# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2004 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 _journal_volume ? _journal_year ? _journal_page_first ? # 1. SUBMISSION DETAILS _publ_contact_author ; ProfD Ernesto Carmona Departamento de Qu\'imica Inorg\'anica-Instituto de Investigaciones Qu\'imicas Universidad de Sevilla-Consejo Superior de Investigaciones Cient\'ificas Avda. Am\'erico Vespucio s/n Isla de la Cartuja Sevilla E-41092 SPAIN ; _publ_contact_author_email GUZMAN@US.ES _publ_contact_letter ; ? ; #=========================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Novel Carbon Dioxide and Carbonyl-Carbonate complexes of Molibdenum.The X-ray structure of trans-[Mo(CO2)2(HN(CH2CH2PMe2)2)(PMe3)] and [Mo3(CO3)(O)2(O)2(CO)2(H2O)(PMe3)6].H2O ; loop_ _publ_author_name _publ_author_address 'Leopoldo Contreras' ; Departamento de Qu\'imica Inorg\'anica-Instituto de Investigaciones Qu\'imicas Universidad de Sevilla-Consejo Superior de Investigaciones Cient\'ificas c/ Am\'erico Vespucio s/n Isla de la Cartuja 41092 Sevilla Spain ; 'Margarita Paneque' ; Departamento de Qu\'imica Inorg\'anica-Instituto de Investigaciones Qu\'imicas Universidad de Sevilla-Consejo Superior de Investigaciones Cient\'ificas c/ Am\'erico Vespucio s/n Isla de la Cartuja 41092 Sevilla Spain ; 'Murielle Sellin' ; Departamento de Qu\'imica Inorg\'anica-Instituto de Investigaciones Qu\'imicas Universidad de Sevilla-Consejo Superior de Investigaciones Cient\'ificas c/ Am\'erico Vespucio s/n Isla de la Cartuja 41092 Sevilla Spain ; 'Ernesto Carmona' ; Departamento de Qu\'imica Inorg\'anica-Instituto de Investigaciones Qu\'imicas Universidad de Sevilla-Consejo Superior de Investigaciones Cient\'ificas c/ Am\'erico Vespucio s/n Isla de la Cartuja 41092 Sevilla Spain ; P.J.Perez ; Departamento de Qu\'imica y Ciencia de los Materiales Universidad de Huleva Carretera de Palos de la Frontera s/n 21819 Huelva Spain ; 'Enrique Gutierrez Puebla' ; Instituto de Ciencia de Materiales CSIC Campus de Cantoblanco 28049 MADRID Spain ; ; A.Monge ; ; Instituto de Ciencia de Materiales CSIC Campus de Cantoblanco 28049 MADRID Spain ; 'Caridad Ruiz' ; Instituto de Ciencia de Materiales CSIC Campus de Cantoblanco 28049 MADRID Spain ; #=========================================================================== #========================================================================== #===== # 4. TEXT _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_experimental ; ; _publ_section_references ; ; _publ_section_figure_captions ; ; _publ_section_acknowledgements ; ; _publ_contact_author_name 'ProfD Ernesto Carmona' #=========================================================================== data_mse11 _database_code_depnum_ccdc_archive 'CCDC 231960' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H30 N O4 P3 Mo ( C3 H8 )0.5' _chemical_formula_weight 474.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.947(5) _cell_length_b 11.670(2) _cell_length_c 20.004(7) _cell_angle_alpha 90.00 _cell_angle_beta 101.878(10) _cell_angle_gamma 90.00 _cell_volume 4557(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1944 _exptl_absorpt_coefficient_mu 0.801 _exptl_absorpt_correction_type ? _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 'NONIUS CAD4' _diffrn_measurement_method '2O/w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5616 _diffrn_reflns_av_R_equivalents 0.0435 _diffrn_reflns_av_sigmaI/netI 0.1840 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 28.01 _reflns_number_total 5459 _reflns_number_gt 2281 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS CAD4' _computing_cell_refinement 'NONIUS CAD4' _computing_data_reduction 'NONIUS CAD4' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w==1/[\s^2^(Fo^2^)+(0.1387P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5459 _refine_ls_number_parameters 207 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2355 _refine_ls_R_factor_gt 0.0645 _refine_ls_wR_factor_ref 0.2384 _refine_ls_wR_factor_gt 0.1734 _refine_ls_goodness_of_fit_ref 0.911 _refine_ls_restrained_S_all 0.911 _refine_ls_shift/su_max 0.140 _refine_ls_shift/su_mean 0.009 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 0.86278(4) 0.38638(6) 0.90271(4) 0.0466(3) Uani 1 1 d . . . P1 P 0.85877(13) 0.4097(3) 0.78103(12) 0.0630(7) Uani 1 1 d . . . C11 C 0.7773(5) 0.4443(10) 0.7269(5) 0.080(3) Uani 1 1 d . . . H11A H 0.7612 0.5160 0.7411 0.120 Uiso 1 1 calc R . . H11B H 0.7448 0.3851 0.7304 0.120 Uiso 1 1 calc R . . H11C H 0.7825 0.4503 0.6804 0.120 Uiso 1 1 calc R . . C12 C 0.9094(6) 0.5257(14) 0.7574(6) 0.118(5) Uani 1 1 d . . . H12A H 0.9552 0.5215 0.7842 0.177 Uiso 1 1 calc R . . H12B H 0.8893 0.5977 0.7656 0.177 Uiso 1 1 calc R . . H12C H 0.9108 0.5195 0.7098 0.177 Uiso 1 1 calc R . . C13 C 0.8860(6) 0.2874(14) 0.7384(6) 0.120(6) Uani 1 1 d . . . H13A H 0.9262 0.2547 0.7667 0.180 Uiso 1 1 calc R . . H13B H 0.8963 0.3111 0.6957 0.180 Uiso 1 1 calc R . . H13C H 0.8500 0.2313 0.7302 0.180 Uiso 1 1 calc R . . P2 P 0.78326(14) 0.5442(2) 0.91618(14) 0.0663(7) Uani 1 1 d . . . C21 C 0.6912(5) 0.5202(13) 0.8961(6) 0.104(4) Uani 1 1 d . . . H21A H 0.6805 0.4534 0.9198 0.157 Uiso 1 1 calc R . . H21B H 0.6763 0.5090 0.8478 0.157 Uiso 1 1 calc R . . H21C H 0.6683 0.5856 0.9101 0.157 Uiso 1 1 calc R . . C22 C 0.7929(7) 0.6852(9) 0.8837(7) 0.105(4) Uani 1 1 d . . . H22A H 0.7789 0.6848 0.8349 0.157 Uiso 1 1 calc R . . H22B H 0.8400 0.7083 0.8964 0.157 Uiso 1 1 calc R . . H22C H 0.7649 0.7381 0.9026 0.157 Uiso 1 1 calc R . . C23 C 0.8055(6) 0.5627(11) 1.0076(6) 0.085(3) Uani 1 1 d . . . H23A H 0.8434 0.6160 1.0190 0.101 Uiso 1 1 calc R . . H23B H 0.7668 0.5950 1.0235 0.101 Uiso 1 1 calc R . . C24 C 0.8255(6) 0.4492(11) 1.0437(5) 0.081(3) Uani 1 1 d . . . H24A H 0.8389 0.4616 1.0926 0.097 Uiso 1 1 calc R . . H24B H 0.7867 0.3973 1.0353 0.097 Uiso 1 1 calc R . . P3 P 0.92660(14) 0.2089(2) 0.93358(14) 0.0671(7) Uani 1 1 d . . . C31 C 0.8787(7) 0.0760(10) 0.9322(6) 0.095(4) Uani 1 1 d . . . H31A H 0.8345 0.0919 0.9419 0.142 Uiso 1 1 calc R . . H31B H 0.9032 0.0245 0.9660 0.142 Uiso 1 1 calc R . . H31C H 0.8732 0.0413 0.8879 0.142 Uiso 1 1 calc R . . C32 C 1.0010(6) 0.1610(12) 0.9044(7) 0.103(4) Uani 1 1 d . . . H32A H 1.0357 0.2194 0.9131 0.155 Uiso 1 1 calc R . . H32B H 0.9891 0.1459 0.8562 0.155 Uiso 1 1 calc R . . H32C H 1.0182 0.0922 0.9282 0.155 Uiso 1 1 calc R . . C33 C 0.9585(6) 0.2344(10) 1.0250(5) 0.088(3) Uani 1 1 d . . . H33A H 0.9708 0.1621 1.0482 0.106 Uiso 1 1 calc R . . H33B H 0.9991 0.2821 1.0316 0.106 Uiso 1 1 calc R . . C34 C 0.9040(7) 0.2929(10) 1.0547(5) 0.085(3) Uani 1 1 d . . . H34A H 0.8650 0.2421 1.0516 0.103 Uiso 1 1 calc R . . H34B H 0.9217 0.3094 1.1026 0.103 Uiso 1 1 calc R . . N1 N 0.8821(4) 0.3992(7) 1.0183(3) 0.059(2) Uani 1 1 d . . . H1 H 0.9177 0.4489 1.0304 0.05(2) Uiso 1 1 calc R . . C1 C 0.7829(5) 0.2787(8) 0.8568(5) 0.057(2) Uani 1 1 d . . . O1 O 0.7829(3) 0.2798(5) 0.9210(3) 0.0616(16) Uani 1 1 d . . . O2 O 0.7464(4) 0.2306(6) 0.8101(4) 0.084(2) Uani 1 1 d . . . C2 C 0.9633(5) 0.4418(10) 0.9098(4) 0.060(2) Uani 1 1 d . . . O3 O 0.9296(3) 0.5313(6) 0.9110(3) 0.0596(16) Uani 1 1 d . . . O4 O 1.0250(3) 0.4258(7) 0.9127(3) 0.077(2) Uani 1 1 d . . . C3 C 0.9201 0.8641 0.7743 0.050 Uiso 0.50 1 d P . . C4 C 0.9816 0.1058 0.2089 0.050 Uiso 0.50 1 d P . . C5 C 0.5582 0.3591 0.7614 0.050 Uiso 0.25 1 d P . . C6 C 0.5276 0.4322 0.7540 0.050 Uiso 0.25 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 Mo1 0.0474(4) 0.0540(4) 0.0392(4) -0.0015(4) 0.0108(3) -0.0081(4) P1 0.0588(14) 0.089(2) 0.0418(12) 0.0002(12) 0.0110(10) -0.0091(13) C11 0.079(7) 0.098(8) 0.059(6) 0.018(6) 0.005(5) -0.008(6) C12 0.108(10) 0.174(15) 0.071(8) 0.022(9) 0.016(7) -0.064(10) C13 0.093(9) 0.200(17) 0.068(8) -0.027(9) 0.019(7) 0.038(10) P2 0.0647(16) 0.0696(17) 0.0667(17) -0.0068(14) 0.0188(13) 0.0038(13) C21 0.060(7) 0.149(13) 0.103(10) -0.006(9) 0.014(7) 0.013(7) C22 0.120(10) 0.071(8) 0.128(11) -0.004(8) 0.037(9) 0.030(8) C23 0.084(8) 0.095(8) 0.079(8) -0.022(7) 0.029(6) 0.008(7) C24 0.099(8) 0.106(9) 0.047(6) -0.008(6) 0.035(6) -0.021(7) P3 0.0677(16) 0.0676(17) 0.0639(16) 0.0061(13) 0.0091(13) 0.0053(13) C31 0.132(11) 0.067(7) 0.082(8) 0.012(6) 0.014(7) -0.013(7) C32 0.099(9) 0.098(9) 0.116(11) 0.003(8) 0.030(8) 0.032(8) C33 0.103(9) 0.087(8) 0.063(7) 0.012(6) -0.011(6) 0.012(7) C34 0.122(10) 0.090(8) 0.043(5) 0.009(6) 0.015(6) -0.005(7) N1 0.062(4) 0.079(6) 0.038(4) -0.002(4) 0.014(3) -0.015(4) C1 0.058(5) 0.055(5) 0.055(6) 0.001(5) 0.006(4) -0.010(4) O1 0.058(4) 0.068(4) 0.061(4) -0.004(3) 0.018(3) -0.024(3) O2 0.083(5) 0.078(5) 0.084(5) -0.014(4) 0.000(4) -0.030(4) C2 0.057(6) 0.084(7) 0.039(5) -0.015(5) 0.006(4) -0.019(5) O3 0.064(4) 0.061(4) 0.054(4) -0.003(3) 0.014(3) -0.015(3) O4 0.050(4) 0.112(6) 0.067(4) -0.012(4) 0.009(3) -0.014(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C2 2.085(9) . ? Mo1 C1 2.088(9) . ? Mo1 O1 2.111(6) . ? Mo1 O3 2.138(6) . ? Mo1 N1 2.270(7) . ? Mo1 P1 2.434(3) . ? Mo1 P3 2.443(3) . ? Mo1 P2 2.481(3) . ? P1 C11 1.803(10) . ? P1 C12 1.810(12) . ? P1 C13 1.802(13) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? P2 C22 1.794(12) . ? P2 C21 1.819(10) . ? P2 C23 1.805(11) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.522(15) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 N1 1.452(12) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? P3 C32 1.793(11) . ? P3 C31 1.819(11) . ? P3 C33 1.833(11) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 C34 1.505(15) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 N1 1.459(12) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? N1 H1 0.9100 . ? C1 O2 1.199(10) . ? C1 O1 1.284(11) . ? C2 O4 1.234(11) . ? C2 O3 1.245(11) . ? C3 C5 0.9100 4_656 ? C3 C6 1.5111 4_656 ? C3 C4 1.9519 5_766 ? C3 C4 2.0001 6_566 ? C4 C6 0.9150 7_656 ? C4 C5 1.1598 7_656 ? C4 C6 1.2295 8 ? C4 C4 1.6570 2_755 ? C4 C5 1.7160 8 ? C4 C3 1.9519 5_766 ? C4 C3 2.0001 6_565 ? C5 C3 0.9100 4_646 ? C5 C6 1.0416 . ? C5 C4 1.1598 7_656 ? C5 C4 1.7160 8_456 ? C5 C6 1.8801 2_656 ? C6 C4 0.9150 7_656 ? C6 C6 1.0796 2_656 ? C6 C4 1.2295 8_456 ? C6 C3 1.5111 4_646 ? C6 C5 1.8801 2_656 ? 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 C2 Mo1 C1 148.6(4) . . ? C2 Mo1 O1 157.1(4) . . ? C1 Mo1 O1 35.6(3) . . ? C2 Mo1 O3 34.3(3) . . ? C1 Mo1 O3 156.5(3) . . ? O1 Mo1 O3 158.9(3) . . ? C2 Mo1 N1 87.2(3) . . ? C1 Mo1 N1 116.2(3) . . ? O1 Mo1 N1 80.7(3) . . ? O3 Mo1 N1 84.0(3) . . ? C2 Mo1 P1 82.3(2) . . ? C1 Mo1 P1 76.2(3) . . ? O1 Mo1 P1 111.59(18) . . ? O3 Mo1 P1 83.18(17) . . ? N1 Mo1 P1 167.2(2) . . ? C2 Mo1 P3 78.6(3) . . ? C1 Mo1 P3 84.9(3) . . ? O1 Mo1 P3 80.17(19) . . ? O3 Mo1 P3 111.5(2) . . ? N1 Mo1 P3 80.1(2) . . ? P1 Mo1 P3 104.81(10) . . ? C2 Mo1 P2 113.0(3) . . ? C1 Mo1 P2 92.7(3) . . ? O1 Mo1 P2 84.05(19) . . ? O3 Mo1 P2 78.9(2) . . ? N1 Mo1 P2 79.5(2) . . ? P1 Mo1 P2 97.79(10) . . ? P3 Mo1 P2 155.96(10) . . ? C11 P1 C12 99.1(6) . . ? C11 P1 C13 102.5(6) . . ? C12 P1 C13 103.3(7) . . ? C11 P1 Mo1 117.7(4) . . ? C12 P1 Mo1 116.1(4) . . ? C13 P1 Mo1 115.7(5) . . ? P1 C11 H11A 109.5 . . ? P1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? P1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? P1 C12 H12A 109.5 . . ? P1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? P1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? P1 C13 H13A 109.5 . . ? P1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? P1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C22 P2 C21 103.8(7) . . ? C22 P2 C23 103.6(6) . . ? C21 P2 C23 105.6(6) . . ? C22 P2 Mo1 121.6(4) . . ? C21 P2 Mo1 120.1(5) . . ? C23 P2 Mo1 99.8(4) . . ? P2 C21 H21A 109.5 . . ? P2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? P2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? P2 C22 H22A 109.5 . . ? P2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? P2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 P2 111.2(7) . . ? C24 C23 H23A 109.4 . . ? P2 C23 H23A 109.4 . . ? C24 C23 H23B 109.4 . . ? P2 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? N1 C24 C23 109.3(8) . . ? N1 C24 H24A 109.8 . . ? C23 C24 H24A 109.8 . . ? N1 C24 H24B 109.8 . . ? C23 C24 H24B 109.8 . . ? H24A C24 H24B 108.3 . . ? C32 P3 C31 101.3(6) . . ? C32 P3 C33 103.6(6) . . ? C31 P3 C33 103.1(6) . . ? C32 P3 Mo1 127.2(5) . . ? C31 P3 Mo1 118.3(4) . . ? C33 P3 Mo1 99.8(4) . . ? P3 C31 H31A 109.5 . . ? P3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? P3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? P3 C32 H32A 109.5 . . ? P3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? P3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 P3 109.7(7) . . ? C34 C33 H33A 109.7 . . ? P3 C33 H33A 109.7 . . ? C34 C33 H33B 109.7 . . ? P3 C33 H33B 109.7 . . ? H33A C33 H33B 108.2 . . ? N1 C34 C33 110.8(9) . . ? N1 C34 H34A 109.5 . . ? C33 C34 H34A 109.5 . . ? N1 C34 H34B 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 108.1 . . ? C34 N1 C24 110.0(8) . . ? C34 N1 Mo1 115.0(6) . . ? C24 N1 Mo1 113.7(6) . . ? C34 N1 H1 105.8 . . ? C24 N1 H1 105.8 . . ? Mo1 N1 H1 105.8 . . ? O2 C1 O1 131.2(9) . . ? O2 C1 Mo1 155.6(8) . . ? O1 C1 Mo1 73.2(5) . . ? C1 O1 Mo1 71.2(5) . . ? O4 C2 O3 131.6(10) . . ? O4 C2 Mo1 153.2(9) . . ? O3 C2 Mo1 75.2(5) . . ? C2 O3 Mo1 70.5(5) . . ? C5 C3 C6 42.5 4_656 4_656 ? C5 C3 C4 61.5 4_656 5_766 ? C6 C3 C4 39.0 4_656 5_766 ? C5 C3 C4 16.9 4_656 6_566 ? C6 C3 C4 25.7 4_656 6_566 ? C4 C3 C4 49.6 5_766 6_566 ? C6 C4 C5 58.9 7_656 7_656 ? C6 C4 C6 58.3 7_656 8 ? C5 C4 C6 103.7 7_656 8 ? C6 C4 C4 46.9 7_656 2_755 ? C5 C4 C4 72.7 7_656 2_755 ? C6 C4 C4 32.9 8 2_755 ? C6 C4 C5 85.5 7_656 8 ? C5 C4 C5 102.7 7_656 8 ? C6 C4 C5 37.0 8 8 ? C4 C4 C5 40.2 2_755 8 ? C6 C4 C3 108.0 7_656 5_766 ? C5 C4 C3 128.1 7_656 5_766 ? C6 C4 C3 50.7 8 5_766 ? C4 C4 C3 66.7 2_755 5_766 ? C5 C4 C3 27.8 8 5_766 ? C6 C4 C3 45.7 7_656 6_565 ? C5 C4 C3 13.2 7_656 6_565 ? C6 C4 C3 92.8 8 6_565 ? C4 C4 C3 63.7 2_755 6_565 ? C5 C4 C3 98.4 8 6_565 ? C3 C4 C3 125.8 5_766 6_565 ? C3 C5 C6 101.3 4_646 . ? C3 C5 C4 150.0 4_646 7_656 ? C6 C5 C4 48.8 . 7_656 ? C3 C5 C4 90.7 4_646 8_456 ? C6 C5 C4 45.2 . 8_456 ? C4 C5 C4 67.2 7_656 8_456 ? C3 C5 C6 114.0 4_646 2_656 ? C6 C5 C6 28.1 . 2_656 ? C4 C5 C6 39.4 7_656 2_656 ? C4 C5 C6 29.0 8_456 2_656 ? C4 C6 C5 72.4 7_656 . ? C4 C6 C6 75.6 7_656 2_656 ? C5 C6 C6 124.8 . 2_656 ? C4 C6 C4 100.2 7_656 8_456 ? C5 C6 C4 97.8 . 8_456 ? C6 C6 C4 46.1 2_656 8_456 ? C4 C6 C3 108.6 7_656 4_646 ? C5 C6 C3 36.2 . 4_646 ? C6 C6 C3 134.9 2_656 4_646 ? C4 C6 C3 90.2 8_456 4_646 ? C4 C6 C5 65.5 7_656 2_656 ? C5 C6 C5 98.0 . 2_656 ? C6 C6 C5 27.1 2_656 2_656 ? C4 C6 C5 36.8 8_456 2_656 ? C3 C6 C5 112.0 4_646 2_656 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 28.01 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.989 _refine_diff_density_min -1.144 _refine_diff_density_rms 0.137 #=========================================================================== data_inter2 _database_code_depnum_ccdc_archive 'CCDC 231961' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H58 Mo3 O11 P6' _chemical_formula_weight 960.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.7692(10) _cell_length_b 16.3332(10) _cell_length_c 24.6818(10) _cell_angle_alpha 90.00 _cell_angle_beta 98.993(10) _cell_angle_gamma 90.00 _cell_volume 3889.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.640 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 1.244 _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11422 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_sigmaI/netI 0.0421 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 29.97 _reflns_number_total 11177 _reflns_number_gt 8010 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w==1/[\s^2^(Fo^2^)+(0.0636P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11177 _refine_ls_number_parameters 404 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0760 _refine_ls_R_factor_gt 0.0327 _refine_ls_wR_factor_ref 0.1038 _refine_ls_wR_factor_gt 0.0889 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.62391(3) 0.153297(15) 0.155387(10) 0.02159(6) Uani 1 1 d . . . Mo2 Mo 0.54974(3) 0.172339(16) 0.363809(11) 0.02424(7) Uani 1 1 d . . . Mo3 Mo 0.78412(3) 0.289760(15) 0.279598(11) 0.02577(7) Uani 1 1 d . . . P1 P 0.49947(9) 0.27920(5) 0.12665(4) 0.03199(18) Uani 1 1 d . . . P2 P 0.47536(10) 0.30088(6) 0.39753(4) 0.03433(19) Uani 1 1 d . . . P3 P 0.85987(9) 0.15526(6) 0.13469(4) 0.03335(18) Uani 1 1 d . . . P4 P 0.77711(9) 0.12258(6) 0.40353(4) 0.03399(19) Uani 1 1 d . . . P5 P 0.48946(9) 0.03128(5) 0.12288(4) 0.03217(18) Uani 1 1 d . . . P6 P 0.37934(10) 0.06290(6) 0.36368(4) 0.0398(2) Uani 1 1 d . . . O1 O 0.4546(2) 0.15966(14) 0.20637(9) 0.0286(5) Uani 1 1 d . . . O2 O 0.4144(2) 0.20717(13) 0.28740(9) 0.0293(5) Uani 1 1 d . . . O3 O 0.5691(2) 0.11086(13) 0.28589(9) 0.0283(4) Uani 1 1 d . . . O4 O 0.5929(3) 0.15666(19) 0.02949(11) 0.0535(8) Uani 1 1 d . . . O5 O 0.7624(3) 0.39554(15) 0.27134(11) 0.0453(6) Uani 1 1 d . . . O6 O 0.6914(2) 0.25723(14) 0.33202(9) 0.0322(5) Uani 1 1 d . . . O7 O 0.9588(3) 0.26897(18) 0.30096(11) 0.0437(6) Uani 1 1 d . . . O8 O 0.7259(2) 0.23694(13) 0.21700(9) 0.0297(5) Uani 1 1 d . . . O9 O 0.5318(3) 0.1488(2) 0.48710(11) 0.0555(8) Uani 1 1 d . . . O10 O 0.7237(2) 0.05865(15) 0.21650(10) 0.0293(5) Uani 1 1 d . . . O11 O 0.1822(4) 0.3072(3) 0.24021(19) 0.0775(12) Uani 1 1 d . . . C1 C 0.4784(3) 0.15979(18) 0.25825(13) 0.0253(6) Uani 1 1 d . . . C2 C 0.6052(4) 0.1548(2) 0.07813(14) 0.0341(7) Uani 1 1 d . . . C3 C 0.5397(4) 0.1575(2) 0.44018(15) 0.0375(8) Uani 1 1 d . . . C11 C 0.3229(4) 0.2630(3) 0.0920(2) 0.0588(12) Uani 1 1 d . . . H11A H 0.2710 0.2343 0.1160 0.088 Uiso 1 1 calc R . . H11B H 0.3246 0.2312 0.0594 0.088 Uiso 1 1 calc R . . H11C H 0.2800 0.3149 0.0823 0.088 Uiso 1 1 calc R . . C12 C 0.4750(5) 0.3511(2) 0.18026(18) 0.0500(10) Uani 1 1 d . . . H12A H 0.5622 0.3758 0.1947 0.075 Uiso 1 1 calc R . . H12B H 0.4391 0.3227 0.2091 0.075 Uiso 1 1 calc R . . H12C H 0.4107 0.3928 0.1654 0.075 Uiso 1 1 calc R . . C13 C 0.5703(5) 0.3464(2) 0.07944(19) 0.0541(11) Uani 1 1 d . . . H13A H 0.5870 0.3157 0.0480 0.081 Uiso 1 1 calc R . . H13B H 0.6558 0.3695 0.0974 0.081 Uiso 1 1 calc R . . H13C H 0.5055 0.3896 0.0680 0.081 Uiso 1 1 calc R . . C21 C 0.4575(4) 0.3820(2) 0.34648(17) 0.0461(9) Uani 1 1 d . . . H21A H 0.3911 0.3659 0.3154 0.069 Uiso 1 1 calc R . . H21B H 0.5454 0.3917 0.3349 0.069 Uiso 1 1 calc R . . H21C H 0.4265 0.4311 0.3621 0.069 Uiso 1 1 calc R . . C22 C 0.5861(6) 0.3482(3) 0.45484(18) 0.0575(12) Uani 1 1 d . . . H22A H 0.6781 0.3538 0.4463 0.086 Uiso 1 1 calc R . . H22B H 0.5885 0.3145 0.4869 0.086 Uiso 1 1 calc R . . H22C H 0.5502 0.4012 0.4618 0.086 Uiso 1 1 calc R . . C23 C 0.3063(5) 0.2995(3) 0.4193(2) 0.0623(13) Uani 1 1 d . . . H23A H 0.3094 0.2650 0.4509 0.093 Uiso 1 1 calc R . . H23B H 0.2388 0.2786 0.3901 0.093 Uiso 1 1 calc R . . H23C H 0.2813 0.3541 0.4283 0.093 Uiso 1 1 calc R . . C31 C 0.9929(4) 0.1257(3) 0.19141(18) 0.0491(10) Uani 1 1 d . . . H31A H 0.9818 0.0689 0.1999 0.074 Uiso 1 1 calc R . . H31B H 0.9842 0.1584 0.2230 0.074 Uiso 1 1 calc R . . H31C H 1.0828 0.1340 0.1812 0.074 Uiso 1 1 calc R . . C32 C 0.9179(5) 0.2554(3) 0.1167(3) 0.0726(16) Uani 1 1 d . . . H32A H 0.8988 0.2947 0.1434 0.109 Uiso 1 1 calc R . . H32B H 0.8700 0.2708 0.0812 0.109 Uiso 1 1 calc R . . H32C H 1.0158 0.2539 0.1159 0.109 Uiso 1 1 calc R . . C33 C 0.9038(5) 0.0902(3) 0.0808(2) 0.0642(14) Uani 1 1 d . . . H33A H 0.8554 0.1085 0.0461 0.096 Uiso 1 1 calc R . . H33B H 0.8775 0.0348 0.0872 0.096 Uiso 1 1 calc R . . H33C H 1.0019 0.0926 0.0806 0.096 Uiso 1 1 calc R . . C41 C 0.8603(4) 0.0676(3) 0.35360(16) 0.0501(10) Uani 1 1 d . . . H41A H 0.8606 0.1011 0.3217 0.075 Uiso 1 1 calc R . . H41B H 0.8103 0.0179 0.3434 0.075 Uiso 1 1 calc R . . H41C H 0.9539 0.0546 0.3694 0.075 Uiso 1 1 calc R . . C42 C 0.9051(4) 0.2001(3) 0.4284(2) 0.0564(11) Uani 1 1 d . . . H42A H 0.8714 0.2329 0.4558 0.085 Uiso 1 1 calc R . . H42B H 0.9213 0.2343 0.3985 0.085 Uiso 1 1 calc R . . H42C H 0.9901 0.1740 0.4441 0.085 Uiso 1 1 calc R . . C43 C 0.7974(5) 0.0504(3) 0.46049(17) 0.0542(11) Uani 1 1 d . . . H43A H 0.7411 0.0030 0.4504 0.081 Uiso 1 1 calc R . . H43B H 0.7690 0.0759 0.4920 0.081 Uiso 1 1 calc R . . H43C H 0.8928 0.0343 0.4691 0.081 Uiso 1 1 calc R . . C51 C 0.4172(4) -0.0250(2) 0.17531(18) 0.0480(10) Uani 1 1 d . . . H51A H 0.3507 0.0086 0.1896 0.072 Uiso 1 1 calc R . . H51B H 0.4902 -0.0397 0.2044 0.072 Uiso 1 1 calc R . . H51C H 0.3726 -0.0738 0.1595 0.072 Uiso 1 1 calc R . . C52 C 0.5848(5) -0.0471(3) 0.09250(19) 0.0555(11) Uani 1 1 d . . . H52A H 0.6565 -0.0686 0.1198 0.083 Uiso 1 1 calc R . . H52B H 0.6257 -0.0237 0.0631 0.083 Uiso 1 1 calc R . . H52C H 0.5228 -0.0904 0.0784 0.083 Uiso 1 1 calc R . . C53 C 0.3373(5) 0.0438(3) 0.0709(2) 0.0715(16) Uani 1 1 d . . . H53A H 0.3633 0.0702 0.0393 0.107 Uiso 1 1 calc R . . H53B H 0.2701 0.0769 0.0853 0.107 Uiso 1 1 calc R . . H53C H 0.2980 -0.0089 0.0607 0.107 Uiso 1 1 calc R . . C61 C 0.4530(7) -0.0372(3) 0.3548(3) 0.094(2) Uani 1 1 d . . . H61A H 0.5213 -0.0328 0.3309 0.141 Uiso 1 1 calc R . . H61B H 0.3810 -0.0740 0.3390 0.141 Uiso 1 1 calc R . . H61C H 0.4958 -0.0579 0.3897 0.141 Uiso 1 1 calc R . . C62 C 0.2357(5) 0.0655(4) 0.3069(2) 0.0742(16) Uani 1 1 d . . . H62A H 0.2712 0.0708 0.2729 0.111 Uiso 1 1 calc R . . H62B H 0.1768 0.1112 0.3113 0.111 Uiso 1 1 calc R . . H62C H 0.1833 0.0157 0.3065 0.111 Uiso 1 1 calc R . . C63 C 0.2869(7) 0.0461(4) 0.4204(2) 0.092(2) Uani 1 1 d . . . H63A H 0.2397 0.0954 0.4277 0.139 Uiso 1 1 calc R . . H63B H 0.3513 0.0310 0.4523 0.139 Uiso 1 1 calc R . . H63C H 0.2206 0.0030 0.4113 0.139 Uiso 1 1 calc R . . H101 H 0.719(4) 0.012(3) 0.2137(15) 0.027(10) Uiso 1 1 d . . . H102 H 0.696(7) 0.072(4) 0.253(3) 0.11(2) Uiso 1 1 d . . . H111 H 0.106(6) 0.297(3) 0.259(2) 0.067(16) Uiso 1 1 d . . . H112 H 0.261(5) 0.271(3) 0.247(2) 0.070(16) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.02429(12) 0.01740(11) 0.02289(12) 0.00039(9) 0.00311(9) -0.00046(9) Mo2 0.02723(13) 0.02101(12) 0.02542(13) 0.00147(9) 0.00701(9) 0.00159(9) Mo3 0.02740(13) 0.01963(12) 0.03051(14) -0.00286(9) 0.00528(10) -0.00585(9) P1 0.0337(4) 0.0242(4) 0.0366(5) 0.0060(3) 0.0008(3) 0.0038(3) P2 0.0400(5) 0.0278(4) 0.0370(5) -0.0039(3) 0.0118(4) 0.0042(4) P3 0.0299(4) 0.0332(4) 0.0386(5) 0.0026(4) 0.0105(3) 0.0015(3) P4 0.0358(4) 0.0350(5) 0.0301(4) 0.0033(3) 0.0018(3) 0.0072(4) P5 0.0341(4) 0.0245(4) 0.0357(5) -0.0026(3) -0.0016(3) -0.0047(3) P6 0.0416(5) 0.0355(5) 0.0428(5) 0.0096(4) 0.0086(4) -0.0095(4) O1 0.0276(11) 0.0309(12) 0.0273(11) -0.0001(9) 0.0044(8) 0.0004(9) O2 0.0294(11) 0.0273(11) 0.0323(12) 0.0008(9) 0.0079(9) 0.0058(9) O3 0.0314(11) 0.0248(11) 0.0285(11) 0.0008(8) 0.0041(9) 0.0043(9) O4 0.071(2) 0.066(2) 0.0238(13) 0.0026(12) 0.0069(12) 0.0016(16) O5 0.0676(18) 0.0219(11) 0.0454(15) -0.0044(10) 0.0055(13) -0.0106(12) O6 0.0333(12) 0.0301(12) 0.0343(12) 0.0010(9) 0.0091(9) -0.0028(9) O7 0.0286(12) 0.0567(17) 0.0450(15) -0.0053(13) 0.0030(10) -0.0061(12) O8 0.0325(11) 0.0231(10) 0.0329(12) -0.0056(9) 0.0033(9) -0.0034(9) O9 0.071(2) 0.067(2) 0.0315(14) 0.0051(13) 0.0183(13) 0.0015(16) O10 0.0366(12) 0.0200(11) 0.0312(12) 0.0032(9) 0.0045(9) 0.0027(9) O11 0.0442(19) 0.080(3) 0.110(3) 0.029(2) 0.017(2) 0.0124(19) C1 0.0245(14) 0.0206(13) 0.0314(15) 0.0001(11) 0.0065(11) -0.0028(11) C2 0.0366(17) 0.0314(17) 0.0340(17) 0.0003(13) 0.0044(13) 0.0013(13) C3 0.0388(18) 0.0370(18) 0.0378(19) 0.0010(15) 0.0094(14) 0.0035(15) C11 0.041(2) 0.049(2) 0.079(3) 0.004(2) -0.015(2) 0.0040(19) C12 0.060(3) 0.0324(19) 0.058(3) 0.0007(17) 0.009(2) 0.0189(18) C13 0.069(3) 0.036(2) 0.058(3) 0.0211(19) 0.012(2) 0.0023(19) C21 0.057(2) 0.0309(18) 0.051(2) 0.0014(16) 0.0097(18) 0.0087(17) C22 0.080(3) 0.043(2) 0.047(2) -0.0111(19) 0.004(2) -0.001(2) C23 0.061(3) 0.051(3) 0.084(4) 0.005(2) 0.039(3) 0.017(2) C31 0.0305(18) 0.059(3) 0.056(3) -0.004(2) 0.0010(16) 0.0050(17) C32 0.041(2) 0.060(3) 0.120(5) 0.029(3) 0.023(3) -0.007(2) C33 0.051(3) 0.086(4) 0.060(3) -0.015(3) 0.023(2) 0.018(2) C41 0.048(2) 0.061(3) 0.041(2) 0.0014(18) 0.0061(17) 0.025(2) C42 0.044(2) 0.058(3) 0.060(3) 0.004(2) -0.013(2) -0.004(2) C43 0.067(3) 0.051(2) 0.043(2) 0.0150(19) 0.003(2) 0.016(2) C51 0.042(2) 0.037(2) 0.065(3) 0.0031(18) 0.0105(18) -0.0149(16) C52 0.078(3) 0.034(2) 0.056(3) -0.0121(18) 0.018(2) -0.003(2) C53 0.061(3) 0.053(3) 0.084(4) 0.010(2) -0.038(3) -0.021(2) C61 0.094(5) 0.030(2) 0.157(7) 0.004(3) 0.016(4) -0.008(3) C62 0.066(3) 0.085(4) 0.065(3) 0.021(3) -0.010(2) -0.042(3) C63 0.102(5) 0.123(5) 0.060(3) 0.002(3) 0.036(3) -0.064(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C2 1.887(4) . ? Mo1 O8 2.167(2) . ? Mo1 O1 2.232(2) . ? Mo1 O10 2.271(2) . ? Mo1 P1 2.4373(9) . ? Mo1 P3 2.4380(9) . ? Mo1 P5 2.4518(9) . ? Mo2 C3 1.918(4) . ? Mo2 O6 2.189(2) . ? Mo2 O2 2.202(2) . ? Mo2 O3 2.204(2) . ? Mo2 P2 2.4120(9) . ? Mo2 P4 2.4238(9) . ? Mo2 P6 2.4423(10) . ? Mo2 C1 2.598(3) . ? Mo3 O7 1.739(3) . ? Mo3 O5 1.749(3) . ? Mo3 O6 1.773(2) . ? Mo3 O8 1.783(2) . ? P1 C12 1.813(4) . ? P1 C13 1.815(4) . ? P1 C11 1.821(4) . ? P2 C22 1.813(4) . ? P2 C23 1.814(4) . ? P2 C21 1.817(4) . ? P3 C33 1.805(4) . ? P3 C32 1.810(5) . ? P3 C31 1.820(4) . ? P4 C41 1.816(4) . ? P4 C42 1.818(4) . ? P4 C43 1.822(4) . ? P5 C52 1.813(4) . ? P5 C53 1.817(4) . ? P5 C51 1.818(4) . ? P6 C63 1.801(5) . ? P6 C61 1.814(5) . ? P6 C62 1.822(5) . ? O1 C1 1.265(4) . ? O2 C1 1.284(4) . ? O3 C1 1.304(4) . ? O4 C2 1.188(4) . ? O9 C3 1.181(4) . ? O10 H101 0.76(4) . ? O10 H102 1.00(7) . ? O11 H111 0.94(5) . ? O11 H112 0.96(5) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? 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 C2 Mo1 O8 131.46(12) . . ? C2 Mo1 O1 127.29(12) . . ? O8 Mo1 O1 82.81(8) . . ? C2 Mo1 O10 130.07(12) . . ? O8 Mo1 O10 81.98(9) . . ? O1 Mo1 O10 86.35(8) . . ? C2 Mo1 P1 74.33(11) . . ? O8 Mo1 P1 79.98(6) . . ? O1 Mo1 P1 75.22(6) . . ? O10 Mo1 P1 155.59(7) . . ? C2 Mo1 P3 74.54(11) . . ? O8 Mo1 P3 78.04(6) . . ? O1 Mo1 P3 157.81(6) . . ? O10 Mo1 P3 79.99(6) . . ? P1 Mo1 P3 111.89(3) . . ? C2 Mo1 P5 73.59(11) . . ? O8 Mo1 P5 154.94(7) . . ? O1 Mo1 P5 79.40(6) . . ? O10 Mo1 P5 79.43(7) . . ? P1 Mo1 P5 111.92(3) . . ? P3 Mo1 P5 114.70(3) . . ? C3 Mo2 O6 124.38(13) . . ? C3 Mo2 O2 139.31(12) . . ? O6 Mo2 O2 81.84(9) . . ? C3 Mo2 O3 145.53(12) . . ? O6 Mo2 O3 80.24(8) . . ? O2 Mo2 O3 59.49(8) . . ? C3 Mo2 P2 72.94(11) . . ? O6 Mo2 P2 79.27(6) . . ? O2 Mo2 P2 84.13(6) . . ? O3 Mo2 P2 140.30(6) . . ? C3 Mo2 P4 75.20(11) . . ? O6 Mo2 P4 76.50(7) . . ? O2 Mo2 P4 145.35(6) . . ? O3 Mo2 P4 90.10(6) . . ? P2 Mo2 P4 117.31(3) . . ? C3 Mo2 P6 76.65(12) . . ? O6 Mo2 P6 158.75(7) . . ? O2 Mo2 P6 82.53(6) . . ? O3 Mo2 P6 79.45(6) . . ? P2 Mo2 P6 113.30(4) . . ? P4 Mo2 P6 109.66(4) . . ? C3 Mo2 C1 158.22(13) . . ? O6 Mo2 C1 77.07(9) . . ? O2 Mo2 C1 29.58(8) . . ? O3 Mo2 C1 30.12(8) . . ? P2 Mo2 C1 111.51(7) . . ? P4 Mo2 C1 117.68(7) . . ? P6 Mo2 C1 82.24(7) . . ? O7 Mo3 O5 108.89(14) . . ? O7 Mo3 O6 108.02(12) . . ? O5 Mo3 O6 108.34(12) . . ? O7 Mo3 O8 109.47(12) . . ? O5 Mo3 O8 111.13(12) . . ? O6 Mo3 O8 110.92(10) . . ? C12 P1 C13 100.6(2) . . ? C12 P1 C11 102.3(2) . . ? C13 P1 C11 102.4(2) . . ? C12 P1 Mo1 116.79(14) . . ? C13 P1 Mo1 118.32(15) . . ? C11 P1 Mo1 114.00(15) . . ? C22 P2 C23 103.5(2) . . ? C22 P2 C21 102.2(2) . . ? C23 P2 C21 102.7(2) . . ? C22 P2 Mo2 117.69(16) . . ? C23 P2 Mo2 115.35(16) . . ? C21 P2 Mo2 113.36(13) . . ? C33 P3 C32 103.4(3) . . ? C33 P3 C31 100.8(2) . . ? C32 P3 C31 102.5(2) . . ? C33 P3 Mo1 119.21(17) . . ? C32 P3 Mo1 113.97(16) . . ? C31 P3 Mo1 114.84(14) . . ? C41 P4 C42 102.5(2) . . ? C41 P4 C43 101.4(2) . . ? C42 P4 C43 101.8(2) . . ? C41 P4 Mo2 111.73(13) . . ? C42 P4 Mo2 116.21(15) . . ? C43 P4 Mo2 120.76(16) . . ? C52 P5 C53 101.8(3) . . ? C52 P5 C51 102.7(2) . . ? C53 P5 C51 101.2(2) . . ? C52 P5 Mo1 115.18(16) . . ? C53 P5 Mo1 118.46(16) . . ? C51 P5 Mo1 115.23(14) . . ? C63 P6 C61 102.3(3) . . ? C63 P6 C62 100.5(3) . . ? C61 P6 C62 101.5(3) . . ? C63 P6 Mo2 122.3(2) . . ? C61 P6 Mo2 112.1(2) . . ? C62 P6 Mo2 115.28(16) . . ? C1 O1 Mo1 122.38(19) . . ? C1 O2 Mo2 92.55(18) . . ? C1 O3 Mo2 91.90(18) . . ? Mo3 O6 Mo2 151.05(13) . . ? Mo3 O8 Mo1 164.20(13) . . ? Mo1 O10 H101 127(3) . . ? Mo1 O10 H102 108(4) . . ? H101 O10 H102 106(4) . . ? H111 O11 H112 118(4) . . ? O1 C1 O2 122.7(3) . . ? O1 C1 O3 122.1(3) . . ? O2 C1 O3 115.3(3) . . ? O1 C1 Mo2 173.3(2) . . ? O2 C1 Mo2 57.87(16) . . ? O3 C1 Mo2 57.98(15) . . ? O4 C2 Mo1 179.2(3) . . ? O9 C3 Mo2 179.1(3) . . ? P1 C11 H11A 109.5 . . ? P1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? P1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? P1 C12 H12A 109.5 . . ? P1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? P1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? P1 C13 H13A 109.5 . . ? P1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? P1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? P2 C21 H21A 109.5 . . ? P2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? P2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? P2 C22 H22A 109.5 . . ? P2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? P2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? P2 C23 H23A 109.5 . . ? P2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? P2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? P3 C31 H31A 109.5 . . ? P3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? P3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? P3 C32 H32A 109.5 . . ? P3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? P3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? P3 C33 H33A 109.5 . . ? P3 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? P3 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? P4 C41 H41A 109.5 . . ? P4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? P4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? P4 C42 H42A 109.5 . . ? P4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? P4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? P4 C43 H43A 109.5 . . ? P4 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? P4 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? P5 C51 H51A 109.5 . . ? P5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? P5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? P5 C52 H52A 109.5 . . ? P5 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? P5 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? P5 C53 H53A 109.5 . . ? P5 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? P5 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? P6 C61 H61A 109.5 . . ? P6 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? P6 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? P6 C62 H62A 109.5 . . ? P6 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? P6 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? P6 C63 H63A 109.5 . . ? P6 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? P6 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 29.97 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.445 _refine_diff_density_min -1.035 _refine_diff_density_rms 0.152 #_eof #end of CIF