# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Dr Narcis Avarvari' _publ_contact_author_address ; Chemistry CNRS-Universite d'Angers 2 Bd. Lavoisier, UFR Sciences, Bat. ANGERS 49045 FRANCE ; _publ_contact_author_email NARCIS.AVARVARI@UNIV-ANGERS.FR _publ_section_title ; 1,4-Dihydro-1,4-diphosphinine fused with two tetrathiafulvalenes ; loop_ _publ_author_name 'Narcis Avarvari' 'Marc Fourmigue' data_na105a _database_code_depnum_ccdc_archive 'CCDC 239190' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'cis-(o-DMTTF)2(PPh)2, THF' _chemical_melting_point ? _chemical_formula_moiety C32H30O1P2S8 _chemical_formula_sum 'C32 H30 O P2 S8' _chemical_formula_weight 748.98 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' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.5674(14) _cell_length_b 13.0748(14) _cell_length_c 13.2647(14) _cell_angle_alpha 62.261(11) _cell_angle_beta 69.342(12) _cell_angle_gamma 67.485(12) _cell_volume 1741.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 1.65 _cell_measurement_theta_max 26.05 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.7 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.429 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 0.631 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 STOE-IPDS _diffrn_measurement_method 'Rotation, Phi. incr. = 1.7' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17474 _diffrn_reflns_av_R_equivalents 0.0692 _diffrn_reflns_av_sigmaI/netI 0.0824 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.90 _reflns_number_total 6205 _reflns_number_gt 3682 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE [STOE-IPDS]' _computing_cell_refinement 'SELECT, CELL [STOE-IPDS]' _computing_data_reduction 'INTEGRATE [STOE-IPDS]' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0411P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6205 _refine_ls_number_parameters 434 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0737 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.1004 _refine_ls_wR_factor_gt 0.0925 _refine_ls_goodness_of_fit_ref 0.822 _refine_ls_restrained_S_all 0.822 _refine_ls_shift/su_max 0.006 _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 S1 S 0.65065(7) 0.60335(9) 0.23884(7) 0.0505(2) Uani 1 1 d . . . S2 S 0.59927(7) 0.61758(9) 0.03198(7) 0.0519(2) Uani 1 1 d . . . S3 S 0.40203(7) 0.53929(9) 0.39407(7) 0.0515(2) Uani 1 1 d . . . S4 S 0.34856(7) 0.55634(10) 0.18778(8) 0.0547(3) Uani 1 1 d . . . S5 S 1.12391(6) 0.63701(9) -0.01722(7) 0.0483(2) Uani 1 1 d . . . S6 S 1.07074(7) 0.65199(9) -0.22188(7) 0.0488(2) Uani 1 1 d . . . S7 S 1.37467(7) 0.70225(10) -0.17680(8) 0.0546(3) Uani 1 1 d . . . S8 S 1.31977(7) 0.71645(10) -0.38025(8) 0.0550(3) Uani 1 1 d . . . P1 P 0.87136(7) 0.68682(9) 0.11463(7) 0.0443(2) Uani 1 1 d . . . P2 P 0.80695(7) 0.70665(9) -0.13813(7) 0.0437(2) Uani 1 1 d . . . C1 C 0.7456(2) 0.6574(3) 0.1044(3) 0.0400(7) Uani 1 1 d . . . C2 C 0.7224(2) 0.6639(3) 0.0102(3) 0.0405(8) Uani 1 1 d . . . C3 C 0.5504(3) 0.5948(3) 0.1797(3) 0.0460(8) Uani 1 1 d . . . C4 C 0.4478(3) 0.5672(3) 0.2455(3) 0.0465(8) Uani 1 1 d . . . C5 C 0.2600(3) 0.5369(4) 0.4060(3) 0.0630(11) Uani 1 1 d . . . C6 C 0.2365(3) 0.5439(4) 0.3131(3) 0.0628(11) Uani 1 1 d . . . C7 C 0.1805(4) 0.5241(6) 0.5226(4) 0.116(2) Uani 1 1 d . . . H7A H 0.2216 0.5208 0.5733 0.175 Uiso 1 1 calc R . . H7B H 0.1562 0.4518 0.5550 0.175 Uiso 1 1 calc R . . H7C H 0.1123 0.5916 0.5147 0.175 Uiso 1 1 calc R . . C8 C 0.1236(4) 0.5387(6) 0.3015(4) 0.113(2) Uani 1 1 d . . . H8A H 0.1317 0.5473 0.2234 0.169 Uiso 1 1 calc R . . H8B H 0.0597 0.6025 0.3181 0.169 Uiso 1 1 calc R . . H8C H 0.1077 0.4631 0.3555 0.169 Uiso 1 1 calc R . . C9 C 0.9735(2) 0.6727(3) -0.0174(3) 0.0406(8) Uani 1 1 d . . . C10 C 0.9494(2) 0.6799(3) -0.1116(3) 0.0393(7) Uani 1 1 d . . . C11 C 1.1711(3) 0.6647(3) -0.1664(3) 0.0449(8) Uani 1 1 d . . . C12 C 1.2739(3) 0.6916(3) -0.2326(3) 0.0448(8) Uani 1 1 d . . . C13 C 1.4652(3) 0.7616(4) -0.3131(3) 0.0581(10) Uani 1 1 d . . . C14 C 1.4407(3) 0.7680(4) -0.4049(3) 0.0589(10) Uani 1 1 d . . . C15 C 1.5662(4) 0.7939(5) -0.3086(4) 0.0873(15) Uani 1 1 d . . . H15A H 1.5619 0.7796 -0.2295 0.131 Uiso 1 1 calc R . . H15B H 1.5614 0.8771 -0.3563 0.131 Uiso 1 1 calc R . . H15C H 1.6397 0.7457 -0.3370 0.131 Uiso 1 1 calc R . . C16 C 1.5072(4) 0.8088(5) -0.5308(4) 0.0917(16) Uani 1 1 d . . . H16A H 1.4683 0.8038 -0.5784 0.138 Uiso 1 1 calc R . . H16B H 1.5864 0.7582 -0.5367 0.138 Uiso 1 1 calc R . . H16C H 1.5091 0.8901 -0.5572 0.138 Uiso 1 1 calc R . . C17 C 0.8219(3) 0.8488(4) 0.0717(3) 0.0541(9) Uani 1 1 d . . . C18 C 0.8857(4) 0.9259(5) -0.0150(4) 0.0916(15) Uani 1 1 d . . . H18 H 0.9572 0.8961 -0.0582 0.110 Uiso 1 1 calc R . . C19 C 0.8455(6) 1.0477(6) -0.0393(6) 0.124(2) Uani 1 1 d . . . H19 H 0.8921 1.0976 -0.0969 0.148 Uiso 1 1 calc R . . C20 C 0.7410(6) 1.0958(6) 0.0180(6) 0.115(2) Uani 1 1 d . . . H20 H 0.7139 1.1781 -0.0012 0.138 Uiso 1 1 calc R . . C21 C 0.6759(5) 1.0211(7) 0.1047(7) 0.131(3) Uani 1 1 d . . . H21 H 0.6036 1.0525 0.1459 0.157 Uiso 1 1 calc R . . C22 C 0.7156(4) 0.9006(5) 0.1317(5) 0.0999(17) Uani 1 1 d . . . H22 H 0.6701 0.8513 0.1923 0.120 Uiso 1 1 calc R . . C23 C 0.7568(3) 0.8696(3) -0.1907(3) 0.0523(9) Uani 1 1 d . . . C24 C 0.8182(4) 0.9357(5) -0.2946(5) 0.108(2) Uani 1 1 d . . . H24 H 0.8842 0.8967 -0.3361 0.129 Uiso 1 1 calc R . . C25 C 0.7825(6) 1.0605(6) -0.3383(6) 0.138(3) Uani 1 1 d . . . H25 H 0.8262 1.1040 -0.4075 0.166 Uiso 1 1 calc R . . C26 C 0.6860(7) 1.1184(6) -0.2817(8) 0.127(3) Uani 1 1 d . . . H26 H 0.6621 1.2017 -0.3112 0.152 Uiso 1 1 calc R . . C27 C 0.6244(6) 1.0546(6) -0.1819(6) 0.1130(19) Uani 1 1 d . . . H27 H 0.5570 1.0943 -0.1425 0.136 Uiso 1 1 calc R . . C28 C 0.6583(4) 0.9326(4) -0.1370(5) 0.0836(13) Uani 1 1 d . . . H28 H 0.6131 0.8911 -0.0677 0.100 Uiso 1 1 calc R . . C29A C 0.885(5) 0.948(5) 0.291(3) 0.194(16) Uani 0.50 1 d P . . C30A C 0.884(5) 0.961(3) 0.413(4) 0.200(13) Uani 0.50 1 d P . . C31A C 0.897(3) 0.824(2) 0.4921(18) 0.167(10) Uani 0.50 1 d P . . O1A O 0.870(3) 0.782(2) 0.435(3) 0.194(10) Uani 0.50 1 d P . . C32A C 0.891(5) 0.840(3) 0.328(3) 0.24(2) Uani 0.50 1 d P . . C29B C 0.791(2) 0.848(3) 0.434(2) 0.150(9) Uani 0.50 1 d P . . O1B O 0.7888(14) 0.951(2) 0.388(3) 0.233(9) Uani 0.50 1 d P . . C30B C 0.893(4) 0.981(3) 0.325(4) 0.166(15) Uani 0.50 1 d P . . C31B C 0.972(3) 0.858(5) 0.392(6) 0.29(3) Uani 0.50 1 d P . . C32B C 0.938(3) 0.763(4) 0.419(4) 0.187(19) Uani 0.50 1 d P . . 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 S1 0.0408(4) 0.0752(7) 0.0408(5) -0.0241(5) 0.0029(3) -0.0289(5) S2 0.0411(4) 0.0774(7) 0.0441(5) -0.0237(5) 0.0000(3) -0.0303(5) S3 0.0369(4) 0.0729(7) 0.0452(5) -0.0236(5) -0.0016(3) -0.0202(4) S4 0.0389(4) 0.0848(8) 0.0466(5) -0.0289(5) 0.0009(3) -0.0268(5) S5 0.0307(4) 0.0722(7) 0.0435(5) -0.0264(5) -0.0018(3) -0.0152(4) S6 0.0347(4) 0.0724(7) 0.0429(5) -0.0305(5) 0.0027(3) -0.0170(4) S7 0.0446(5) 0.0750(7) 0.0532(5) -0.0304(5) -0.0001(4) -0.0269(5) S8 0.0457(4) 0.0756(7) 0.0440(5) -0.0214(5) 0.0021(4) -0.0289(5) P1 0.0335(4) 0.0636(7) 0.0428(5) -0.0284(5) 0.0019(3) -0.0187(4) P2 0.0338(4) 0.0584(6) 0.0383(5) -0.0186(4) -0.0024(3) -0.0163(4) C1 0.0312(14) 0.046(2) 0.0406(18) -0.0189(16) -0.0007(12) -0.0110(14) C2 0.0294(14) 0.049(2) 0.0424(18) -0.0177(16) -0.0018(12) -0.0143(14) C3 0.0366(16) 0.055(2) 0.0441(19) -0.0196(17) 0.0001(13) -0.0175(16) C4 0.0332(15) 0.056(2) 0.048(2) -0.0207(18) -0.0008(13) -0.0149(16) C5 0.0344(17) 0.100(4) 0.051(2) -0.026(2) 0.0045(15) -0.0284(19) C6 0.0381(17) 0.109(4) 0.047(2) -0.035(2) 0.0043(15) -0.031(2) C7 0.058(3) 0.251(8) 0.060(3) -0.073(4) 0.018(2) -0.072(4) C8 0.053(2) 0.230(7) 0.079(3) -0.068(4) 0.005(2) -0.067(3) C9 0.0289(14) 0.048(2) 0.0445(19) -0.0215(17) -0.0013(12) -0.0104(14) C10 0.0304(14) 0.045(2) 0.0401(17) -0.0199(16) 0.0000(12) -0.0102(14) C11 0.0353(15) 0.054(2) 0.0447(19) -0.0241(17) -0.0027(13) -0.0101(15) C12 0.0360(16) 0.051(2) 0.0445(19) -0.0200(17) -0.0001(13) -0.0134(15) C13 0.0456(19) 0.068(3) 0.059(2) -0.022(2) 0.0014(16) -0.0274(19) C14 0.0459(18) 0.070(3) 0.053(2) -0.016(2) 0.0025(16) -0.0295(19) C15 0.067(3) 0.124(4) 0.088(3) -0.039(3) -0.002(2) -0.057(3) C16 0.081(3) 0.129(5) 0.061(3) -0.026(3) 0.016(2) -0.065(3) C17 0.0485(19) 0.065(3) 0.065(2) -0.041(2) 0.0006(16) -0.0222(19) C18 0.090(3) 0.071(4) 0.105(4) -0.052(3) 0.027(3) -0.032(3) C19 0.160(6) 0.081(5) 0.123(5) -0.056(4) 0.032(4) -0.060(4) C20 0.148(6) 0.066(4) 0.141(6) -0.064(4) -0.032(5) -0.006(4) C21 0.100(4) 0.107(6) 0.201(8) -0.112(6) 0.024(4) -0.026(4) C22 0.075(3) 0.092(4) 0.141(5) -0.082(4) 0.028(3) -0.029(3) C23 0.0469(19) 0.054(2) 0.053(2) -0.0110(19) -0.0181(16) -0.0161(18) C24 0.076(3) 0.084(4) 0.088(4) 0.016(3) -0.011(3) -0.013(3) C25 0.115(5) 0.087(5) 0.129(6) 0.040(4) -0.037(4) -0.037(4) C26 0.148(6) 0.056(4) 0.170(8) -0.005(5) -0.094(6) -0.013(4) C27 0.130(5) 0.067(4) 0.121(5) -0.035(4) -0.044(4) 0.009(4) C28 0.079(3) 0.061(3) 0.089(3) -0.026(3) -0.012(2) -0.005(3) C29A 0.30(4) 0.17(4) 0.12(2) -0.04(2) 0.00(2) -0.13(4) C30A 0.26(3) 0.15(3) 0.23(3) -0.08(3) -0.12(3) -0.03(2) C31A 0.26(3) 0.120(19) 0.134(16) -0.029(13) -0.034(16) -0.09(2) O1A 0.20(2) 0.085(14) 0.24(3) -0.048(16) -0.01(2) -0.029(15) C32A 0.51(7) 0.12(2) 0.104(16) -0.029(17) -0.12(3) -0.05(3) C29B 0.103(12) 0.113(19) 0.20(2) -0.055(19) 0.012(13) -0.039(13) O1B 0.143(12) 0.140(16) 0.34(3) -0.054(18) -0.028(16) -0.025(11) C30B 0.26(3) 0.111(19) 0.14(3) -0.05(2) 0.01(3) -0.10(2) C31B 0.127(19) 0.24(5) 0.41(7) -0.05(5) -0.02(3) -0.09(3) C32B 0.15(2) 0.18(3) 0.20(3) -0.12(3) -0.08(2) 0.09(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C1 1.753(3) . ? S1 C3 1.761(3) . ? S2 C3 1.748(3) . ? S2 C2 1.757(3) . ? S3 C4 1.744(3) . ? S3 C5 1.747(3) . ? S4 C6 1.745(3) . ? S4 C4 1.753(3) . ? S5 C11 1.751(3) . ? S5 C9 1.766(3) . ? S6 C11 1.758(3) . ? S6 C10 1.760(3) . ? S7 C12 1.750(3) . ? S7 C13 1.756(4) . ? S8 C12 1.740(3) . ? S8 C14 1.760(3) . ? P1 C9 1.812(3) . ? P1 C17 1.821(4) . ? P1 C1 1.825(3) . ? P2 C2 1.807(3) . ? P2 C10 1.818(3) . ? P2 C23 1.823(4) . ? C1 C2 1.339(4) . ? C3 C4 1.350(4) . ? C5 C6 1.319(5) . ? C5 C7 1.489(5) . ? C6 C8 1.510(5) . ? C9 C10 1.339(4) . ? C11 C12 1.351(4) . ? C13 C14 1.317(5) . ? C13 C15 1.511(5) . ? C14 C16 1.517(5) . ? C17 C18 1.368(6) . ? C17 C22 1.391(6) . ? C18 C19 1.384(7) . ? C19 C20 1.344(8) . ? C20 C21 1.359(8) . ? C21 C22 1.363(8) . ? C23 C28 1.364(6) . ? C23 C24 1.376(6) . ? C24 C25 1.394(8) . ? C25 C26 1.339(10) . ? C26 C27 1.338(9) . ? C27 C28 1.361(7) . ? C29A C30B 0.80(3) . ? C29A C32A 1.25(5) . ? C29A O1B 1.43(5) . ? C29A C30A 1.70(4) . ? C29A C31B 1.72(7) . ? C29A C29B 2.01(4) . ? C30A C30B 1.04(4) . ? C30A O1B 1.41(3) . ? C30A C31B 1.46(7) . ? C30A C31A 1.58(4) . ? C31A O1A 1.30(3) . ? C31A C31B 1.32(5) . ? C31A C32B 1.37(4) . ? C31A C29B 1.63(4) . ? O1A C32B 0.77(3) . ? O1A C29B 1.04(3) . ? O1A C32A 1.25(4) . ? O1A C31B 1.69(4) . ? C32A C32B 1.32(4) . ? C32A C29B 1.53(5) . ? C32A C31B 1.67(6) . ? C32A O1B 1.82(4) . ? C32A C30B 1.84(4) . ? C29B O1B 1.18(3) . ? C29B C32B 1.75(3) . ? O1B C30B 1.38(4) . ? C30B C31B 1.55(7) . ? C31B C32B 1.31(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 S1 C3 95.17(14) . . ? C3 S2 C2 95.44(14) . . ? C4 S3 C5 95.22(15) . . ? C6 S4 C4 94.83(15) . . ? C11 S5 C9 93.97(14) . . ? C11 S6 C10 93.92(14) . . ? C12 S7 C13 95.37(16) . . ? C12 S8 C14 95.45(16) . . ? C9 P1 C17 101.49(16) . . ? C9 P1 C1 99.70(13) . . ? C17 P1 C1 100.92(15) . . ? C2 P2 C10 99.73(13) . . ? C2 P2 C23 101.69(17) . . ? C10 P2 C23 100.96(15) . . ? C2 C1 S1 117.3(2) . . ? C2 C1 P1 128.4(2) . . ? S1 C1 P1 114.12(16) . . ? C1 C2 S2 117.1(2) . . ? C1 C2 P2 128.3(2) . . ? S2 C2 P2 114.51(16) . . ? C4 C3 S2 123.7(2) . . ? C4 C3 S1 122.1(3) . . ? S2 C3 S1 114.06(16) . . ? C3 C4 S3 123.5(2) . . ? C3 C4 S4 122.4(3) . . ? S3 C4 S4 114.05(16) . . ? C6 C5 C7 127.9(3) . . ? C6 C5 S3 117.2(3) . . ? C7 C5 S3 114.9(3) . . ? C5 C6 C8 127.9(3) . . ? C5 C6 S4 117.8(2) . . ? C8 C6 S4 114.2(3) . . ? C10 C9 S5 116.6(2) . . ? C10 C9 P1 128.2(2) . . ? S5 C9 P1 115.11(16) . . ? C9 C10 S6 116.8(2) . . ? C9 C10 P2 128.5(2) . . ? S6 C10 P2 114.57(16) . . ? C12 C11 S5 124.3(2) . . ? C12 C11 S6 122.9(3) . . ? S5 C11 S6 112.76(16) . . ? C11 C12 S8 123.4(2) . . ? C11 C12 S7 122.9(3) . . ? S8 C12 S7 113.75(16) . . ? C14 C13 C15 128.1(3) . . ? C14 C13 S7 117.2(3) . . ? C15 C13 S7 114.6(3) . . ? C13 C14 C16 128.4(3) . . ? C13 C14 S8 117.2(3) . . ? C16 C14 S8 114.4(3) . . ? C18 C17 C22 116.0(4) . . ? C18 C17 P1 124.0(3) . . ? C22 C17 P1 120.0(3) . . ? C17 C18 C19 121.0(5) . . ? C20 C19 C18 121.8(6) . . ? C19 C20 C21 118.3(6) . . ? C20 C21 C22 120.6(6) . . ? C21 C22 C17 122.2(5) . . ? C28 C23 C24 116.5(4) . . ? C28 C23 P2 124.7(3) . . ? C24 C23 P2 118.7(4) . . ? C23 C24 C25 120.6(6) . . ? C26 C25 C24 120.7(6) . . ? C27 C26 C25 118.9(6) . . ? C26 C27 C28 121.4(7) . . ? C27 C28 C23 121.8(5) . . ? C30B C29A C32A 126(7) . . ? C30B C29A O1B 70(5) . . ? C32A C29A O1B 85(3) . . ? C30B C29A C30A 26(4) . . ? C32A C29A C30A 101(3) . . ? O1B C29A C30A 52.9(19) . . ? C30B C29A C31B 65(6) . . ? C32A C29A C31B 66(4) . . ? O1B C29A C31B 86(3) . . ? C30A C29A C31B 51(3) . . ? C30B C29A C29B 93(5) . . ? C32A C29A C29B 50(3) . . ? O1B C29A C29B 35.6(14) . . ? C30A C29A C29B 68(2) . . ? C31B C29A C29B 71.3(18) . . ? C30B C30A O1B 66(3) . . ? C30B C30A C31B 75(5) . . ? O1B C30A C31B 97(3) . . ? C30B C30A C31A 113(3) . . ? O1B C30A C31A 83(3) . . ? C31B C30A C31A 51(2) . . ? C30B C30A C29A 20(2) . . ? O1B C30A C29A 54(2) . . ? C31B C30A C29A 65(3) . . ? C31A C30A C29A 95(2) . . ? O1A C31A C31B 81(3) . . ? O1A C31A C32B 33.2(19) . . ? C31B C31A C32B 58(3) . . ? O1A C31A C30A 105(2) . . ? C31B C31A C30A 60(3) . . ? C32B C31A C30A 107(3) . . ? O1A C31A C29B 39.6(18) . . ? C31B C31A C29B 95(3) . . ? C32B C31A C29B 71(2) . . ? C30A C31A C29B 81(2) . . ? C32B O1A C29B 151(6) . . ? C32B O1A C32A 78(5) . . ? C29B O1A C32A 83(3) . . ? C32B O1A C31A 79(5) . . ? C29B O1A C31A 88(3) . . ? C32A O1A C31A 112(3) . . ? C32B O1A C31B 48(5) . . ? C29B O1A C31B 104(3) . . ? C32A O1A C31B 67(3) . . ? C31A O1A C31B 50(3) . . ? O1A C32A C29A 119(3) . . ? O1A C32A C32B 35(2) . . ? C29A C32A C32B 120(4) . . ? O1A C32A C29B 42(2) . . ? C29A C32A C29B 92(3) . . ? C32B C32A C29B 75(2) . . ? O1A C32A C31B 69(2) . . ? C29A C32A C31B 70(3) . . ? C32B C32A C31B 50(3) . . ? C29B C32A C31B 86(2) . . ? O1A C32A O1B 76(2) . . ? C29A C32A O1B 52(2) . . ? C32B C32A O1B 99(2) . . ? C29B C32A O1B 40.3(15) . . ? C31B C32A O1B 76(3) . . ? O1A C32A C30B 100(2) . . ? C29A C32A C30B 21(2) . . ? C32B C32A C30B 100(3) . . ? C29B C32A C30B 81(2) . . ? C31B C32A C30B 52(3) . . ? O1B C32A C30B 44.3(17) . . ? O1A C29B O1B 121(2) . . ? O1A C29B C32A 54(2) . . ? O1B C29B C32A 83(2) . . ? O1A C29B C31A 53(2) . . ? O1B C29B C31A 89(2) . . ? C32A C29B C31A 84(2) . . ? O1A C29B C32B 12(3) . . ? O1B C29B C32B 109(3) . . ? C32A C29B C32B 47(2) . . ? C31A C29B C32B 48(2) . . ? O1A C29B C29A 84(2) . . ? O1B C29B C29A 45(2) . . ? C32A C29B C29A 38.5(18) . . ? C31A C29B C29A 82.8(18) . . ? C32B C29B C29A 72(3) . . ? C29B O1B C30B 118(2) . . ? C29B O1B C30A 107(3) . . ? C30B O1B C30A 43.8(19) . . ? C29B O1B C29A 100(3) . . ? C30B O1B C29A 33.1(14) . . ? C30A O1B C29A 73(2) . . ? C29B O1B C32A 57(2) . . ? C30B O1B C32A 69(2) . . ? C30A O1B C32A 90(2) . . ? C29A O1B C32A 43(2) . . ? C29A C30B C30A 134(6) . . ? C29A C30B O1B 77(6) . . ? C30A C30B O1B 70(3) . . ? C29A C30B C31B 87(6) . . ? C30A C30B C31B 65(5) . . ? O1B C30B C31B 95(2) . . ? C29A C30B C32A 33(5) . . ? C30A C30B C32A 102(3) . . ? O1B C30B C32A 67(2) . . ? C31B C30B C32A 58(3) . . ? C32B C31B C31A 63(2) . . ? C32B C31B C30A 118(3) . . ? C31A C31B C30A 69(4) . . ? C32B C31B C30B 116(4) . . ? C31A C31B C30B 100(4) . . ? C30A C31B C30B 40(2) . . ? C32B C31B C32A 51(3) . . ? C31A C31B C32A 89(3) . . ? C30A C31B C32A 94(3) . . ? C30B C31B C32A 69(3) . . ? C32B C31B O1A 25.9(12) . . ? C31A C31B O1A 49.0(15) . . ? C30A C31B O1A 93(3) . . ? C30B C31B O1A 95(3) . . ? C32A C31B O1A 44(2) . . ? C32B C31B C29A 93(4) . . ? C31A C31B C29A 105(3) . . ? C30A C31B C29A 64(3) . . ? C30B C31B C29A 27.8(16) . . ? C32A C31B C29A 43(2) . . ? O1A C31B C29A 78(3) . . ? O1A C32B C31B 106(5) . . ? O1A C32B C32A 68(4) . . ? C31B C32B C32A 79(4) . . ? O1A C32B C31A 68(4) . . ? C31B C32B C31A 59(3) . . ? C32A C32B C31A 103(3) . . ? O1A C32B C29B 17(3) . . ? C31B C32B C29B 90(2) . . ? C32A C32B C29B 58(2) . . ? C31A C32B C29B 61(2) . . ? _diffrn_measured_fraction_theta_max 0.916 _diffrn_reflns_theta_full 25.90 _diffrn_measured_fraction_theta_full 0.916 _refine_diff_density_max 0.483 _refine_diff_density_min -0.293 _refine_diff_density_rms 0.058 #===END data_(cis-1-O2)2Mo6O19 _database_code_depnum_ccdc_archive 'CCDC 239193' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(cis-(o-DMTTF)2(PhPO)2)2(Mo6O19), 2H2O' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H48 Mo6 O25 P4 S16' _chemical_formula_weight 2333.42 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 20.573(3) _cell_length_b 14.086(2) _cell_length_c 14.0657(15) _cell_angle_alpha 90.00 _cell_angle_beta 100.809(14) _cell_angle_gamma 90.00 _cell_volume 4003.8(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 4.4 _cell_measurement_theta_max 50.4 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.366 _exptl_crystal_size_mid 0.123 _exptl_crystal_size_min 0.116 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.936 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2304 _exptl_absorpt_coefficient_mu 1.481 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.6964 _exptl_absorpt_correction_T_max 0.9262 _exptl_absorpt_process_details multiscan _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 STOE-IPDS _diffrn_measurement_method 'Oscillation, Phi. incr. = 1.1' _diffrn_detector_area_resol_mean 6.6 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15710 _diffrn_reflns_av_R_equivalents 0.1367 _diffrn_reflns_av_sigmaI/netI 0.1148 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 25.77 _reflns_number_total 3917 _reflns_number_gt 2113 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE [STOE-IPDS]' _computing_cell_refinement 'SELECT, CELL [STOE-IPDS]' _computing_data_reduction 'INTEGRATE [STOE-IPDS]' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1359P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3917 _refine_ls_number_parameters 256 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1336 _refine_ls_R_factor_gt 0.0786 _refine_ls_wR_factor_ref 0.2227 _refine_ls_wR_factor_gt 0.1898 _refine_ls_goodness_of_fit_ref 0.928 _refine_ls_restrained_S_all 0.928 _refine_ls_shift/su_max 0.030 _refine_ls_shift/su_mean 0.003 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 0.47447(5) 0.11628(7) 0.10345(7) 0.0498(3) Uani 1 1 d . . . Mo2 Mo 0.60898(7) 0.0000 0.08150(10) 0.0518(4) Uani 1 2 d S . . O1 O 0.5000 0.0000 0.0000 0.037(3) Uani 1 4 d S . . O2 O 0.6874(6) 0.0000 0.1409(9) 0.077(4) Uani 1 2 d S . . O3 O 0.5000 0.1880(7) 0.0000 0.053(3) Uani 1 2 d S . . O4 O 0.3915(4) 0.0939(6) 0.0164(6) 0.060(2) Uani 1 1 d . . . O5 O 0.5662(4) 0.0936(6) 0.1499(5) 0.0539(19) Uani 1 1 d . . . O6 O 0.4578(5) 0.0000 0.1675(8) 0.053(3) Uani 1 2 d S . . O7 O 0.4544(4) 0.1993(6) 0.1790(6) 0.068(2) Uani 1 1 d . . . P1 P 0.26435(13) 0.12286(18) 0.3522(2) 0.0434(7) Uani 1 1 d . . . S1 S 0.41190(12) 0.10376(18) 0.3767(2) 0.0419(6) Uani 1 1 d . . . S2 S 0.56879(13) 0.10228(19) 0.3809(2) 0.0466(7) Uani 1 1 d . . . S3 S 0.14153(14) 0.1032(2) 0.4430(2) 0.0543(8) Uani 1 1 d . . . S4 S -0.01870(15) 0.1038(2) 0.3630(3) 0.0637(9) Uani 1 1 d . . . O8 O 0.2858(4) 0.2134(5) 0.4117(6) 0.0520(19) Uani 1 1 d . . . C1 C 0.3358(5) 0.0460(7) 0.3579(8) 0.042(2) Uani 1 1 d . . . C2 C 0.4626(6) 0.0000 0.3769(8) 0.021(2) Uani 1 2 d S . . C3 C 0.5246(7) 0.0000 0.3833(10) 0.041(3) Uani 1 2 d S . . C4 C 0.6424(5) 0.0486(8) 0.3717(8) 0.051(3) Uani 1 1 d . . . C5 C 0.6986(7) 0.1096(10) 0.3572(10) 0.072(4) Uani 1 1 d . . . H5A H 0.6863 0.1752 0.3603 0.108 Uiso 1 1 calc R . . H5B H 0.7094 0.0965 0.2950 0.108 Uiso 1 1 calc R . . H5C H 0.7363 0.0967 0.4070 0.108 Uiso 1 1 calc R . . C6 C 0.2081(5) 0.0503(7) 0.3991(8) 0.047(3) Uani 1 1 d . . . C7 C 0.0926(8) 0.0000 0.4241(13) 0.056(4) Uani 1 2 d S . . C8 C 0.0280(7) 0.0000 0.3885(11) 0.051(4) Uani 1 2 d S . . C9 C -0.0900(5) 0.0471(8) 0.3001(8) 0.055(3) Uani 1 1 d . . . C10 C -0.1449(7) 0.1131(11) 0.2558(12) 0.086(5) Uani 1 1 d . . . H10A H -0.1306 0.1777 0.2673 0.129 Uiso 1 1 calc R . . H10B H -0.1830 0.1019 0.2844 0.129 Uiso 1 1 calc R . . H10C H -0.1560 0.1019 0.1873 0.129 Uiso 1 1 calc R . . C11 C 0.2313(5) 0.1386(7) 0.2269(9) 0.049(3) Uani 1 1 d . . . C12 C 0.2690(7) 0.1224(11) 0.1572(11) 0.079(4) Uani 1 1 d . . . H12 H 0.3124 0.1009 0.1734 0.095 Uiso 1 1 calc R . . C13 C 0.2392(9) 0.1394(15) 0.0619(12) 0.110(7) Uani 1 1 d . . . H13 H 0.2638 0.1286 0.0139 0.132 Uiso 1 1 calc R . . C14 C 0.1787(10) 0.1696(15) 0.0358(12) 0.110(6) Uani 1 1 d . . . H14 H 0.1619 0.1816 -0.0291 0.132 Uiso 1 1 calc R . . C15 C 0.1394(9) 0.1840(15) 0.1041(13) 0.110(6) Uani 1 1 d . . . H15 H 0.0960 0.2049 0.0857 0.132 Uiso 1 1 calc R . . C16 C 0.1658(8) 0.1670(11) 0.2004(10) 0.081(4) Uani 1 1 d . . . H16 H 0.1397 0.1745 0.2472 0.097 Uiso 1 1 calc R . . OW O 0.0145(10) 0.0000 0.9105(14) 0.171(11) Uani 1 2 d S . . 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 0.0565(6) 0.0575(6) 0.0355(6) -0.0053(4) 0.0092(4) 0.0035(4) Mo2 0.0405(7) 0.0736(10) 0.0381(8) 0.000 -0.0010(6) 0.000 O1 0.036(7) 0.057(8) 0.016(7) 0.000 0.000(5) 0.000 O2 0.038(6) 0.129(11) 0.059(8) 0.000 -0.007(5) 0.000 O3 0.060(6) 0.058(6) 0.035(6) 0.000 -0.007(5) 0.000 O4 0.050(4) 0.073(5) 0.056(5) 0.006(4) 0.006(4) 0.015(4) O5 0.048(4) 0.070(5) 0.041(5) -0.012(4) 0.002(3) -0.007(4) O6 0.049(6) 0.065(7) 0.043(7) 0.000 0.008(5) 0.000 O7 0.076(6) 0.074(6) 0.059(6) -0.019(4) 0.021(5) 0.001(4) P1 0.0376(13) 0.0424(14) 0.0495(17) 0.0031(12) 0.0059(12) 0.0029(11) S1 0.0388(13) 0.0430(14) 0.0441(16) 0.0030(11) 0.0081(11) -0.0005(10) S2 0.0443(14) 0.0494(15) 0.0450(16) 0.0034(12) 0.0061(11) -0.0043(11) S3 0.0437(14) 0.0545(17) 0.066(2) -0.0048(14) 0.0153(13) 0.0019(12) S4 0.0464(16) 0.0638(19) 0.078(2) 0.0048(16) 0.0031(15) 0.0061(14) O8 0.065(5) 0.036(4) 0.057(5) -0.003(3) 0.018(4) 0.007(3) C1 0.036(5) 0.045(5) 0.044(6) -0.011(5) 0.006(4) -0.004(4) C2 0.036(7) 0.010(5) 0.014(6) 0.000 -0.005(5) 0.000 C3 0.040(8) 0.051(8) 0.033(8) 0.000 0.007(6) 0.000 C4 0.044(6) 0.076(7) 0.032(6) 0.003(5) 0.005(5) -0.002(5) C5 0.065(8) 0.078(9) 0.064(9) 0.001(7) -0.011(7) -0.023(7) C6 0.045(6) 0.041(5) 0.054(7) -0.002(5) 0.003(5) 0.007(4) C7 0.048(9) 0.070(11) 0.050(10) 0.000 0.010(8) 0.000 C8 0.030(7) 0.080(11) 0.040(9) 0.000 0.002(6) 0.000 C9 0.041(6) 0.081(7) 0.046(7) 0.007(6) 0.014(5) -0.009(5) C10 0.054(8) 0.115(12) 0.089(12) 0.037(10) 0.011(7) 0.011(8) C11 0.051(6) 0.038(5) 0.055(7) 0.006(5) 0.003(5) 0.014(5) C12 0.058(8) 0.112(12) 0.067(10) 0.031(9) 0.008(7) 0.013(8) C13 0.085(12) 0.183(19) 0.059(10) 0.033(11) 0.009(8) 0.058(12) C14 0.129(16) 0.151(17) 0.045(9) 0.010(10) 0.006(10) 0.038(13) C15 0.085(11) 0.170(18) 0.070(12) 0.029(12) 0.002(9) 0.045(12) C16 0.079(10) 0.107(11) 0.054(9) 0.003(8) 0.004(7) 0.027(9) OW 0.100(14) 0.36(4) 0.069(12) 0.000 0.056(11) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O7 1.683(8) . ? Mo1 O5 1.904(7) . ? Mo1 O3 1.924(6) . ? Mo1 O6 1.931(6) . ? Mo1 O4 1.931(8) . ? Mo1 O1 2.3157(10) . ? Mo2 O2 1.673(11) . ? Mo2 O4 1.908(9) 2_655 ? Mo2 O4 1.908(9) 5_655 ? Mo2 O5 1.938(8) . ? Mo2 O5 1.938(8) 6 ? Mo2 O1 2.3188(13) . ? O1 Mo1 2.3157(10) 5_655 ? O1 Mo1 2.3157(10) 6 ? O1 Mo1 2.3157(10) 2_655 ? O1 Mo2 2.3188(13) 5_655 ? O3 Mo1 1.924(6) 2_655 ? O4 Mo2 1.908(9) 5_655 ? O6 Mo1 1.931(6) 6 ? P1 O8 1.543(7) . ? P1 C6 1.761(12) . ? P1 C11 1.781(12) . ? P1 C1 1.816(10) . ? S1 C1 1.739(10) . ? S1 C2 1.795(7) . ? S2 C3 1.707(8) . ? S2 C4 1.720(11) . ? S3 C7 1.760(9) . ? S3 C6 1.770(11) . ? S4 C9 1.757(11) . ? S4 C8 1.750(8) . ? C1 C1 1.297(19) 6 ? C2 C3 1.264(18) . ? C2 S1 1.795(7) 6 ? C3 S2 1.707(8) 6 ? C4 C4 1.37(2) 6 ? C4 C5 1.484(17) . ? C6 C6 1.42(2) 6 ? C7 C8 1.33(2) . ? C7 S3 1.760(9) 6 ? C8 S4 1.750(8) 6 ? C9 C9 1.33(2) 6 ? C9 C10 1.505(17) . ? C11 C16 1.387(17) . ? C11 C12 1.378(19) . ? C12 C13 1.39(2) . ? C13 C14 1.30(2) . ? C14 C15 1.38(2) . ? C15 C16 1.38(2) . ? 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 O7 Mo1 O5 104.1(4) . . ? O7 Mo1 O3 104.3(4) . . ? O5 Mo1 O3 87.4(3) . . ? O7 Mo1 O6 102.0(4) . . ? O5 Mo1 O6 87.1(4) . . ? O3 Mo1 O6 153.7(4) . . ? O7 Mo1 O4 102.8(4) . . ? O5 Mo1 O4 153.1(3) . . ? O3 Mo1 O4 86.6(3) . . ? O6 Mo1 O4 86.8(4) . . ? O7 Mo1 O1 178.7(3) . . ? O5 Mo1 O1 76.7(2) . . ? O3 Mo1 O1 76.7(3) . . ? O6 Mo1 O1 77.0(3) . . ? O4 Mo1 O1 76.3(2) . . ? O2 Mo2 O4 103.6(4) . 2_655 ? O2 Mo2 O4 103.6(4) . 5_655 ? O4 Mo2 O4 87.7(5) 2_655 5_655 ? O2 Mo2 O5 103.7(4) . . ? O4 Mo2 O5 86.9(4) 2_655 . ? O4 Mo2 O5 152.7(3) 5_655 . ? O2 Mo2 O5 103.7(4) . 6 ? O4 Mo2 O5 152.7(3) 2_655 6 ? O4 Mo2 O5 86.9(4) 5_655 6 ? O5 Mo2 O5 85.7(5) . 6 ? O2 Mo2 O1 179.6(5) . . ? O4 Mo2 O1 76.7(2) 2_655 . ? O4 Mo2 O1 76.7(2) 5_655 . ? O5 Mo2 O1 76.0(2) . . ? O5 Mo2 O1 76.0(2) 6 . ? Mo1 O1 Mo1 89.97(5) 5_655 6 ? Mo1 O1 Mo1 180.00(7) 5_655 . ? Mo1 O1 Mo1 90.03(5) 6 . ? Mo1 O1 Mo1 90.03(5) 5_655 2_655 ? Mo1 O1 Mo1 180.00(7) 6 2_655 ? Mo1 O1 Mo1 89.97(5) . 2_655 ? Mo1 O1 Mo2 89.91(4) 5_655 . ? Mo1 O1 Mo2 90.09(4) 6 . ? Mo1 O1 Mo2 90.09(4) . . ? Mo1 O1 Mo2 89.91(4) 2_655 . ? Mo1 O1 Mo2 90.09(4) 5_655 5_655 ? Mo1 O1 Mo2 89.91(4) 6 5_655 ? Mo1 O1 Mo2 89.91(4) . 5_655 ? Mo1 O1 Mo2 90.09(4) 2_655 5_655 ? Mo2 O1 Mo2 180.00(8) . 5_655 ? Mo1 O3 Mo1 116.6(5) 2_655 . ? Mo2 O4 Mo1 117.0(4) 5_655 . ? Mo1 O5 Mo2 117.2(4) . . ? Mo1 O6 Mo1 116.0(6) 6 . ? O8 P1 C6 114.7(5) . . ? O8 P1 C11 116.8(5) . . ? C6 P1 C11 106.7(5) . . ? O8 P1 C1 108.8(4) . . ? C6 P1 C1 102.8(5) . . ? C11 P1 C1 105.9(5) . . ? C1 S1 C2 97.2(5) . . ? C3 S2 C4 96.3(6) . . ? C7 S3 C6 93.3(6) . . ? C9 S4 C8 95.6(6) . . ? C1 C1 S1 117.9(3) 6 . ? C1 C1 P1 126.6(3) 6 . ? S1 C1 P1 115.2(5) . . ? C3 C2 S1 125.4(3) . 6 ? C3 C2 S1 125.4(3) . . ? S1 C2 S1 109.1(6) 6 . ? C2 C3 S2 122.2(4) . . ? C2 C3 S2 122.2(4) . 6 ? S2 C3 S2 115.2(8) . 6 ? C4 C4 C5 125.4(7) 6 . ? C4 C4 S2 116.1(4) 6 . ? C5 C4 S2 118.4(9) . . ? C6 C6 P1 125.5(3) 6 . ? C6 C6 S3 114.9(4) 6 . ? P1 C6 S3 119.5(6) . . ? C8 C7 S3 124.0(5) . . ? C8 C7 S3 124.0(5) . 6 ? S3 C7 S3 111.4(9) . 6 ? C7 C8 S4 123.3(4) . 6 ? C7 C8 S4 123.3(4) . . ? S4 C8 S4 113.3(8) 6 . ? C9 C9 C10 128.2(8) 6 . ? C9 C9 S4 117.0(4) 6 . ? C10 C9 S4 114.8(9) . . ? C16 C11 C12 120.3(12) . . ? C16 C11 P1 118.2(10) . . ? C12 C11 P1 121.5(9) . . ? C13 C12 C11 116.9(14) . . ? C14 C13 C12 123.7(17) . . ? C13 C14 C15 120.3(16) . . ? C14 C15 C16 118.9(16) . . ? C11 C16 C15 119.7(15) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.77 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 3.381 _refine_diff_density_min -0.938 _refine_diff_density_rms 0.205