B C13B W1 72.4(7) . . ? C17B C13B H13B 126.0 . . ? C14B C13B H13B 126.0 . . ? W1 C13B H13B 121.0 . . ? C15B C14B C13B 108.0 . . ? C15B C14B W1 71.9(7) . . ? C13B C14B W1 73.3(7) . . ? C15B C14B H14B 126.0 . . ? C13B C14B H14B 126.0 . . ? W1 C14B H14B 120.6 . . ? C16B C15B C14B 108.0 . . ? C16B C15B W1 72.6(7) . . ? C14B C15B W1 73.6(7) . . ? C16B C15B H15B 126.0 . . ? C14B C15B H15B 126.0 . . ? W1 C15B H15B 119.7 . . ? C17B C16B C15B 108.0 . . ? C17B C16B W1 73.5(7) . . ? C15B C16B W1 72.7(7) . . ? C17B C16B H16B 126.0 . . ? C15B C16B H16B 126.0 . . ? W1 C16B H16B 119.6 . . ? C16B C17B C13B 108.0 . . ? C16B C17B W1 71.9(7) . . ? C13B C17B W1 73.4(7) . . ? C16B C17B H17B 126.0 . . ? C13B C17B H17B 126.0 . . ? W1 C17B H17B 120.4 . . ? F3B B1 F1 115.6(13) . . ? F4A B1 F1 139.7(14) . . ? F3B B1 F2 119.8(13) . . ? F4A B1 F2 100.9(12) . . ? F1 B1 F2 107.5(9) . . ? F4A B1 F3A 106.2(12) . . ? F1 B1 F3A 94.4(10) . . ? F2 B1 F3A 103.6(11) . . ? F3B B1 F4B 107.5(13) . . ? F1 B1 F4B 88.5(12) . . ? F2 B1 F4B 113.7(11) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.92 _refine_diff_density_min -0.64 _refine_diff_density_rms 0.17 # === END of CIF