# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email DOMINIQUE.LORCY@UNIV-RENNES1.FR _publ_contact_author_name 'Prof Lorcy Dominique' _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_address ; Institut de Chimie Universite de Rennes 1 Campus de Beaulieu Bat 10 A Rennes 35042 FRANCE ; _publ_section_title ; Unprecedented metal template effect on the coupling of dithiafulvene moieties ; _publ_requested_category FM loop_ _publ_author_name 'Lorcy Dominique' 'Roger Carlier' 'Michel Guerro' 'Pascal Pellon' data_compound5b _database_code_depnum_ccdc_archive 'CCDC 215143' _audit_creation_date 2003-07-11T12:04:33-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C40 H34 Mo1 O4 P2 S4' _chemical_formula_sum 'C40 H34 Mo O4 P2 S4' _chemical_formula_weight 864.79 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c c n' _symmetry_space_group_name_Hall '-P 2ab 2ac' _symmetry_Int_Tables_number 56 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x-1/2, y, z-1/2' 'x, -y-1/2, z-1/2' _cell_length_a 10.52900(10) _cell_length_b 18.2873(2) _cell_length_c 20.6979(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3985.32(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 23783 _cell_measurement_theta_min 2.546 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.6 _exptl_crystal_size_min 0.4 _exptl_crystal_density_diffrn 1.441 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1768 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.32 -1 0 0 0.28 0 1 0 0.32 0 -1 0 0.33 0 0 1 0.2 0 0 -1 0.18 4 -3 -5 0.221 -13 10 -1 0.274 -1 1 -8 0.168 4 -3 0 0.291 1 2 0 0.32 -1 -2 0 0.3 1 14 15 0.273 0 -4 -5 0.235 -3 -4 1 0.268 -1 2 6 0.267 2 -3 -7 0.191 2 1 -4 0.272 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.658 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.6934 _exptl_absorpt_correction_T_max 0.7787 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.91034E-2 _diffrn_orient_matrix_ub_12 0.348779E-1 _diffrn_orient_matrix_ub_13 -0.369767E-1 _diffrn_orient_matrix_ub_21 -0.825228E-1 _diffrn_orient_matrix_ub_22 -0.234801E-1 _diffrn_orient_matrix_ub_23 -0.12027E-1 _diffrn_orient_matrix_ub_31 -0.462363E-1 _diffrn_orient_matrix_ub_32 0.350403E-1 _diffrn_orient_matrix_ub_33 0.287462E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0388 _diffrn_reflns_av_unetI/netI 0.0322 _diffrn_reflns_number 26818 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.971 _diffrn_measured_fraction_theta_max 0.971 _reflns_number_total 4470 _reflns_number_gt 3077 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0226P)^2^+4.4458P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 4470 _refine_ls_number_parameters 231 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0706 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0857 _refine_ls_wR_factor_gt 0.0713 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.451 _refine_diff_density_min -0.384 _refine_diff_density_rms 0.065 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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 0.75 0.25 0.445872(14) 0.03262(10) Uani 1 2 d S . . C102 C 0.7956(3) 0.31772(17) 0.51617(14) 0.0507(8) Uani 1 1 d . . . O2 O 0.8139(3) 0.35572(14) 0.55951(12) 0.0856(9) Uani 1 1 d . . . C101 C 0.5771(3) 0.29935(17) 0.45226(15) 0.0476(7) Uani 1 1 d . . . O1 O 0.4834(2) 0.32871(15) 0.46259(14) 0.0792(8) Uani 1 1 d . . . P1 P 0.68259(7) 0.15012(4) 0.36512(3) 0.03570(17) Uani 1 1 d . . . C31 C 0.7930(3) 0.07207(15) 0.36706(13) 0.0387(6) Uani 1 1 d . . . C36 C 0.7972(3) 0.03091(18) 0.42270(17) 0.0593(9) Uani 1 1 d . . . H36 H 0.7408 0.0415 0.456 0.071 Uiso 1 1 calc R . . C35 C 0.8832(4) -0.02587(19) 0.43044(19) 0.0677(10) Uani 1 1 d . . . H35 H 0.8857 -0.0516 0.4692 0.081 Uiso 1 1 calc R . . C34 C 0.9631(3) -0.0440(2) 0.3821(2) 0.0672(10) Uani 1 1 d . . . H34 H 1.0194 -0.0828 0.3867 0.081 Uiso 1 1 calc R . . C33 C 0.9598(4) -0.0044(3) 0.3264(2) 0.0837(13) Uani 1 1 d . . . H33 H 1.015 -0.0164 0.2929 0.1 Uiso 1 1 calc R . . C32 C 0.8757(3) 0.0536(2) 0.31844(16) 0.0642(10) Uani 1 1 d . . . H32 H 0.8754 0.0799 0.28 0.077 Uiso 1 1 calc R . . C21 C 0.5315(3) 0.10330(16) 0.38347(13) 0.0401(7) Uani 1 1 d . . . C26 C 0.4441(3) 0.1329(2) 0.42510(17) 0.0606(9) Uani 1 1 d . . . H26 H 0.4622 0.1767 0.4461 0.073 Uiso 1 1 calc R . . C25 C 0.3284(3) 0.0980(2) 0.4363(2) 0.0749(11) Uani 1 1 d . . . H25 H 0.2691 0.119 0.4639 0.09 Uiso 1 1 calc R . . C24 C 0.3023(4) 0.0335(2) 0.40688(19) 0.0691(11) Uani 1 1 d . . . H24 H 0.2257 0.0099 0.4149 0.083 Uiso 1 1 calc R . . C23 C 0.3884(4) 0.0031(2) 0.36538(17) 0.0685(11) Uani 1 1 d . . . H23 H 0.37 -0.0411 0.3452 0.082 Uiso 1 1 calc R . . C22 C 0.5022(3) 0.03745(18) 0.35326(15) 0.0573(9) Uani 1 1 d . . . H22 H 0.5598 0.0165 0.3247 0.069 Uiso 1 1 calc R . . C1 C 0.6642(3) 0.16893(16) 0.27981(13) 0.0425(7) Uani 1 1 d . . . H1 H 0.7161 0.1438 0.251 0.051 Uiso 1 1 calc R . . C2 C 0.5814(3) 0.21635(16) 0.25560(13) 0.0426(7) Uani 1 1 d . . . C4 C 0.4412(3) 0.29787(18) 0.17787(15) 0.0537(8) Uani 1 1 d . . . C6 C 0.3882(4) 0.3266(2) 0.11516(18) 0.0795(12) Uani 1 1 d . . . H6C H 0.4363 0.3071 0.0797 0.119 Uiso 1 1 calc R . . H6B H 0.3933 0.379 0.1148 0.119 Uiso 1 1 calc R . . H6A H 0.301 0.3118 0.111 0.119 Uiso 1 1 calc R . . C3 C 0.3986(3) 0.3129(2) 0.23632(17) 0.0605(9) Uani 1 1 d . . . C5 C 0.2914(4) 0.3635(2) 0.2544(2) 0.0912(14) Uani 1 1 d . . . H5A H 0.2817 0.3641 0.3006 0.137 Uiso 1 1 calc R . . H5B H 0.2141 0.3467 0.2348 0.137 Uiso 1 1 calc R . . H5C H 0.31 0.412 0.2395 0.137 Uiso 1 1 calc R . . S3 S 0.56975(9) 0.23698(5) 0.17306(4) 0.0582(2) Uani 1 1 d . . . S4 S 0.47461(10) 0.26854(5) 0.30131(4) 0.0667(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.03657(17) 0.03005(18) 0.03125(15) 0 0 -0.00038(16) C102 0.069(2) 0.0397(17) 0.0434(16) 0.0039(14) -0.0104(15) -0.0013(15) O2 0.139(3) 0.0605(17) 0.0574(15) -0.0161(13) -0.0311(16) -0.0048(17) C101 0.0501(18) 0.0407(18) 0.0521(17) -0.0080(14) -0.0007(15) -0.0013(15) O1 0.0515(14) 0.0774(19) 0.109(2) -0.0245(16) 0.0085(15) 0.0204(14) P1 0.0396(4) 0.0331(4) 0.0344(3) -0.0006(3) 0.0033(3) -0.0026(3) C31 0.0435(16) 0.0325(15) 0.0401(14) -0.0063(12) 0.0000(12) -0.0017(12) C36 0.071(2) 0.048(2) 0.0588(19) 0.0074(16) 0.0133(17) 0.0175(17) C35 0.072(2) 0.049(2) 0.082(3) 0.0096(18) 0.000(2) 0.0137(19) C34 0.056(2) 0.050(2) 0.096(3) -0.013(2) -0.007(2) 0.0141(18) C33 0.076(3) 0.100(3) 0.075(3) -0.016(2) 0.018(2) 0.036(3) C32 0.066(2) 0.075(3) 0.0520(19) 0.0015(17) 0.0100(17) 0.019(2) C21 0.0421(16) 0.0395(17) 0.0387(14) 0.0056(12) -0.0016(12) -0.0042(13) C26 0.052(2) 0.056(2) 0.074(2) -0.0119(17) 0.0151(18) -0.0139(17) C25 0.053(2) 0.081(3) 0.091(3) -0.006(2) 0.023(2) -0.019(2) C24 0.057(2) 0.081(3) 0.070(2) 0.016(2) -0.003(2) -0.030(2) C23 0.082(3) 0.061(2) 0.063(2) 0.0000(18) -0.008(2) -0.033(2) C22 0.066(2) 0.052(2) 0.0530(19) -0.0055(15) 0.0033(17) -0.0175(17) C1 0.0510(18) 0.0407(17) 0.0360(14) -0.0013(12) 0.0053(13) -0.0061(14) C2 0.0489(17) 0.0418(16) 0.0370(14) 0.0016(12) -0.0019(13) -0.0105(14) C4 0.058(2) 0.051(2) 0.0521(18) 0.0106(15) -0.0096(16) -0.0082(16) C6 0.079(3) 0.092(3) 0.068(2) 0.030(2) -0.017(2) -0.002(2) C3 0.056(2) 0.064(2) 0.062(2) 0.0107(17) -0.0065(17) 0.0058(18) C5 0.084(3) 0.097(3) 0.093(3) 0.015(3) -0.001(2) 0.033(3) S3 0.0716(5) 0.0650(6) 0.0380(4) 0.0077(4) -0.0013(4) 0.0048(4) S4 0.0767(6) 0.0793(7) 0.0440(4) 0.0013(4) 0.0005(4) 0.0252(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C102 1.970(3) . ? Mo1 C102 1.970(3) 2_655 ? Mo1 C101 2.036(3) 2_655 ? Mo1 C101 2.036(3) . ? Mo1 P1 2.5756(7) . ? Mo1 P1 2.5756(7) 2_655 ? C102 O2 1.151(4) . ? C101 O1 1.143(4) . ? P1 C1 1.809(3) . ? P1 C31 1.842(3) . ? P1 C21 1.846(3) . ? C31 C32 1.373(4) . ? C31 C36 1.376(4) . ? C36 C35 1.387(5) . ? C36 H36 0.93 . ? C35 C34 1.349(5) . ? C35 H35 0.93 . ? C34 C33 1.361(5) . ? C34 H34 0.93 . ? C33 C32 1.391(5) . ? C33 H33 0.93 . ? C32 H32 0.93 . ? C21 C26 1.372(4) . ? C21 C22 1.392(4) . ? C26 C25 1.395(5) . ? C26 H26 0.93 . ? C25 C24 1.355(5) . ? C25 H25 0.93 . ? C24 C23 1.367(5) . ? C24 H24 0.93 . ? C23 C22 1.375(5) . ? C23 H23 0.93 . ? C22 H22 0.93 . ? C1 C2 1.328(4) . ? C1 H1 0.93 . ? C2 S4 1.752(3) . ? C2 S3 1.754(3) . ? C4 C3 1.319(5) . ? C4 C6 1.507(4) . ? C4 S3 1.755(4) . ? C6 H6C 0.96 . ? C6 H6B 0.96 . ? C6 H6A 0.96 . ? C3 C5 1.507(5) . ? C3 S4 1.763(3) . ? C5 H5A 0.96 . ? C5 H5B 0.96 . ? C5 H5C 0.96 . ? 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 C102 Mo1 C102 84.78(18) . 2_655 ? C102 Mo1 C101 90.74(13) . 2_655 ? C102 Mo1 C101 83.75(13) 2_655 2_655 ? C102 Mo1 C101 83.75(13) . . ? C102 Mo1 C101 90.74(13) 2_655 . ? C101 Mo1 C101 172.55(17) 2_655 . ? C102 Mo1 P1 172.85(9) . . ? C102 Mo1 P1 88.07(9) 2_655 . ? C101 Mo1 P1 88.52(9) 2_655 . ? C101 Mo1 P1 96.32(8) . . ? C102 Mo1 P1 88.07(9) . 2_655 ? C102 Mo1 P1 172.85(9) 2_655 2_655 ? C101 Mo1 P1 96.32(8) 2_655 2_655 ? C101 Mo1 P1 88.52(9) . 2_655 ? P1 Mo1 P1 99.08(3) . 2_655 ? O2 C102 Mo1 174.9(3) . . ? O1 C101 Mo1 172.6(3) . . ? C1 P1 C31 103.66(13) . . ? C1 P1 C21 101.34(13) . . ? C31 P1 C21 100.39(13) . . ? C1 P1 Mo1 121.87(10) . . ? C31 P1 Mo1 111.19(9) . . ? C21 P1 Mo1 115.65(9) . . ? C32 C31 C36 117.3(3) . . ? C32 C31 P1 125.1(2) . . ? C36 C31 P1 117.5(2) . . ? C31 C36 C35 121.8(3) . . ? C31 C36 H36 119.1 . . ? C35 C36 H36 119.1 . . ? C34 C35 C36 120.3(4) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C35 C34 C33 118.8(3) . . ? C35 C34 H34 120.6 . . ? C33 C34 H34 120.6 . . ? C34 C33 C32 121.4(4) . . ? C34 C33 H33 119.3 . . ? C32 C33 H33 119.3 . . ? C31 C32 C33 120.3(3) . . ? C31 C32 H32 119.8 . . ? C33 C32 H32 119.8 . . ? C26 C21 C22 118.4(3) . . ? C26 C21 P1 121.6(2) . . ? C22 C21 P1 120.0(2) . . ? C21 C26 C25 120.6(3) . . ? C21 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C24 C25 C26 120.1(4) . . ? C24 C25 H25 120 . . ? C26 C25 H25 120 . . ? C25 C24 C23 120.1(3) . . ? C25 C24 H24 120 . . ? C23 C24 H24 120 . . ? C24 C23 C22 120.4(3) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C22 C21 120.4(3) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C2 C1 P1 124.2(2) . . ? C2 C1 H1 117.9 . . ? P1 C1 H1 117.9 . . ? C1 C2 S4 125.0(2) . . ? C1 C2 S3 123.6(2) . . ? S4 C2 S3 111.36(17) . . ? C3 C4 C6 126.2(3) . . ? C3 C4 S3 116.5(2) . . ? C6 C4 S3 117.2(3) . . ? C4 C6 H6C 109.5 . . ? C4 C6 H6B 109.5 . . ? H6C C6 H6B 109.5 . . ? C4 C6 H6A 109.5 . . ? H6C C6 H6A 109.5 . . ? H6B C6 H6A 109.5 . . ? C4 C3 C5 127.7(3) . . ? C4 C3 S4 116.7(3) . . ? C5 C3 S4 115.7(3) . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C2 S3 C4 97.75(15) . . ? C2 S4 C3 97.47(16) . . ? 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 C102 Mo1 C102 O2 -44(3) 2_655 . . . ? C101 Mo1 C102 O2 -127(3) 2_655 . . . ? C101 Mo1 C102 O2 48(3) . . . . ? P1 Mo1 C102 O2 -43(4) . . . . ? P1 Mo1 C102 O2 136(3) 2_655 . . . ? C102 Mo1 C101 O1 -26(2) . . . . ? C102 Mo1 C101 O1 59(2) 2_655 . . . ? C101 Mo1 C101 O1 17(2) 2_655 . . . ? P1 Mo1 C101 O1 147(2) . . . . ? P1 Mo1 C101 O1 -114(2) 2_655 . . . ? C102 Mo1 P1 C1 168.3(8) . . . . ? C102 Mo1 P1 C1 168.58(15) 2_655 . . . ? C101 Mo1 P1 C1 -107.62(15) 2_655 . . . ? C101 Mo1 P1 C1 78.06(15) . . . . ? P1 Mo1 P1 C1 -11.45(12) 2_655 . . . ? C102 Mo1 P1 C31 -69.1(8) . . . . ? C102 Mo1 P1 C31 -68.78(14) 2_655 . . . ? C101 Mo1 P1 C31 15.02(13) 2_655 . . . ? C101 Mo1 P1 C31 -159.30(13) . . . . ? P1 Mo1 P1 C31 111.19(10) 2_655 . . . ? C102 Mo1 P1 C21 44.5(8) . . . . ? C102 Mo1 P1 C21 44.85(14) 2_655 . . . ? C101 Mo1 P1 C21 128.64(13) 2_655 . . . ? C101 Mo1 P1 C21 -45.68(13) . . . . ? P1 Mo1 P1 C21 -135.19(10) 2_655 . . . ? C1 P1 C31 C32 22.0(3) . . . . ? C21 P1 C31 C32 126.5(3) . . . . ? Mo1 P1 C31 C32 -110.6(3) . . . . ? C1 P1 C31 C36 -161.0(3) . . . . ? C21 P1 C31 C36 -56.5(3) . . . . ? Mo1 P1 C31 C36 66.4(3) . . . . ? C32 C31 C36 C35 1.6(5) . . . . ? P1 C31 C36 C35 -175.6(3) . . . . ? C31 C36 C35 C34 -2.3(6) . . . . ? C36 C35 C34 C33 1.6(6) . . . . ? C35 C34 C33 C32 -0.4(7) . . . . ? C36 C31 C32 C33 -0.4(5) . . . . ? P1 C31 C32 C33 176.6(3) . . . . ? C34 C33 C32 C31 -0.2(6) . . . . ? C1 P1 C21 C26 -115.8(3) . . . . ? C31 P1 C21 C26 137.9(3) . . . . ? Mo1 P1 C21 C26 18.1(3) . . . . ? C1 P1 C21 C22 62.2(3) . . . . ? C31 P1 C21 C22 -44.2(3) . . . . ? Mo1 P1 C21 C22 -163.9(2) . . . . ? C22 C21 C26 C25 -0.6(5) . . . . ? P1 C21 C26 C25 177.4(3) . . . . ? C21 C26 C25 C24 1.3(6) . . . . ? C26 C25 C24 C23 -1.1(6) . . . . ? C25 C24 C23 C22 0.2(6) . . . . ? C24 C23 C22 C21 0.5(5) . . . . ? C26 C21 C22 C23 -0.3(5) . . . . ? P1 C21 C22 C23 -178.4(3) . . . . ? C31 P1 C1 C2 172.3(3) . . . . ? C21 P1 C1 C2 68.6(3) . . . . ? Mo1 P1 C1 C2 -61.6(3) . . . . ? P1 C1 C2 S4 -0.5(4) . . . . ? P1 C1 C2 S3 176.98(16) . . . . ? C6 C4 C3 C5 -2.3(6) . . . . ? S3 C4 C3 C5 179.3(3) . . . . ? C6 C4 C3 S4 177.3(3) . . . . ? S3 C4 C3 S4 -1.1(4) . . . . ? C1 C2 S3 C4 177.7(3) . . . . ? S4 C2 S3 C4 -4.52(19) . . . . ? C3 C4 S3 C2 3.5(3) . . . . ? C6 C4 S3 C2 -175.1(3) . . . . ? C1 C2 S4 C3 -178.2(3) . . . . ? S3 C2 S4 C3 4.0(2) . . . . ? C4 C3 S4 C2 -1.9(3) . . . . ? C5 C3 S4 C2 177.8(3) . . . . ? data_compound5a _database_code_depnum_ccdc_archive 'CCDC 215144' _audit_creation_date 2003-07-11T12:07:51-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C40 H34 Mo1 O4 P2 S4' _chemical_formula_sum 'C40 H34 Mo O4 P2 S4' _chemical_formula_weight 864.79 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.3608(5) _cell_length_b 19.7947(4) _cell_length_c 19.4065(5) _cell_angle_alpha 90 _cell_angle_beta 116.3260(10) _cell_angle_gamma 90 _cell_volume 8043.2(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9072 _cell_measurement_theta_min 2.396 _cell_measurement_theta_max 27.103 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.428 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3536 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.06 -1 0 0 0.08 0 1 0 0.09 0 -1 0 0.08 0 0 1 0.06 0 0 -1 0.06 -1 -5 5 0.077 1 5 3 0.059 -1 -5 -14 0.061 3 13 -12 0.057 -3 0 2 0.041 3 0 -2 0.012 5 -4 -4 0.043 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.652 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9142 _exptl_absorpt_correction_T_max 0.9681 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.161403E-1 _diffrn_orient_matrix_ub_12 -0.47263E-1 _diffrn_orient_matrix_ub_13 0.33294E-2 _diffrn_orient_matrix_ub_21 0.284964E-1 _diffrn_orient_matrix_ub_22 0.64997E-2 _diffrn_orient_matrix_ub_23 0.560293E-1 _diffrn_orient_matrix_ub_31 -0.347629E-1 _diffrn_orient_matrix_ub_32 -0.16616E-1 _diffrn_orient_matrix_ub_33 0.124469E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0542 _diffrn_reflns_av_unetI/netI 0.0794 _diffrn_reflns_number 17403 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 27.1 _diffrn_reflns_theta_full 27.1 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 8861 _reflns_number_gt 5247 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0628P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.00031(7) _refine_ls_number_reflns 8861 _refine_ls_number_parameters 461 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1026 _refine_ls_R_factor_gt 0.048 _refine_ls_wR_factor_ref 0.1365 _refine_ls_wR_factor_gt 0.1114 _refine_ls_goodness_of_fit_ref 0.99 _refine_ls_restrained_S_all 0.99 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.469 _refine_diff_density_min -0.536 _refine_diff_density_rms 0.073 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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 0.708219(18) -0.307952(15) 0.11554(2) 0.04264(13) Uani 1 1 d . . . C101 C 0.7034(2) -0.4093(2) 0.1165(2) 0.0507(10) Uani 1 1 d . . . O1 O 0.70164(19) -0.46698(15) 0.1114(2) 0.0799(11) Uani 1 1 d . . . C102 C 0.6604(3) -0.3136(2) 0.0021(3) 0.0618(12) Uani 1 1 d . . . O2 O 0.6334(2) -0.32002(18) -0.0642(2) 0.0945(13) Uani 1 1 d . . . C103 C 0.7887(3) -0.3159(2) 0.1065(3) 0.0581(12) Uani 1 1 d . . . O3 O 0.8361(2) -0.31980(18) 0.1009(2) 0.0839(11) Uani 1 1 d . . . C104 C 0.7182(2) -0.2063(2) 0.1041(3) 0.0553(11) Uani 1 1 d . . . O4 O 0.7256(2) -0.15113(15) 0.0936(2) 0.0849(11) Uani 1 1 d . . . C31 C 0.5858(2) -0.19492(18) 0.1110(3) 0.0489(10) Uani 1 1 d . . . C36 C 0.6084(2) -0.1499(2) 0.1730(3) 0.0576(12) Uani 1 1 d . . . H36 H 0.6281 -0.1663 0.2231 0.069 Uiso 1 1 calc R . . C35 C 0.6017(2) -0.0808(2) 0.1601(3) 0.0706(14) Uani 1 1 d . . . H35 H 0.6169 -0.0513 0.2017 0.085 Uiso 1 1 calc R . . C34 C 0.5726(3) -0.0557(2) 0.0864(4) 0.0752(15) Uani 1 1 d . . . H34 H 0.5687 -0.0093 0.0781 0.09 Uiso 1 1 calc R . . C33 C 0.5492(3) -0.0995(2) 0.0250(3) 0.0744(15) Uani 1 1 d . . . H33 H 0.5286 -0.0827 -0.0248 0.089 Uiso 1 1 calc R . . C32 C 0.5561(2) -0.1685(2) 0.0372(3) 0.0604(12) Uani 1 1 d . . . H32 H 0.5406 -0.1977 -0.0047 0.072 Uiso 1 1 calc R . . C21 C 0.5311(2) -0.32560(19) 0.0530(2) 0.0464(10) Uani 1 1 d . . . C22 C 0.5348(2) -0.38159(19) 0.0122(2) 0.0525(11) Uani 1 1 d . . . H22 H 0.5744 -0.397 0.0184 0.063 Uiso 1 1 calc R . . C23 C 0.4799(2) -0.4146(2) -0.0376(3) 0.0627(13) Uani 1 1 d . . . H23 H 0.4828 -0.4522 -0.0647 0.075 Uiso 1 1 calc R . . C24 C 0.4214(2) -0.3923(2) -0.0474(3) 0.0636(13) Uani 1 1 d . . . H24 H 0.3846 -0.4149 -0.081 0.076 Uiso 1 1 calc R . . C25 C 0.4168(2) -0.3371(2) -0.0080(3) 0.0646(13) Uani 1 1 d . . . H25 H 0.3769 -0.3216 -0.0154 0.078 Uiso 1 1 calc R . . C26 C 0.4714(2) -0.3041(2) 0.0429(3) 0.0591(12) Uani 1 1 d . . . H26 H 0.4681 -0.2672 0.0706 0.071 Uiso 1 1 calc R . . C1 C 0.5990(2) -0.30260(19) 0.2128(2) 0.0491(10) Uani 1 1 d . . . H1 H 0.5987 -0.2653 0.2418 0.059 Uiso 1 1 calc R . . C2 C 0.5953(2) -0.36348(19) 0.2412(2) 0.0480(10) Uani 1 1 d . . . C4 C 0.5994(2) -0.4619(2) 0.3340(3) 0.0611(12) Uani 1 1 d . . . C6 C 0.6059(3) -0.4947(3) 0.4070(3) 0.0897(19) Uani 1 1 d . . . H6C H 0.6058 -0.4607 0.4421 0.135 Uiso 1 1 calc R . . H6B H 0.6453 -0.5195 0.4299 0.135 Uiso 1 1 calc R . . H6A H 0.5707 -0.525 0.3955 0.135 Uiso 1 1 calc R . . C3 C 0.5984(3) -0.4932(2) 0.2729(3) 0.0668(13) Uani 1 1 d . . . C5 C 0.6027(4) -0.5673(3) 0.2612(4) 0.116(3) Uani 1 1 d . . . H5A H 0.6003 -0.5751 0.2112 0.174 Uiso 1 1 calc R . . H5B H 0.568 -0.5901 0.2652 0.174 Uiso 1 1 calc R . . H5C H 0.6425 -0.5844 0.2997 0.174 Uiso 1 1 calc R . . S2 S 0.59501(7) -0.37388(6) 0.33056(7) 0.0673(4) Uani 1 1 d . . . S1 S 0.59062(7) -0.44104(5) 0.19526(7) 0.0602(3) Uani 1 1 d . . . P1 P 0.60425(5) -0.28550(5) 0.12498(6) 0.0430(3) Uani 1 1 d . . . P2 P 0.77211(5) -0.30852(5) 0.26124(6) 0.0442(3) Uani 1 1 d . . . C51 C 0.8589(2) -0.3100(2) 0.2928(2) 0.0490(10) Uani 1 1 d . . . C52 C 0.8863(2) -0.3712(2) 0.2845(3) 0.0621(12) Uani 1 1 d . . . H52 H 0.8606 -0.4091 0.2654 0.074 Uiso 1 1 calc R . . C53 C 0.9502(3) -0.3754(3) 0.3042(3) 0.0797(16) Uani 1 1 d . . . H53 H 0.9677 -0.4163 0.2997 0.096 Uiso 1 1 calc R . . C54 C 0.9885(3) -0.3192(4) 0.3305(3) 0.0826(17) Uani 1 1 d . . . H54 H 1.0317 -0.3223 0.3432 0.099 Uiso 1 1 calc R . . C55 C 0.9630(2) -0.2587(3) 0.3380(3) 0.0741(15) Uani 1 1 d . . . H55 H 0.9888 -0.2206 0.3548 0.089 Uiso 1 1 calc R . . C56 C 0.8994(2) -0.2550(2) 0.3206(3) 0.0625(12) Uani 1 1 d . . . H56 H 0.8829 -0.2142 0.3277 0.075 Uiso 1 1 calc R . . C41 C 0.7591(2) -0.23689(19) 0.3133(2) 0.0502(10) Uani 1 1 d . . . C46 C 0.7671(2) -0.1720(2) 0.2920(3) 0.0589(12) Uani 1 1 d . . . H46 H 0.7801 -0.1658 0.2536 0.071 Uiso 1 1 calc R . . C45 C 0.7558(3) -0.1157(2) 0.3280(4) 0.0776(17) Uani 1 1 d . . . H45 H 0.7616 -0.0723 0.3139 0.093 Uiso 1 1 calc R . . C44 C 0.7361(3) -0.1250(3) 0.3839(4) 0.0816(17) Uani 1 1 d . . . H44 H 0.7294 -0.0877 0.4086 0.098 Uiso 1 1 calc R . . C43 C 0.7261(3) -0.1883(3) 0.4038(3) 0.0771(16) Uani 1 1 d . . . H43 H 0.7117 -0.194 0.441 0.092 Uiso 1 1 calc R . . C42 C 0.7375(2) -0.2449(2) 0.3684(3) 0.0624(12) Uani 1 1 d . . . H42 H 0.7306 -0.2881 0.3822 0.075 Uiso 1 1 calc R . . C11 C 0.7612(2) -0.3820(2) 0.3086(3) 0.0523(11) Uani 1 1 d . . . H11 H 0.727 -0.4096 0.2784 0.063 Uiso 1 1 calc R . . C12 C 0.7954(2) -0.4026(2) 0.3812(3) 0.0541(11) Uani 1 1 d . . . C13 C 0.8384(3) -0.4709(2) 0.5089(3) 0.0698(14) Uani 1 1 d . . . C15 C 0.8426(3) -0.5275(3) 0.5637(4) 0.105(2) Uani 1 1 d . . . H15A H 0.811 -0.5613 0.5365 0.158 Uiso 1 1 calc R . . H15B H 0.8349 -0.5097 0.6049 0.158 Uiso 1 1 calc R . . H15C H 0.8843 -0.5475 0.5844 0.158 Uiso 1 1 calc R . . C14 C 0.8751(2) -0.4156(3) 0.5268(3) 0.0661(13) Uani 1 1 d . . . C16 C 0.9273(3) -0.3958(3) 0.6040(3) 0.096(2) Uani 1 1 d . . . H16C H 0.9455 -0.3535 0.5995 0.144 Uiso 1 1 calc R . . H16B H 0.9599 -0.4299 0.6214 0.144 Uiso 1 1 calc R . . H16A H 0.9099 -0.3913 0.6402 0.144 Uiso 1 1 calc R . . S3 S 0.77972(7) -0.47827(6) 0.41512(9) 0.0747(4) Uani 1 1 d . . . S4 S 0.86130(6) -0.35966(6) 0.45149(7) 0.0651(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0496(2) 0.03226(17) 0.0453(2) -0.00160(13) 0.02036(16) 0.00024(15) C101 0.057(3) 0.043(2) 0.055(3) -0.0002(18) 0.027(2) 0.0060(19) O1 0.108(3) 0.0387(17) 0.099(3) 0.0003(16) 0.051(2) 0.0074(18) C102 0.076(4) 0.046(2) 0.068(3) 0.000(2) 0.036(3) -0.008(2) O2 0.130(4) 0.090(3) 0.049(2) -0.0067(18) 0.027(2) -0.026(2) C103 0.067(3) 0.052(2) 0.065(3) -0.006(2) 0.038(3) -0.004(2) O3 0.085(3) 0.079(2) 0.109(3) -0.001(2) 0.064(3) 0.001(2) C104 0.058(3) 0.046(2) 0.059(3) -0.0046(19) 0.024(2) -0.001(2) O4 0.114(3) 0.0422(17) 0.097(3) 0.0050(17) 0.046(3) -0.0116(19) C31 0.048(3) 0.0368(19) 0.058(3) 0.0023(18) 0.020(2) 0.0023(18) C36 0.048(3) 0.047(2) 0.065(3) -0.004(2) 0.013(2) -0.0001(19) C35 0.066(3) 0.045(2) 0.095(4) -0.011(2) 0.030(3) -0.003(2) C34 0.071(4) 0.039(2) 0.112(5) 0.014(3) 0.037(3) 0.012(2) C33 0.086(4) 0.051(3) 0.085(4) 0.021(3) 0.037(3) 0.014(3) C32 0.075(3) 0.046(2) 0.057(3) 0.0049(19) 0.026(3) 0.006(2) C21 0.048(3) 0.045(2) 0.040(2) 0.0039(16) 0.0147(19) 0.0010(18) C22 0.053(3) 0.043(2) 0.050(3) -0.0040(17) 0.012(2) 0.0002(19) C23 0.061(3) 0.059(3) 0.055(3) -0.008(2) 0.013(2) -0.007(2) C24 0.056(3) 0.060(3) 0.056(3) -0.001(2) 0.007(2) -0.014(2) C25 0.045(3) 0.073(3) 0.070(3) 0.011(2) 0.020(3) 0.001(2) C26 0.057(3) 0.059(3) 0.059(3) 0.000(2) 0.024(2) -0.001(2) C1 0.052(3) 0.043(2) 0.050(2) -0.0011(17) 0.020(2) 0.0031(19) C2 0.048(3) 0.053(2) 0.043(2) -0.0017(17) 0.020(2) 0.0006(19) C4 0.070(3) 0.058(3) 0.058(3) 0.007(2) 0.032(3) -0.002(2) C6 0.132(6) 0.082(4) 0.077(4) 0.021(3) 0.066(4) 0.007(4) C3 0.089(4) 0.052(2) 0.067(3) 0.004(2) 0.041(3) -0.005(2) C5 0.214(9) 0.056(3) 0.100(5) 0.011(3) 0.090(6) 0.011(4) S2 0.0965(11) 0.0605(7) 0.0573(7) 0.0013(5) 0.0453(7) 0.0031(7) S1 0.0845(9) 0.0466(6) 0.0520(7) -0.0025(5) 0.0326(6) -0.0070(6) P1 0.0460(6) 0.0353(5) 0.0434(6) -0.0006(4) 0.0160(5) 0.0013(4) P2 0.0427(6) 0.0387(5) 0.0484(6) -0.0040(4) 0.0177(5) -0.0008(4) C51 0.046(2) 0.057(2) 0.043(2) 0.0014(18) 0.0178(19) 0.004(2) C52 0.054(3) 0.063(3) 0.072(3) 0.001(2) 0.030(3) 0.007(2) C53 0.074(4) 0.095(4) 0.076(4) 0.012(3) 0.039(3) 0.019(3) C54 0.041(3) 0.145(6) 0.057(3) 0.001(3) 0.018(3) 0.004(3) C55 0.043(3) 0.098(4) 0.073(4) -0.015(3) 0.017(3) -0.017(3) C56 0.057(3) 0.065(3) 0.063(3) -0.007(2) 0.025(3) -0.006(2) C41 0.043(2) 0.045(2) 0.049(2) -0.0091(17) 0.008(2) 0.0007(18) C46 0.052(3) 0.049(2) 0.062(3) -0.012(2) 0.013(2) -0.003(2) C45 0.061(3) 0.048(3) 0.099(4) -0.023(3) 0.014(3) 0.000(2) C44 0.069(4) 0.070(3) 0.092(4) -0.038(3) 0.023(3) 0.008(3) C43 0.058(3) 0.099(4) 0.071(3) -0.022(3) 0.025(3) 0.012(3) C42 0.057(3) 0.065(3) 0.066(3) -0.008(2) 0.028(3) 0.007(2) C11 0.045(3) 0.045(2) 0.066(3) -0.0011(19) 0.024(2) -0.0013(19) C12 0.052(3) 0.045(2) 0.065(3) 0.0037(19) 0.025(2) 0.004(2) C13 0.075(4) 0.066(3) 0.082(4) 0.022(3) 0.047(3) 0.020(3) C15 0.131(6) 0.086(4) 0.127(6) 0.051(4) 0.081(5) 0.024(4) C14 0.057(3) 0.081(3) 0.063(3) 0.018(2) 0.028(3) 0.012(3) C16 0.082(5) 0.130(5) 0.071(4) 0.027(3) 0.029(3) 0.007(4) S3 0.0840(10) 0.0524(6) 0.0904(10) 0.0127(6) 0.0411(8) -0.0065(6) S4 0.0577(8) 0.0675(7) 0.0608(7) 0.0132(6) 0.0177(6) -0.0079(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C103 1.971(5) . ? Mo1 C102 1.982(5) . ? Mo1 C101 2.009(4) . ? Mo1 C104 2.049(4) . ? Mo1 P2 2.5456(11) . ? Mo1 P1 2.5543(12) . ? C101 O1 1.146(5) . ? C102 O2 1.161(6) . ? C103 O3 1.162(6) . ? C104 O4 1.138(5) . ? C31 C32 1.387(6) . ? C31 C36 1.399(6) . ? C31 P1 1.836(4) . ? C36 C35 1.385(6) . ? C36 H36 0.93 . ? C35 C34 1.377(7) . ? C35 H35 0.93 . ? C34 C33 1.375(7) . ? C34 H34 0.93 . ? C33 C32 1.384(6) . ? C33 H33 0.93 . ? C32 H32 0.93 . ? C21 C26 1.386(6) . ? C21 C22 1.387(5) . ? C21 P1 1.840(4) . ? C22 C23 1.380(6) . ? C22 H22 0.93 . ? C23 C24 1.368(7) . ? C23 H23 0.93 . ? C24 C25 1.366(7) . ? C24 H24 0.93 . ? C25 C26 1.384(6) . ? C25 H25 0.93 . ? C26 H26 0.93 . ? C1 C2 1.343(5) . ? C1 P1 1.795(4) . ? C1 H1 0.93 . ? C2 S2 1.750(4) . ? C2 S1 1.754(4) . ? C4 C3 1.330(6) . ? C4 C6 1.503(6) . ? C4 S2 1.744(4) . ? C6 H6C 0.96 . ? C6 H6B 0.96 . ? C6 H6A 0.96 . ? C3 C5 1.495(7) . ? C3 S1 1.768(5) . ? C5 H5A 0.96 . ? C5 H5B 0.96 . ? C5 H5C 0.96 . ? P2 C11 1.798(4) . ? P2 C51 1.839(4) . ? P2 C41 1.843(4) . ? C51 C56 1.385(6) . ? C51 C52 1.412(6) . ? C52 C53 1.369(7) . ? C52 H52 0.93 . ? C53 C54 1.375(8) . ? C53 H53 0.93 . ? C54 C55 1.373(8) . ? C54 H54 0.93 . ? C55 C56 1.373(7) . ? C55 H55 0.93 . ? C56 H56 0.93 . ? C41 C42 1.378(6) . ? C41 C46 1.388(6) . ? C46 C45 1.401(6) . ? C46 H46 0.93 . ? C45 C44 1.366(8) . ? C45 H45 0.93 . ? C44 C43 1.362(8) . ? C44 H44 0.93 . ? C43 C42 1.400(6) . ? C43 H43 0.93 . ? C42 H42 0.93 . ? C11 C12 1.338(6) . ? C11 H11 0.93 . ? C12 S3 1.740(4) . ? C12 S4 1.757(5) . ? C13 C14 1.337(7) . ? C13 C15 1.519(7) . ? C13 S3 1.733(6) . ? C15 H15A 0.96 . ? C15 H15B 0.96 . ? C15 H15C 0.96 . ? C14 C16 1.504(7) . ? C14 S4 1.746(5) . ? C16 H16C 0.96 . ? C16 H16B 0.96 . ? C16 H16A 0.96 . ? 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 C103 Mo1 C102 89.2(2) . . ? C103 Mo1 C101 88.87(17) . . ? C102 Mo1 C101 87.01(17) . . ? C103 Mo1 C104 84.84(18) . . ? C102 Mo1 C104 88.28(17) . . ? C101 Mo1 C104 172.20(18) . . ? C103 Mo1 P2 89.22(14) . . ? C102 Mo1 P2 176.27(13) . . ? C101 Mo1 P2 89.58(12) . . ? C104 Mo1 P2 94.94(13) . . ? C103 Mo1 P1 174.49(13) . . ? C102 Mo1 P1 90.25(15) . . ? C101 Mo1 P1 96.57(13) . . ? C104 Mo1 P1 89.66(13) . . ? P2 Mo1 P1 91.65(4) . . ? O1 C101 Mo1 173.9(4) . . ? O2 C102 Mo1 176.8(4) . . ? O3 C103 Mo1 179.2(4) . . ? O4 C104 Mo1 174.5(4) . . ? C32 C31 C36 118.2(4) . . ? C32 C31 P1 119.8(3) . . ? C36 C31 P1 121.4(3) . . ? C35 C36 C31 120.3(5) . . ? C35 C36 H36 119.9 . . ? C31 C36 H36 119.9 . . ? C34 C35 C36 120.6(5) . . ? C34 C35 H35 119.7 . . ? C36 C35 H35 119.7 . . ? C33 C34 C35 119.7(4) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? C34 C33 C32 120.2(5) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C33 C32 C31 121.0(5) . . ? C33 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C26 C21 C22 118.5(4) . . ? C26 C21 P1 120.8(3) . . ? C22 C21 P1 120.4(3) . . ? C23 C22 C21 120.4(4) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C24 C23 C22 120.3(4) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C25 C24 C23 120.2(4) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 120.1(5) . . ? C24 C25 H25 120 . . ? C26 C25 H25 120 . . ? C25 C26 C21 120.5(4) . . ? C25 C26 H26 119.8 . . ? C21 C26 H26 119.8 . . ? C2 C1 P1 127.0(3) . . ? C2 C1 H1 116.5 . . ? P1 C1 H1 116.5 . . ? C1 C2 S2 122.7(3) . . ? C1 C2 S1 125.3(3) . . ? S2 C2 S1 112.0(2) . . ? C3 C4 C6 126.3(5) . . ? C3 C4 S2 117.0(3) . . ? C6 C4 S2 116.6(4) . . ? C4 C6 H6C 109.5 . . ? C4 C6 H6B 109.5 . . ? H6C C6 H6B 109.5 . . ? C4 C6 H6A 109.5 . . ? H6C C6 H6A 109.5 . . ? H6B C6 H6A 109.5 . . ? C4 C3 C5 128.1(5) . . ? C4 C3 S1 116.3(4) . . ? C5 C3 S1 115.6(4) . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 S2 C2 97.5(2) . . ? C2 S1 C3 96.8(2) . . ? C1 P1 C31 102.32(19) . . ? C1 P1 C21 101.98(19) . . ? C31 P1 C21 103.36(18) . . ? C1 P1 Mo1 120.23(14) . . ? C31 P1 Mo1 109.16(15) . . ? C21 P1 Mo1 117.59(14) . . ? C11 P2 C51 101.65(19) . . ? C11 P2 C41 104.3(2) . . ? C51 P2 C41 104.81(19) . . ? C11 P2 Mo1 115.16(15) . . ? C51 P2 Mo1 112.73(14) . . ? C41 P2 Mo1 116.59(14) . . ? C56 C51 C52 116.9(4) . . ? C56 C51 P2 125.4(3) . . ? C52 C51 P2 117.7(3) . . ? C53 C52 C51 120.9(5) . . ? C53 C52 H52 119.5 . . ? C51 C52 H52 119.5 . . ? C52 C53 C54 120.2(5) . . ? C52 C53 H53 119.9 . . ? C54 C53 H53 119.9 . . ? C55 C54 C53 120.2(5) . . ? C55 C54 H54 119.9 . . ? C53 C54 H54 119.9 . . ? C56 C55 C54 119.5(5) . . ? C56 C55 H55 120.2 . . ? C54 C55 H55 120.2 . . ? C55 C56 C51 122.1(5) . . ? C55 C56 H56 118.9 . . ? C51 C56 H56 118.9 . . ? C42 C41 C46 118.8(4) . . ? C42 C41 P2 122.9(3) . . ? C46 C41 P2 118.1(4) . . ? C41 C46 C45 120.5(5) . . ? C41 C46 H46 119.7 . . ? C45 C46 H46 119.7 . . ? C44 C45 C46 119.5(5) . . ? C44 C45 H45 120.2 . . ? C46 C45 H45 120.2 . . ? C43 C44 C45 120.6(5) . . ? C43 C44 H44 119.7 . . ? C45 C44 H44 119.7 . . ? C44 C43 C42 120.3(6) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? C41 C42 C43 120.2(5) . . ? C41 C42 H42 119.9 . . ? C43 C42 H42 119.9 . . ? C12 C11 P2 129.1(3) . . ? C12 C11 H11 115.5 . . ? P2 C11 H11 115.5 . . ? C11 C12 S3 122.1(3) . . ? C11 C12 S4 125.4(3) . . ? S3 C12 S4 112.4(3) . . ? C14 C13 C15 126.0(6) . . ? C14 C13 S3 117.4(4) . . ? C15 C13 S3 116.6(5) . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C14 C16 128.0(5) . . ? C13 C14 S4 116.3(4) . . ? C16 C14 S4 115.8(4) . . ? C14 C16 H16C 109.5 . . ? C14 C16 H16B 109.5 . . ? H16C C16 H16B 109.5 . . ? C14 C16 H16A 109.5 . . ? H16C C16 H16A 109.5 . . ? H16B C16 H16A 109.5 . . ? C13 S3 C12 97.1(2) . . ? C14 S4 C12 96.7(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C103 Mo1 C101 O1 -50(4) . . . . ? C102 Mo1 C101 O1 39(4) . . . . ? C104 Mo1 C101 O1 -14(5) . . . . ? P2 Mo1 C101 O1 -139(4) . . . . ? P1 Mo1 C101 O1 129(4) . . . . ? C103 Mo1 C102 O2 67(8) . . . . ? C101 Mo1 C102 O2 -22(8) . . . . ? C104 Mo1 C102 O2 152(8) . . . . ? P2 Mo1 C102 O2 2(10) . . . . ? P1 Mo1 C102 O2 -119(8) . . . . ? C102 Mo1 C103 O3 8E1(4) . . . . ? C101 Mo1 C103 O3 17E1(10) . . . . ? C104 Mo1 C103 O3 -1E1(4) . . . . ? P2 Mo1 C103 O3 -10E1(4) . . . . ? P1 Mo1 C103 O3 -1E1(4) . . . . ? C103 Mo1 C104 O4 37(5) . . . . ? C102 Mo1 C104 O4 -52(5) . . . . ? C101 Mo1 C104 O4 0(5) . . . . ? P2 Mo1 C104 O4 126(5) . . . . ? P1 Mo1 C104 O4 -143(5) . . . . ? C32 C31 C36 C35 -0.7(7) . . . . ? P1 C31 C36 C35 170.8(4) . . . . ? C31 C36 C35 C34 0.2(8) . . . . ? C36 C35 C34 C33 0.9(8) . . . . ? C35 C34 C33 C32 -1.4(9) . . . . ? C34 C33 C32 C31 0.9(8) . . . . ? C36 C31 C32 C33 0.2(7) . . . . ? P1 C31 C32 C33 -171.4(4) . . . . ? C26 C21 C22 C23 0.4(6) . . . . ? P1 C21 C22 C23 175.2(3) . . . . ? C21 C22 C23 C24 0.2(7) . . . . ? C22 C23 C24 C25 0.2(7) . . . . ? C23 C24 C25 C26 -1.0(7) . . . . ? C24 C25 C26 C21 1.6(7) . . . . ? C22 C21 C26 C25 -1.3(6) . . . . ? P1 C21 C26 C25 -176.1(3) . . . . ? P1 C1 C2 S2 176.2(3) . . . . ? P1 C1 C2 S1 -3.6(6) . . . . ? C6 C4 C3 C5 0.9(11) . . . . ? S2 C4 C3 C5 178.8(6) . . . . ? C6 C4 C3 S1 -179.7(5) . . . . ? S2 C4 C3 S1 -1.7(6) . . . . ? C3 C4 S2 C2 -3.1(5) . . . . ? C6 C4 S2 C2 175.1(4) . . . . ? C1 C2 S2 C4 -173.2(4) . . . . ? S1 C2 S2 C4 6.6(3) . . . . ? C1 C2 S1 C3 172.5(4) . . . . ? S2 C2 S1 C3 -7.3(3) . . . . ? C4 C3 S1 C2 5.6(5) . . . . ? C5 C3 S1 C2 -174.9(5) . . . . ? C2 C1 P1 C31 165.3(4) . . . . ? C2 C1 P1 C21 58.6(4) . . . . ? C2 C1 P1 Mo1 -73.6(4) . . . . ? C32 C31 P1 C1 -149.7(4) . . . . ? C36 C31 P1 C1 38.9(4) . . . . ? C32 C31 P1 C21 -44.0(4) . . . . ? C36 C31 P1 C21 144.6(4) . . . . ? C32 C31 P1 Mo1 81.9(4) . . . . ? C36 C31 P1 Mo1 -89.5(4) . . . . ? C26 C21 P1 C1 61.4(4) . . . . ? C22 C21 P1 C1 -113.3(3) . . . . ? C26 C21 P1 C31 -44.6(4) . . . . ? C22 C21 P1 C31 140.7(3) . . . . ? C26 C21 P1 Mo1 -164.9(3) . . . . ? C22 C21 P1 Mo1 20.4(4) . . . . ? C103 Mo1 P1 C1 -118.0(15) . . . . ? C102 Mo1 P1 C1 157.82(19) . . . . ? C101 Mo1 P1 C1 70.80(19) . . . . ? C104 Mo1 P1 C1 -113.90(19) . . . . ? P2 Mo1 P1 C1 -18.97(15) . . . . ? C103 Mo1 P1 C31 -0.4(15) . . . . ? C102 Mo1 P1 C31 -84.54(19) . . . . ? C101 Mo1 P1 C31 -171.57(19) . . . . ? C104 Mo1 P1 C31 3.7(2) . . . . ? P2 Mo1 P1 C31 98.66(15) . . . . ? C103 Mo1 P1 C21 116.9(15) . . . . ? C102 Mo1 P1 C21 32.69(18) . . . . ? C101 Mo1 P1 C21 -54.34(18) . . . . ? C104 Mo1 P1 C21 120.97(18) . . . . ? P2 Mo1 P1 C21 -144.11(14) . . . . ? C103 Mo1 P2 C11 -112.3(2) . . . . ? C102 Mo1 P2 C11 -48(2) . . . . ? C101 Mo1 P2 C11 -23.5(2) . . . . ? C104 Mo1 P2 C11 162.9(2) . . . . ? P1 Mo1 P2 C11 73.11(16) . . . . ? C103 Mo1 P2 C51 3.69(18) . . . . ? C102 Mo1 P2 C51 68(2) . . . . ? C101 Mo1 P2 C51 92.57(19) . . . . ? C104 Mo1 P2 C51 -81.06(19) . . . . ? P1 Mo1 P2 C51 -170.87(14) . . . . ? C103 Mo1 P2 C41 125.0(2) . . . . ? C102 Mo1 P2 C41 -170(2) . . . . ? C101 Mo1 P2 C41 -146.1(2) . . . . ? C104 Mo1 P2 C41 40.2(2) . . . . ? P1 Mo1 P2 C41 -49.56(17) . . . . ? C11 P2 C51 C56 -133.2(4) . . . . ? C41 P2 C51 C56 -24.8(4) . . . . ? Mo1 P2 C51 C56 103.0(4) . . . . ? C11 P2 C51 C52 50.2(4) . . . . ? C41 P2 C51 C52 158.6(3) . . . . ? Mo1 P2 C51 C52 -73.6(4) . . . . ? C56 C51 C52 C53 0.8(7) . . . . ? P2 C51 C52 C53 177.7(4) . . . . ? C51 C52 C53 C54 -1.8(8) . . . . ? C52 C53 C54 C55 0.8(8) . . . . ? C53 C54 C55 C56 1.3(8) . . . . ? C54 C55 C56 C51 -2.4(8) . . . . ? C52 C51 C56 C55 1.3(7) . . . . ? P2 C51 C56 C55 -175.3(4) . . . . ? C11 P2 C41 C42 -7.4(4) . . . . ? C51 P2 C41 C42 -113.9(4) . . . . ? Mo1 P2 C41 C42 120.7(4) . . . . ? C11 P2 C41 C46 177.2(3) . . . . ? C51 P2 C41 C46 70.7(4) . . . . ? Mo1 P2 C41 C46 -54.7(4) . . . . ? C42 C41 C46 C45 2.3(7) . . . . ? P2 C41 C46 C45 177.9(4) . . . . ? C41 C46 C45 C44 -0.6(7) . . . . ? C46 C45 C44 C43 -1.3(8) . . . . ? C45 C44 C43 C42 1.6(8) . . . . ? C46 C41 C42 C43 -2.1(7) . . . . ? P2 C41 C42 C43 -177.4(4) . . . . ? C44 C43 C42 C41 0.1(8) . . . . ? C51 P2 C11 C12 45.0(5) . . . . ? C41 P2 C11 C12 -63.8(5) . . . . ? Mo1 P2 C11 C12 167.2(4) . . . . ? P2 C11 C12 S3 -176.4(3) . . . . ? P2 C11 C12 S4 1.5(7) . . . . ? C15 C13 C14 C16 -1.4(9) . . . . ? S3 C13 C14 C16 177.5(5) . . . . ? C15 C13 C14 S4 178.3(4) . . . . ? S3 C13 C14 S4 -2.8(6) . . . . ? C14 C13 S3 C12 -0.2(5) . . . . ? C15 C13 S3 C12 178.8(4) . . . . ? C11 C12 S3 C13 -178.8(4) . . . . ? S4 C12 S3 C13 3.0(3) . . . . ? C13 C14 S4 C12 4.3(5) . . . . ? C16 C14 S4 C12 -176.0(4) . . . . ? C11 C12 S4 C14 177.7(4) . . . . ? S3 C12 S4 C14 -4.2(3) . . . . ? data_compound6 _database_code_depnum_ccdc_archive 'CCDC 215145' _chemical_name_common metallacycle _audit_creation_date 2003-07-11T11:38:40-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C40 H32 Mo1 O4 P2 S4' _chemical_formula_sum 'C40 H32 Mo O4 P2 S4' _chemical_formula_weight 862.78 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.58400(10) _cell_length_b 11.91010(10) _cell_length_c 15.1839(2) _cell_angle_alpha 82.6920(10) _cell_angle_beta 87.9870(10) _cell_angle_gamma 70.5230(10) _cell_volume 1958.89(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 40839 _cell_measurement_theta_min 2.396 _cell_measurement_theta_max 30.034 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.95 _exptl_crystal_size_mid 0.8 _exptl_crystal_size_min 0.14 _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.67 _exptl_absorpt_correction_T_min 0.5688 _exptl_absorpt_correction_T_max 0.9121 _exptl_absorpt_correction_type sphere _exptl_absorpt_process_details 'Sheldrick, G.M. (2002) SADABS Bruker AXS Inc., Madison, Wisconsin, USA' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.138795E-1 _diffrn_orient_matrix_ub_12 -0.512843E-1 _diffrn_orient_matrix_ub_13 0.587531E-1 _diffrn_orient_matrix_ub_21 -0.28522E-2 _diffrn_orient_matrix_ub_22 -0.694167E-1 _diffrn_orient_matrix_ub_23 -0.295582E-1 _diffrn_orient_matrix_ub_31 0.904974E-1 _diffrn_orient_matrix_ub_32 -0.244578E-1 _diffrn_orient_matrix_ub_33 -0.93837E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0393 _diffrn_reflns_av_unetI/netI 0.0486 _diffrn_reflns_number 34395 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.929 _diffrn_measured_fraction_theta_max 0.929 _reflns_number_total 8374 _reflns_number_gt 5466 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0055P)^2^+4.7314P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 8374 _refine_ls_number_parameters 460 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0908 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.0975 _refine_ls_wR_factor_gt 0.0741 _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_restrained_S_all 1.128 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.812 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.096 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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 0.66630(3) 0.42478(3) 0.22819(2) 0.03120(10) Uani 1 1 d . . . S3 S 0.77352(9) -0.12244(9) 0.31203(7) 0.0358(2) Uani 1 1 d . . . S4 S 0.99098(8) -0.06677(8) 0.25716(7) 0.0338(2) Uani 1 1 d . . . P2 P 0.82861(8) 0.22687(8) 0.22261(6) 0.0240(2) Uani 1 1 d . . . P1 P 0.54954(8) 0.28503(8) 0.27870(6) 0.0279(2) Uani 1 1 d . . . S1 S 0.41367(9) 0.09062(10) 0.20474(7) 0.0408(3) Uani 1 1 d . . . S2 S 0.64623(9) -0.03150(10) 0.12627(7) 0.0391(2) Uani 1 1 d . . . C101 C 0.5174(4) 0.5706(4) 0.2305(3) 0.0461(11) Uani 1 1 d . . . O1 O 0.4308(3) 0.6526(3) 0.2306(3) 0.0784(11) Uani 1 1 d . . . O2 O 0.7496(4) 0.4465(3) 0.4208(3) 0.0781(11) Uani 1 1 d . . . C102 C 0.7163(4) 0.4368(4) 0.3527(3) 0.0461(11) Uani 1 1 d . . . C103 C 0.7689(4) 0.5251(4) 0.1865(3) 0.0504(12) Uani 1 1 d . . . O3 O 0.8267(3) 0.5850(3) 0.1630(3) 0.0847(13) Uani 1 1 d . . . C104 C 0.6354(4) 0.4150(4) 0.0992(3) 0.0547(13) Uani 1 1 d . . . O4 O 0.6259(3) 0.4076(5) 0.0255(2) 0.0998(16) Uani 1 1 d . . . C31 C 0.5440(3) 0.2439(3) 0.3986(2) 0.0311(8) Uani 1 1 d . . . C32 C 0.5121(5) 0.3338(4) 0.4542(3) 0.0556(13) Uani 1 1 d . . . H32 H 0.4922 0.4135 0.4295 0.067 Uiso 1 1 calc R . . C33 C 0.5095(6) 0.3072(5) 0.5448(3) 0.0726(16) Uani 1 1 d . . . H33 H 0.487 0.3685 0.5808 0.087 Uiso 1 1 calc R . . C34 C 0.5400(5) 0.1901(5) 0.5819(3) 0.0638(14) Uani 1 1 d . . . H34 H 0.5389 0.1718 0.6432 0.077 Uiso 1 1 calc R . . C35 C 0.5719(5) 0.1007(4) 0.5293(3) 0.0594(13) Uani 1 1 d . . . H35 H 0.5924 0.0213 0.5549 0.071 Uiso 1 1 calc R . . C36 C 0.5740(4) 0.1269(4) 0.4375(3) 0.0432(10) Uani 1 1 d . . . H36 H 0.596 0.0648 0.4021 0.052 Uiso 1 1 calc R . . C21 C 0.3885(3) 0.3434(3) 0.2447(3) 0.0404(10) Uani 1 1 d . . . C22 C 0.2942(4) 0.3506(4) 0.3058(4) 0.0576(13) Uani 1 1 d . . . H22 H 0.3123 0.3172 0.3645 0.069 Uiso 1 1 calc R . . C23 C 0.1734(4) 0.4077(5) 0.2786(6) 0.086(2) Uani 1 1 d . . . H23 H 0.1106 0.4112 0.3192 0.103 Uiso 1 1 calc R . . C24 C 0.1460(5) 0.4585(5) 0.1933(6) 0.093(3) Uani 1 1 d . . . H24 H 0.0649 0.499 0.1763 0.112 Uiso 1 1 calc R . . C25 C 0.2362(6) 0.4506(6) 0.1329(5) 0.099(2) Uani 1 1 d . . . H25 H 0.2168 0.4836 0.0743 0.119 Uiso 1 1 calc R . . C26 C 0.3580(4) 0.3931(5) 0.1587(4) 0.0685(16) Uani 1 1 d . . . H26 H 0.4196 0.3884 0.1169 0.082 Uiso 1 1 calc R . . C51 C 0.9459(3) 0.1837(3) 0.3100(2) 0.0252(7) Uani 1 1 d . . . C52 C 1.0690(3) 0.1652(4) 0.2952(3) 0.0389(9) Uani 1 1 d . . . H52 H 1.0975 0.1739 0.2375 0.047 Uiso 1 1 calc R . . C53 C 1.1501(4) 0.1337(4) 0.3666(3) 0.0537(12) Uani 1 1 d . . . H53 H 1.2326 0.1227 0.3566 0.064 Uiso 1 1 calc R . . C54 C 1.1095(4) 0.1188(4) 0.4516(3) 0.0574(13) Uani 1 1 d . . . H54 H 1.1647 0.0953 0.4989 0.069 Uiso 1 1 calc R . . C55 C 0.9871(4) 0.1384(4) 0.4669(3) 0.0499(11) Uani 1 1 d . . . H55 H 0.9592 0.1295 0.5247 0.06 Uiso 1 1 calc R . . C56 C 0.9059(4) 0.1711(3) 0.3968(2) 0.0362(9) Uani 1 1 d . . . H56 H 0.8231 0.185 0.4077 0.043 Uiso 1 1 calc R . . C41 C 0.9101(3) 0.2162(3) 0.1169(2) 0.0274(8) Uani 1 1 d . . . C42 C 0.8924(4) 0.1485(4) 0.0552(3) 0.0404(10) Uani 1 1 d . . . H42 H 0.8453 0.0991 0.0696 0.049 Uiso 1 1 calc R . . C43 C 0.9443(4) 0.1532(4) -0.0286(3) 0.0521(12) Uani 1 1 d . . . H43 H 0.9309 0.1077 -0.0701 0.063 Uiso 1 1 calc R . . C44 C 1.0150(4) 0.2246(4) -0.0504(3) 0.0518(12) Uani 1 1 d . . . H44 H 1.0505 0.2266 -0.1062 0.062 Uiso 1 1 calc R . . C45 C 1.0332(4) 0.2928(4) 0.0103(3) 0.0489(11) Uani 1 1 d . . . H45 H 1.0816 0.3409 -0.0042 0.059 Uiso 1 1 calc R . . C46 C 0.9797(4) 0.2904(4) 0.0933(3) 0.0395(10) Uani 1 1 d . . . H46 H 0.9904 0.3388 0.1336 0.047 Uiso 1 1 calc R . . C1 C 0.6258(3) 0.1434(3) 0.2338(2) 0.0261(8) Uani 1 1 d . . . C11 C 0.7607(3) 0.1065(3) 0.2383(2) 0.0231(7) Uani 1 1 d . . . C2 C 0.5684(3) 0.0792(3) 0.1939(2) 0.0296(8) Uani 1 1 d . . . C12 C 0.8314(3) -0.0101(3) 0.2655(2) 0.0253(7) Uani 1 1 d . . . C5 C 0.2979(4) -0.0469(4) 0.1344(4) 0.0577(13) Uani 1 1 d . . . H5B H 0.2362 0.0073 0.167 0.086 Uiso 1 1 calc R . . H5A H 0.3073 -0.1281 0.1584 0.086 Uiso 1 1 calc R . . H5C H 0.2738 -0.034 0.0731 0.086 Uiso 1 1 calc R . . C3 C 0.4179(3) -0.0248(3) 0.1420(3) 0.0375(9) Uani 1 1 d . . . C4 C 0.5243(3) -0.0815(3) 0.1061(3) 0.0354(9) Uani 1 1 d . . . C6 C 0.5542(4) -0.1848(4) 0.0528(3) 0.0480(11) Uani 1 1 d . . . H6C H 0.6386 -0.207 0.0357 0.072 Uiso 1 1 calc R . . H6A H 0.5032 -0.1619 0.0006 0.072 Uiso 1 1 calc R . . H6B H 0.5398 -0.2518 0.0878 0.072 Uiso 1 1 calc R . . C13 C 0.9137(4) -0.2339(3) 0.3404(3) 0.0392(10) Uani 1 1 d . . . C15 C 0.9060(5) -0.3485(4) 0.3918(4) 0.0716(16) Uani 1 1 d . . . H15C H 0.8216 -0.3414 0.4014 0.107 Uiso 1 1 calc R . . H15A H 0.947 -0.3623 0.448 0.107 Uiso 1 1 calc R . . H15B H 0.9445 -0.4144 0.3586 0.107 Uiso 1 1 calc R . . C14 C 1.0143(4) -0.2091(3) 0.3143(3) 0.0383(9) Uani 1 1 d . . . C16 C 1.1460(4) -0.2874(4) 0.3291(4) 0.0644(14) Uani 1 1 d . . . H16A H 1.1986 -0.2451 0.3025 0.097 Uiso 1 1 calc R . . H16C H 1.1606 -0.3597 0.3025 0.097 Uiso 1 1 calc R . . H16B H 1.1628 -0.307 0.3916 0.097 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 0.02508(17) 0.02613(17) 0.0391(2) 0.00385(14) 0.00351(13) -0.00731(13) S3 0.0337(5) 0.0306(5) 0.0445(6) 0.0012(4) -0.0007(4) -0.0145(4) S4 0.0248(5) 0.0297(5) 0.0442(6) -0.0062(4) 0.0043(4) -0.0052(4) P2 0.0214(4) 0.0290(5) 0.0217(5) -0.0003(4) 0.0009(3) -0.0095(4) P1 0.0221(4) 0.0275(5) 0.0324(5) -0.0008(4) 0.0023(4) -0.0070(4) S1 0.0272(5) 0.0511(6) 0.0529(7) -0.0213(5) 0.0082(4) -0.0199(5) S2 0.0292(5) 0.0524(6) 0.0380(6) -0.0197(5) 0.0012(4) -0.0116(5) C101 0.036(2) 0.039(2) 0.055(3) 0.002(2) 0.010(2) -0.006(2) O1 0.052(2) 0.052(2) 0.106(3) -0.005(2) 0.013(2) 0.0132(18) O2 0.094(3) 0.072(3) 0.072(3) -0.028(2) -0.017(2) -0.024(2) C102 0.047(3) 0.034(2) 0.057(3) -0.009(2) 0.001(2) -0.013(2) C103 0.031(2) 0.037(2) 0.073(3) 0.012(2) 0.002(2) -0.0054(19) O3 0.053(2) 0.060(2) 0.139(4) 0.024(2) 0.014(2) -0.0302(19) C104 0.033(2) 0.065(3) 0.046(3) 0.012(2) 0.000(2) 0.004(2) O4 0.067(3) 0.164(4) 0.037(2) 0.005(2) -0.0066(18) -0.003(3) C31 0.0303(19) 0.031(2) 0.031(2) -0.0035(16) 0.0066(15) -0.0099(16) C32 0.089(4) 0.036(2) 0.044(3) -0.009(2) 0.020(2) -0.025(2) C33 0.113(5) 0.065(3) 0.046(3) -0.025(3) 0.025(3) -0.033(3) C34 0.086(4) 0.074(4) 0.030(3) -0.001(3) 0.008(2) -0.027(3) C35 0.078(3) 0.050(3) 0.039(3) 0.008(2) 0.004(2) -0.011(3) C36 0.050(3) 0.036(2) 0.037(2) -0.0066(19) 0.0079(19) -0.006(2) C21 0.0242(19) 0.027(2) 0.069(3) -0.001(2) -0.0032(19) -0.0084(16) C22 0.031(2) 0.049(3) 0.095(4) -0.028(3) 0.012(2) -0.011(2) C23 0.026(3) 0.061(4) 0.174(7) -0.053(4) 0.012(3) -0.008(3) C24 0.035(3) 0.038(3) 0.207(9) -0.011(4) -0.036(4) -0.008(2) C25 0.060(4) 0.082(4) 0.151(7) 0.039(4) -0.056(4) -0.032(3) C26 0.040(3) 0.076(4) 0.087(4) 0.028(3) -0.024(3) -0.027(3) C51 0.0295(18) 0.0249(18) 0.0229(19) -0.0037(15) -0.0043(14) -0.0108(15) C52 0.028(2) 0.052(3) 0.035(2) 0.0010(19) -0.0031(16) -0.0124(18) C53 0.028(2) 0.077(3) 0.053(3) 0.000(3) -0.009(2) -0.016(2) C54 0.053(3) 0.071(3) 0.043(3) -0.001(2) -0.023(2) -0.014(3) C55 0.060(3) 0.063(3) 0.025(2) -0.004(2) -0.003(2) -0.017(2) C56 0.038(2) 0.043(2) 0.026(2) -0.0067(18) 0.0016(16) -0.0104(18) C41 0.0238(17) 0.0335(19) 0.0220(19) 0.0017(15) 0.0003(14) -0.0075(15) C42 0.044(2) 0.049(2) 0.033(2) -0.0071(19) 0.0095(18) -0.022(2) C43 0.068(3) 0.064(3) 0.028(2) -0.017(2) 0.011(2) -0.025(3) C44 0.056(3) 0.068(3) 0.031(2) -0.002(2) 0.017(2) -0.024(2) C45 0.050(3) 0.062(3) 0.041(3) -0.001(2) 0.014(2) -0.031(2) C46 0.040(2) 0.053(3) 0.032(2) -0.0046(19) 0.0048(17) -0.024(2) C1 0.0235(17) 0.0296(19) 0.0245(19) -0.0013(15) 0.0006(14) -0.0086(15) C11 0.0209(16) 0.0253(18) 0.0235(18) -0.0032(14) -0.0006(13) -0.0081(14) C2 0.0230(17) 0.039(2) 0.026(2) -0.0040(16) 0.0019(14) -0.0097(16) C12 0.0259(18) 0.0299(19) 0.0217(18) -0.0049(15) 0.0020(14) -0.0110(15) C5 0.043(3) 0.056(3) 0.086(4) -0.023(3) -0.002(2) -0.026(2) C3 0.034(2) 0.037(2) 0.045(2) -0.0064(19) -0.0062(18) -0.0150(18) C4 0.038(2) 0.037(2) 0.033(2) -0.0030(17) -0.0105(17) -0.0134(18) C6 0.057(3) 0.038(2) 0.047(3) -0.008(2) -0.009(2) -0.012(2) C13 0.050(3) 0.0221(19) 0.044(2) -0.0043(17) -0.0037(19) -0.0092(18) C15 0.078(4) 0.031(2) 0.098(4) 0.011(3) 0.005(3) -0.015(2) C14 0.037(2) 0.029(2) 0.045(3) -0.0109(18) -0.0040(18) -0.0034(17) C16 0.045(3) 0.039(3) 0.093(4) -0.007(3) -0.008(3) 0.008(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C103 1.986(4) . ? Mo1 C101 2.002(4) . ? Mo1 C104 2.027(5) . ? Mo1 C102 2.033(5) . ? Mo1 P2 2.4865(9) . ? Mo1 P1 2.5084(10) . ? S3 C13 1.747(4) . ? S3 C12 1.750(3) . ? S4 C14 1.743(4) . ? S4 C12 1.750(3) . ? P2 C41 1.831(3) . ? P2 C51 1.833(3) . ? P2 C11 1.839(3) . ? P1 C21 1.828(4) . ? P1 C31 1.828(4) . ? P1 C1 1.829(4) . ? S1 C2 1.755(3) . ? S1 C3 1.757(4) . ? S2 C4 1.756(4) . ? S2 C2 1.758(4) . ? C101 O1 1.143(5) . ? O2 C102 1.148(5) . ? C103 O3 1.148(5) . ? C104 O4 1.147(6) . ? C31 C36 1.377(5) . ? C31 C32 1.393(6) . ? C32 C33 1.373(7) . ? C32 H32 0.93 . ? C33 C34 1.368(7) . ? C33 H33 0.93 . ? C34 C35 1.357(7) . ? C34 H34 0.93 . ? C35 C36 1.390(6) . ? C35 H35 0.93 . ? C36 H36 0.93 . ? C21 C26 1.370(6) . ? C21 C22 1.395(6) . ? C22 C23 1.388(7) . ? C22 H22 0.93 . ? C23 C24 1.360(9) . ? C23 H23 0.93 . ? C24 C25 1.352(10) . ? C24 H24 0.93 . ? C25 C26 1.393(7) . ? C25 H25 0.93 . ? C26 H26 0.93 . ? C51 C52 1.384(5) . ? C51 C56 1.389(5) . ? C52 C53 1.390(5) . ? C52 H52 0.93 . ? C53 C54 1.368(6) . ? C53 H53 0.93 . ? C54 C55 1.374(6) . ? C54 H54 0.93 . ? C55 C56 1.375(5) . ? C55 H55 0.93 . ? C56 H56 0.93 . ? C41 C42 1.372(5) . ? C41 C46 1.391(5) . ? C42 C43 1.391(5) . ? C42 H42 0.93 . ? C43 C44 1.369(6) . ? C43 H43 0.93 . ? C44 C45 1.368(6) . ? C44 H44 0.93 . ? C45 C46 1.387(5) . ? C45 H45 0.93 . ? C46 H46 0.93 . ? C1 C2 1.371(5) . ? C1 C11 1.478(4) . ? C11 C12 1.375(5) . ? C5 C3 1.510(5) . ? C5 H5B 0.96 . ? C5 H5A 0.96 . ? C5 H5C 0.96 . ? C3 C4 1.327(5) . ? C4 C6 1.496(5) . ? C6 H6C 0.96 . ? C6 H6A 0.96 . ? C6 H6B 0.96 . ? C13 C14 1.330(6) . ? C13 C15 1.511(6) . ? C15 H15C 0.96 . ? C15 H15A 0.96 . ? C15 H15B 0.96 . ? C14 C16 1.507(5) . ? C16 H16A 0.96 . ? C16 H16C 0.96 . ? C16 H16B 0.96 . ? 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 C103 Mo1 C101 91.32(17) . . ? C103 Mo1 C104 88.2(2) . . ? C101 Mo1 C104 91.53(18) . . ? C103 Mo1 C102 85.85(19) . . ? C101 Mo1 C102 91.78(18) . . ? C104 Mo1 C102 173.29(18) . . ? C103 Mo1 P2 96.76(12) . . ? C101 Mo1 P2 171.11(13) . . ? C104 Mo1 P2 85.04(13) . . ? C102 Mo1 P2 92.49(12) . . ? C103 Mo1 P1 175.86(12) . . ? C101 Mo1 P1 92.76(12) . . ? C104 Mo1 P1 90.96(14) . . ? C102 Mo1 P1 94.70(12) . . ? P2 Mo1 P1 79.12(3) . . ? C13 S3 C12 97.55(18) . . ? C14 S4 C12 98.20(18) . . ? C41 P2 C51 106.48(16) . . ? C41 P2 C11 107.60(16) . . ? C51 P2 C11 103.96(15) . . ? C41 P2 Mo1 112.80(11) . . ? C51 P2 Mo1 115.41(11) . . ? C11 P2 Mo1 109.97(11) . . ? C21 P1 C31 103.77(19) . . ? C21 P1 C1 109.83(17) . . ? C31 P1 C1 105.08(16) . . ? C21 P1 Mo1 113.71(13) . . ? C31 P1 Mo1 116.32(12) . . ? C1 P1 Mo1 107.72(11) . . ? C2 S1 C3 97.58(18) . . ? C4 S2 C2 98.18(18) . . ? O1 C101 Mo1 178.4(4) . . ? O2 C102 Mo1 175.9(4) . . ? O3 C103 Mo1 178.7(4) . . ? O4 C104 Mo1 175.6(4) . . ? C36 C31 C32 117.7(4) . . ? C36 C31 P1 123.0(3) . . ? C32 C31 P1 119.2(3) . . ? C33 C32 C31 121.4(4) . . ? C33 C32 H32 119.3 . . ? C31 C32 H32 119.3 . . ? C34 C33 C32 119.8(5) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C35 C34 C33 120.1(5) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? C34 C35 C36 120.5(4) . . ? C34 C35 H35 119.7 . . ? C36 C35 H35 119.7 . . ? C31 C36 C35 120.5(4) . . ? C31 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? C26 C21 C22 118.3(4) . . ? C26 C21 P1 119.5(3) . . ? C22 C21 P1 121.9(4) . . ? C23 C22 C21 119.8(6) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C24 C23 C22 120.5(6) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C25 C24 C23 120.3(5) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C26 120.0(6) . . ? C24 C25 H25 120 . . ? C26 C25 H25 120 . . ? C21 C26 C25 120.9(6) . . ? C21 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C52 C51 C56 118.8(3) . . ? C52 C51 P2 124.6(3) . . ? C56 C51 P2 116.5(3) . . ? C51 C52 C53 119.8(4) . . ? C51 C52 H52 120.1 . . ? C53 C52 H52 120.1 . . ? C54 C53 C52 120.6(4) . . ? C54 C53 H53 119.7 . . ? C52 C53 H53 119.7 . . ? C53 C54 C55 119.9(4) . . ? C53 C54 H54 120.1 . . ? C55 C54 H54 120.1 . . ? C54 C55 C56 120.1(4) . . ? C54 C55 H55 120 . . ? C56 C55 H55 120 . . ? C55 C56 C51 120.8(4) . . ? C55 C56 H56 119.6 . . ? C51 C56 H56 119.6 . . ? C42 C41 C46 118.6(3) . . ? C42 C41 P2 121.9(3) . . ? C46 C41 P2 119.0(3) . . ? C41 C42 C43 120.6(4) . . ? C41 C42 H42 119.7 . . ? C43 C42 H42 119.7 . . ? C44 C43 C42 120.3(4) . . ? C44 C43 H43 119.8 . . ? C42 C43 H43 119.8 . . ? C45 C44 C43 119.8(4) . . ? C45 C44 H44 120.1 . . ? C43 C44 H44 120.1 . . ? C44 C45 C46 120.2(4) . . ? C44 C45 H45 119.9 . . ? C46 C45 H45 119.9 . . ? C45 C46 C41 120.5(4) . . ? C45 C46 H46 119.8 . . ? C41 C46 H46 119.8 . . ? C2 C1 C11 121.3(3) . . ? C2 C1 P1 125.6(3) . . ? C11 C1 P1 113.0(2) . . ? C12 C11 C1 121.6(3) . . ? C12 C11 P2 120.9(2) . . ? C1 C11 P2 116.9(2) . . ? C1 C2 S1 126.2(3) . . ? C1 C2 S2 122.6(3) . . ? S1 C2 S2 111.1(2) . . ? C11 C12 S4 124.7(3) . . ? C11 C12 S3 124.5(3) . . ? S4 C12 S3 110.86(19) . . ? C3 C5 H5B 109.5 . . ? C3 C5 H5A 109.5 . . ? H5B C5 H5A 109.5 . . ? C3 C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? C4 C3 C5 127.4(4) . . ? C4 C3 S1 117.3(3) . . ? C5 C3 S1 115.3(3) . . ? C3 C4 C6 128.2(4) . . ? C3 C4 S2 115.8(3) . . ? C6 C4 S2 115.9(3) . . ? C4 C6 H6C 109.5 . . ? C4 C6 H6A 109.5 . . ? H6C C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6C C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C14 C13 C15 127.5(4) . . ? C14 C13 S3 116.9(3) . . ? C15 C13 S3 115.6(3) . . ? C13 C15 H15C 109.5 . . ? C13 C15 H15A 109.5 . . ? H15C C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15C C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C14 C16 128.4(4) . . ? C13 C14 S4 115.9(3) . . ? C16 C14 S4 115.7(3) . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? H16C C16 H16B 109.5 . . ? 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 C103 Mo1 P2 C41 -49.6(2) . . . . ? C101 Mo1 P2 C41 105.6(9) . . . . ? C104 Mo1 P2 C41 38.00(19) . . . . ? C102 Mo1 P2 C41 -135.75(18) . . . . ? P1 Mo1 P2 C41 129.94(13) . . . . ? C103 Mo1 P2 C51 73.07(19) . . . . ? C101 Mo1 P2 C51 -131.7(9) . . . . ? C104 Mo1 P2 C51 160.70(19) . . . . ? C102 Mo1 P2 C51 -13.05(17) . . . . ? P1 Mo1 P2 C51 -107.36(13) . . . . ? C103 Mo1 P2 C11 -169.75(19) . . . . ? C101 Mo1 P2 C11 -14.5(9) . . . . ? C104 Mo1 P2 C11 -82.11(18) . . . . ? C102 Mo1 P2 C11 104.14(17) . . . . ? P1 Mo1 P2 C11 9.83(12) . . . . ? C103 Mo1 P1 C21 -141(2) . . . . ? C101 Mo1 P1 C21 29.4(2) . . . . ? C104 Mo1 P1 C21 -62.2(2) . . . . ? C102 Mo1 P1 C21 121.4(2) . . . . ? P2 Mo1 P1 C21 -146.97(16) . . . . ? C103 Mo1 P1 C31 98(2) . . . . ? C101 Mo1 P1 C31 -91.11(19) . . . . ? C104 Mo1 P1 C31 177.31(18) . . . . ? C102 Mo1 P1 C31 0.91(18) . . . . ? P2 Mo1 P1 C31 92.55(13) . . . . ? C103 Mo1 P1 C1 -19(2) . . . . ? C101 Mo1 P1 C1 151.33(18) . . . . ? C104 Mo1 P1 C1 59.75(17) . . . . ? C102 Mo1 P1 C1 -116.65(17) . . . . ? P2 Mo1 P1 C1 -25.01(12) . . . . ? C103 Mo1 C101 O1 129(15) . . . . ? C104 Mo1 C101 O1 41(15) . . . . ? C102 Mo1 C101 O1 -145(15) . . . . ? P2 Mo1 C101 O1 -26(16) . . . . ? P1 Mo1 C101 O1 -50(15) . . . . ? C103 Mo1 C102 O2 -11(6) . . . . ? C101 Mo1 C102 O2 -102(6) . . . . ? C104 Mo1 C102 O2 17(7) . . . . ? P2 Mo1 C102 O2 85(6) . . . . ? P1 Mo1 C102 O2 165(6) . . . . ? C101 Mo1 C103 O3 2E1(2) . . . . ? C104 Mo1 C103 O3 11E1(2) . . . . ? C102 Mo1 C103 O3 -7E1(2) . . . . ? P2 Mo1 C103 O3 -16E1(2) . . . . ? P1 Mo1 C103 O3 -17E1(10) . . . . ? C103 Mo1 C104 O4 48(6) . . . . ? C101 Mo1 C104 O4 139(6) . . . . ? C102 Mo1 C104 O4 20(7) . . . . ? P2 Mo1 C104 O4 -49(6) . . . . ? P1 Mo1 C104 O4 -128(6) . . . . ? C21 P1 C31 C36 105.6(4) . . . . ? C1 P1 C31 C36 -9.7(4) . . . . ? Mo1 P1 C31 C36 -128.7(3) . . . . ? C21 P1 C31 C32 -76.7(4) . . . . ? C1 P1 C31 C32 168.0(3) . . . . ? Mo1 P1 C31 C32 49.0(4) . . . . ? C36 C31 C32 C33 -0.6(7) . . . . ? P1 C31 C32 C33 -178.5(4) . . . . ? C31 C32 C33 C34 0.8(9) . . . . ? C32 C33 C34 C35 -0.5(9) . . . . ? C33 C34 C35 C36 0.1(8) . . . . ? C32 C31 C36 C35 0.2(6) . . . . ? P1 C31 C36 C35 177.9(3) . . . . ? C34 C35 C36 C31 0.1(7) . . . . ? C31 P1 C21 C26 174.1(4) . . . . ? C1 P1 C21 C26 -73.9(4) . . . . ? Mo1 P1 C21 C26 46.8(4) . . . . ? C31 P1 C21 C22 1.1(4) . . . . ? C1 P1 C21 C22 113.0(4) . . . . ? Mo1 P1 C21 C22 -126.3(3) . . . . ? C26 C21 C22 C23 -0.4(7) . . . . ? P1 C21 C22 C23 172.8(4) . . . . ? C21 C22 C23 C24 -1.1(8) . . . . ? C22 C23 C24 C25 2.2(9) . . . . ? C23 C24 C25 C26 -1.8(9) . . . . ? C22 C21 C26 C25 0.7(8) . . . . ? P1 C21 C26 C25 -172.6(4) . . . . ? C24 C25 C26 C21 0.3(9) . . . . ? C41 P2 C51 C52 8.7(4) . . . . ? C11 P2 C51 C52 122.2(3) . . . . ? Mo1 P2 C51 C52 -117.3(3) . . . . ? C41 P2 C51 C56 -172.4(3) . . . . ? C11 P2 C51 C56 -58.9(3) . . . . ? Mo1 P2 C51 C56 61.6(3) . . . . ? C56 C51 C52 C53 0.5(6) . . . . ? P2 C51 C52 C53 179.4(3) . . . . ? C51 C52 C53 C54 1.1(7) . . . . ? C52 C53 C54 C55 -1.9(8) . . . . ? C53 C54 C55 C56 1.0(8) . . . . ? C54 C55 C56 C51 0.6(7) . . . . ? C52 C51 C56 C55 -1.4(6) . . . . ? P2 C51 C56 C55 179.7(3) . . . . ? C51 P2 C41 C42 125.5(3) . . . . ? C11 P2 C41 C42 14.5(4) . . . . ? Mo1 P2 C41 C42 -107.0(3) . . . . ? C51 P2 C41 C46 -62.9(3) . . . . ? C11 P2 C41 C46 -173.9(3) . . . . ? Mo1 P2 C41 C46 64.6(3) . . . . ? C46 C41 C42 C43 0.7(6) . . . . ? P2 C41 C42 C43 172.3(3) . . . . ? C41 C42 C43 C44 0.8(7) . . . . ? C42 C43 C44 C45 -0.9(7) . . . . ? C43 C44 C45 C46 -0.4(7) . . . . ? C44 C45 C46 C41 1.9(7) . . . . ? C42 C41 C46 C45 -2.1(6) . . . . ? P2 C41 C46 C45 -173.9(3) . . . . ? C21 P1 C1 C2 -10.5(4) . . . . ? C31 P1 C1 C2 100.6(3) . . . . ? Mo1 P1 C1 C2 -134.8(3) . . . . ? C21 P1 C1 C11 165.2(3) . . . . ? C31 P1 C1 C11 -83.8(3) . . . . ? Mo1 P1 C1 C11 40.9(3) . . . . ? C2 C1 C11 C12 -47.8(5) . . . . ? P1 C1 C11 C12 136.3(3) . . . . ? C2 C1 C11 P2 141.3(3) . . . . ? P1 C1 C11 P2 -34.5(3) . . . . ? C41 P2 C11 C12 77.4(3) . . . . ? C51 P2 C11 C12 -35.3(3) . . . . ? Mo1 P2 C11 C12 -159.4(3) . . . . ? C41 P2 C11 C1 -111.7(3) . . . . ? C51 P2 C11 C1 135.6(3) . . . . ? Mo1 P2 C11 C1 11.5(3) . . . . ? C11 C1 C2 S1 164.7(3) . . . . ? P1 C1 C2 S1 -20.0(5) . . . . ? C11 C1 C2 S2 -13.2(5) . . . . ? P1 C1 C2 S2 162.1(2) . . . . ? C3 S1 C2 C1 -176.0(3) . . . . ? C3 S1 C2 S2 2.1(2) . . . . ? C4 S2 C2 C1 175.9(3) . . . . ? C4 S2 C2 S1 -2.3(2) . . . . ? C1 C11 C12 S4 169.9(3) . . . . ? P2 C11 C12 S4 -19.6(4) . . . . ? C1 C11 C12 S3 -9.3(5) . . . . ? P2 C11 C12 S3 161.1(2) . . . . ? C14 S4 C12 C11 173.7(3) . . . . ? C14 S4 C12 S3 -7.0(2) . . . . ? C13 S3 C12 C11 -173.2(3) . . . . ? C13 S3 C12 S4 7.5(2) . . . . ? C2 S1 C3 C4 -1.1(4) . . . . ? C2 S1 C3 C5 179.6(3) . . . . ? C5 C3 C4 C6 -3.0(7) . . . . ? S1 C3 C4 C6 177.7(3) . . . . ? C5 C3 C4 S2 178.9(4) . . . . ? S1 C3 C4 S2 -0.4(5) . . . . ? C2 S2 C4 C3 1.7(4) . . . . ? C2 S2 C4 C6 -176.7(3) . . . . ? C12 S3 C13 C14 -5.5(4) . . . . ? C12 S3 C13 C15 174.9(4) . . . . ? C15 C13 C14 C16 -0.3(8) . . . . ? S3 C13 C14 C16 -179.9(4) . . . . ? C15 C13 C14 S4 -179.1(4) . . . . ? S3 C13 C14 S4 1.3(5) . . . . ? C12 S4 C14 C13 3.6(4) . . . . ? C12 S4 C14 C16 -175.4(3) . . . . ?