# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global #TrackingRef '- C1DT10099H_ccdc_807550_807553_cif.txt' _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author 'Oleksandr O. Kovalenko' _publ_contact_author_email kovalenko.chem@gmail.com _publ_contact_author_address ; Department of Inorganic Chemistry, National Taras Shevchenko University, Volodymyrska str. 64, Kyiv 01601, Ukraine ; loop_ _publ_author_name _publ_author_address 'Oleksandr O. Kovalenko' ; Department of Inorganic Chemistry, National Taras Shevchenko University, Volodymyrska str. 64, Kyiv 01601, Ukraine ; 'Oleksii A. Brusylovets' ; Department of Inorganic Chemistry, National Taras Shevchenko University, Volodymyrska str. 64, Kyiv 01601, Ukraine ; 'Vasyl Kinzhybalo' ; Faculty of Chemistry, University of Wroclaw, Joliot-Curie 14, 50-383 Wroclaw, Poland ; 'Tadeusz Lis' ; Faculty of Chemistry, University of Wroclaw, Joliot-Curie 14, 50-383 Wroclaw, Poland ; ; A.I.Brusilovets ; ; Department of Inorganic Chemistry, National Taras Shevchenko University, Volodymyrska str. 64, Kyiv 01601, Ukraine ; _publ_contact_author_name 'Oleksandr O. Kovalenko' #===================================================================== data_anat11pa #TrackingRef '- C1DT10099H_ccdc_807550_807553_cif.txt' _database_code_depnum_ccdc_archive 'CCDC 807550' #TrackingRef 'Kovalenko_ChemCommun.cif' #===================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H69 N2 O6 P Si3 W2' _chemical_formula_weight 1000.78 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' Si Si 0.0817 0.0704 '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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 11.679(3) _cell_length_b 16.861(4) _cell_length_c 21.651(6) _cell_angle_alpha 90.00 _cell_angle_beta 99.88(3) _cell_angle_gamma 90.00 _cell_volume 4200.3(19) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 31714 _cell_measurement_theta_min 3 _cell_measurement_theta_max 33 _exptl_crystal_description block _exptl_crystal_colour dark-red _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.583 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1992 _exptl_absorpt_coefficient_mu 5.631 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.272 _exptl_absorpt_correction_T_max 0.374 _exptl_absorpt_process_details ; CrysAlis RED (Oxford Diffraction, 2003), analytical numeric absorption using a multifaceted crystal model ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Kuma KM-4 CCD' _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 64307 _diffrn_reflns_av_R_equivalents 0.0245 _diffrn_reflns_av_sigmaI/netI 0.0211 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 32.50 _reflns_number_total 15009 _reflns_number_gt 12588 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisCCD (Oxford Diffraction, 2003)' _computing_cell_refinement 'CrysAlisRED (Oxford Diffraction, 2003)' _computing_data_reduction CrysAlisRED _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^)+(0.0264P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15009 _refine_ls_number_parameters 391 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0304 _refine_ls_R_factor_gt 0.0196 _refine_ls_wR_factor_ref 0.0448 _refine_ls_wR_factor_gt 0.0420 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.462558(6) 0.822781(4) 0.763790(3) 0.01356(2) Uani 1 1 d . . . W2 W 0.583226(6) 0.710992(4) 0.779977(3) 0.01432(2) Uani 1 1 d . . . P P 0.45464(4) 0.75831(3) 0.86999(2) 0.01481(8) Uani 1 1 d . . . N1 N 0.54430(14) 0.68274(9) 0.86364(7) 0.0163(3) Uani 1 1 d . . . Si1 Si 0.61963(5) 0.60988(3) 0.91301(2) 0.02027(10) Uani 1 1 d . . . C1 C 0.5743(2) 0.50859(12) 0.88371(11) 0.0318(5) Uani 1 1 d . . . H1A H 0.4929 0.4997 0.8876 0.048 Uiso 1 1 calc R . . H1B H 0.6234 0.4689 0.9086 0.048 Uiso 1 1 calc R . . H1C H 0.5828 0.5040 0.8396 0.048 Uiso 1 1 calc R . . C2 C 0.5916(2) 0.62296(13) 0.99453(10) 0.0295(4) Uani 1 1 d . . . H2A H 0.5079 0.6192 0.9947 0.044 Uiso 1 1 calc R . . H2B H 0.6198 0.6751 1.0103 0.044 Uiso 1 1 calc R . . H2C H 0.6322 0.5814 1.0215 0.044 Uiso 1 1 calc R . . C3 C 0.77706(18) 0.61946(14) 0.90873(10) 0.0287(4) Uani 1 1 d . . . H3A H 0.8042 0.6726 0.9226 0.043 Uiso 1 1 calc R . . H3B H 0.7885 0.6112 0.8654 0.043 Uiso 1 1 calc R . . H3C H 0.8213 0.5796 0.9359 0.043 Uiso 1 1 calc R . . N2 N 0.33049(14) 0.72432(9) 0.89201(7) 0.0181(3) Uani 1 1 d . . . O1 O 0.30944(11) 0.77894(8) 0.73582(6) 0.0192(3) Uani 1 1 d . . . C10 C 0.15968(19) 0.87520(13) 0.74562(11) 0.0293(4) Uani 1 1 d . . . H10A H 0.2170 0.9098 0.7708 0.044 Uiso 1 1 calc R . . H10B H 0.1260 0.8395 0.7734 0.044 Uiso 1 1 calc R . . H10C H 0.0980 0.9076 0.7215 0.044 Uiso 1 1 calc R . . C11 C 0.21861(16) 0.82670(12) 0.70095(9) 0.0217(4) Uani 1 1 d . . . H11 H 0.2539 0.8638 0.6734 0.026 Uiso 1 1 calc R . . C12 C 0.13554(19) 0.77182(16) 0.65988(10) 0.0320(5) Uani 1 1 d . . . H12A H 0.1781 0.7414 0.6326 0.048 Uiso 1 1 calc R . . H12B H 0.0746 0.8032 0.6341 0.048 Uiso 1 1 calc R . . H12C H 0.1001 0.7353 0.6863 0.048 Uiso 1 1 calc R . . O2 O 0.46158(11) 0.87584(8) 0.68415(6) 0.0202(3) Uani 1 1 d . . . C13 C 0.4165(2) 0.83841(14) 0.57568(10) 0.0288(4) Uani 1 1 d . . . H13A H 0.3705 0.7943 0.5879 0.043 Uiso 1 1 calc R . . H13B H 0.4515 0.8226 0.5395 0.043 Uiso 1 1 calc R . . H13C H 0.3659 0.8844 0.5645 0.043 Uiso 1 1 calc R . . C14 C 0.51177(17) 0.85990(13) 0.63014(9) 0.0234(4) Uani 1 1 d . . . H14 H 0.5664 0.8141 0.6392 0.028 Uiso 1 1 calc R . . C15 C 0.5791(2) 0.93194(16) 0.61494(12) 0.0395(6) Uani 1 1 d . . . H15A H 0.6388 0.9451 0.6511 0.059 Uiso 1 1 calc R . . H15B H 0.5259 0.9769 0.6052 0.059 Uiso 1 1 calc R . . H15C H 0.6163 0.9204 0.5787 0.059 Uiso 1 1 calc R . . O3 O 0.55696(12) 0.90714(8) 0.80763(6) 0.0195(3) Uani 1 1 d . . . C16 C 0.4609(3) 1.02638(15) 0.83415(12) 0.0413(6) Uani 1 1 d . . . H16A H 0.3868 0.9979 0.8284 0.062 Uiso 1 1 calc R . . H16B H 0.4469 1.0822 0.8226 0.062 Uiso 1 1 calc R . . H16C H 0.4986 1.0229 0.8781 0.062 Uiso 1 1 calc R . . C17 C 0.53862(19) 0.98977(11) 0.79308(10) 0.0245(4) Uani 1 1 d . . . H17 H 0.4996 0.9946 0.7484 0.029 Uiso 1 1 calc R . . C18 C 0.6549(3) 1.02971(16) 0.8002(2) 0.0689(11) Uani 1 1 d . . . H18A H 0.7027 1.0034 0.7732 0.103 Uiso 1 1 calc R . . H18B H 0.6938 1.0262 0.8440 0.103 Uiso 1 1 calc R . . H18C H 0.6443 1.0856 0.7881 0.103 Uiso 1 1 calc R . . O4 O 0.54198(12) 0.63773(8) 0.71445(6) 0.0197(3) Uani 1 1 d . . . C19 C 0.4060(2) 0.55508(14) 0.64706(11) 0.0341(5) Uani 1 1 d . . . H19A H 0.3554 0.5525 0.6787 0.051 Uiso 1 1 calc R . . H19B H 0.4613 0.5109 0.6532 0.051 Uiso 1 1 calc R . . H19C H 0.3587 0.5515 0.6051 0.051 Uiso 1 1 calc R . . C20 C 0.47181(17) 0.63275(12) 0.65333(9) 0.0219(4) Uani 1 1 d . . . H20 H 0.4151 0.6777 0.6477 0.026 Uiso 1 1 calc R . . C21 C 0.5498(2) 0.63889(16) 0.60435(10) 0.0357(5) Uani 1 1 d . . . H21A H 0.5942 0.6884 0.6104 0.054 Uiso 1 1 calc R . . H21B H 0.5021 0.6384 0.5624 0.054 Uiso 1 1 calc R . . H21C H 0.6035 0.5938 0.6086 0.054 Uiso 1 1 calc R . . O5 O 0.73336(11) 0.75027(8) 0.77869(6) 0.0209(3) Uani 1 1 d . . . C22 C 0.86823(19) 0.85758(15) 0.80612(11) 0.0331(5) Uani 1 1 d . . . H22A H 0.8289 0.8744 0.8404 0.050 Uiso 1 1 calc R . . H22B H 0.9036 0.9038 0.7894 0.050 Uiso 1 1 calc R . . H22C H 0.9288 0.8188 0.8219 0.050 Uiso 1 1 calc R . . C23 C 0.78095(17) 0.82020(12) 0.75473(10) 0.0230(4) Uani 1 1 d . . . H23 H 0.7168 0.8588 0.7407 0.028 Uiso 1 1 calc R . . C24 C 0.8348(2) 0.79553(14) 0.69871(11) 0.0316(5) Uani 1 1 d . . . H24A H 0.7751 0.7717 0.6668 0.047 Uiso 1 1 calc R . . H24B H 0.8966 0.7567 0.7120 0.047 Uiso 1 1 calc R . . H24C H 0.8676 0.8422 0.6812 0.047 Uiso 1 1 calc R . . Si2 Si 0.25118(5) 0.64119(3) 0.85774(3) 0.02075(10) Uani 1 1 d . . . C4 C 0.31211(18) 0.59842(12) 0.79135(10) 0.0253(4) Uani 1 1 d . . . H4A H 0.3122 0.6389 0.7589 0.038 Uiso 1 1 calc R . . H4B H 0.2644 0.5533 0.7738 0.038 Uiso 1 1 calc R . . H4C H 0.3919 0.5805 0.8063 0.038 Uiso 1 1 calc R . . C5 C 0.09634(18) 0.66388(13) 0.82333(11) 0.0274(4) Uani 1 1 d . . . H5A H 0.0489 0.6628 0.8565 0.041 Uiso 1 1 calc R . . H5B H 0.0674 0.6241 0.7914 0.041 Uiso 1 1 calc R . . H5C H 0.0917 0.7166 0.8041 0.041 Uiso 1 1 calc R . . C6 C 0.2523(2) 0.56346(14) 0.91925(12) 0.0350(5) Uani 1 1 d . . . H6A H 0.2099 0.5828 0.9516 0.052 Uiso 1 1 calc R . . H6B H 0.3327 0.5515 0.9383 0.052 Uiso 1 1 calc R . . H6C H 0.2147 0.5153 0.9002 0.052 Uiso 1 1 calc R . . Si3 Si 0.27649(5) 0.77888(3) 0.95130(3) 0.02249(11) Uani 1 1 d . . . C7 C 0.2718(2) 0.88734(13) 0.93363(10) 0.0303(5) Uani 1 1 d . . . H7A H 0.3499 0.9058 0.9300 0.045 Uiso 1 1 calc R . . H7B H 0.2442 0.9161 0.9675 0.045 Uiso 1 1 calc R . . H7C H 0.2189 0.8970 0.8941 0.045 Uiso 1 1 calc R . . C8 C 0.1210(2) 0.75360(17) 0.95429(11) 0.0364(5) Uani 1 1 d . . . H8A H 0.1139 0.6964 0.9606 0.055 Uiso 1 1 calc R . . H8B H 0.0720 0.7691 0.9148 0.055 Uiso 1 1 calc R . . H8C H 0.0959 0.7821 0.9891 0.055 Uiso 1 1 calc R . . C9 C 0.3531(2) 0.75529(15) 1.03225(9) 0.0324(5) Uani 1 1 d . . . H9A H 0.3400 0.6995 1.0417 0.049 Uiso 1 1 calc R . . H9B H 0.3228 0.7892 1.0625 0.049 Uiso 1 1 calc R . . H9C H 0.4366 0.7648 1.0350 0.049 Uiso 1 1 calc R . . O6 O 0.50606(12) 0.79961(8) 0.93685(6) 0.0196(3) Uani 1 1 d . . . C25 C 0.7128(2) 0.82971(16) 0.94661(12) 0.0374(6) Uani 1 1 d . . . H25A H 0.7151 0.8057 0.9056 0.056 Uiso 1 1 calc R . . H25B H 0.7318 0.7895 0.9795 0.056 Uiso 1 1 calc R . . H25C H 0.7696 0.8729 0.9540 0.056 Uiso 1 1 calc R . . C26 C 0.59301(19) 0.86199(12) 0.94773(9) 0.0249(4) Uani 1 1 d . . . H26 H 0.5743 0.9036 0.9147 0.030 Uiso 1 1 calc R . . C27 C 0.5848(2) 0.89749(15) 1.01124(11) 0.0364(5) Uani 1 1 d . . . H27A H 0.5050 0.9155 1.0114 0.055 Uiso 1 1 calc R . . H27B H 0.6380 0.9426 1.0194 0.055 Uiso 1 1 calc R . . H27C H 0.6059 0.8573 1.0439 0.055 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.01418(3) 0.01273(3) 0.01344(3) 0.00087(2) 0.00147(2) 0.00037(2) W2 0.01452(3) 0.01395(3) 0.01441(3) -0.00047(2) 0.00225(2) 0.00139(2) P 0.0180(2) 0.01272(19) 0.01357(19) 0.00025(15) 0.00229(16) 0.00170(16) N1 0.0192(7) 0.0133(6) 0.0161(7) 0.0016(5) 0.0018(6) 0.0024(5) Si1 0.0238(3) 0.0167(2) 0.0196(2) 0.00262(19) 0.0015(2) 0.0060(2) C1 0.0371(12) 0.0170(9) 0.0394(12) 0.0022(8) 0.0013(10) 0.0062(8) C2 0.0363(11) 0.0291(11) 0.0226(10) 0.0074(8) 0.0042(8) 0.0084(9) C3 0.0256(10) 0.0313(11) 0.0282(10) 0.0004(8) 0.0017(8) 0.0102(8) N2 0.0205(7) 0.0176(7) 0.0175(7) 0.0011(6) 0.0065(6) 0.0009(6) O1 0.0158(6) 0.0178(6) 0.0230(6) 0.0025(5) 0.0001(5) 0.0004(5) C10 0.0275(10) 0.0229(10) 0.0367(12) 0.0022(9) 0.0036(9) 0.0036(8) C11 0.0162(8) 0.0277(10) 0.0204(9) 0.0051(7) 0.0007(7) 0.0016(7) C12 0.0204(9) 0.0478(14) 0.0261(10) -0.0066(9) -0.0012(8) -0.0006(9) O2 0.0206(6) 0.0224(6) 0.0174(6) 0.0048(5) 0.0028(5) 0.0018(5) C13 0.0313(11) 0.0354(11) 0.0199(9) 0.0007(8) 0.0043(8) 0.0067(9) C14 0.0213(9) 0.0302(10) 0.0196(9) 0.0068(8) 0.0061(7) 0.0022(8) C15 0.0310(12) 0.0488(15) 0.0398(13) 0.0165(11) 0.0094(10) -0.0088(11) O3 0.0236(6) 0.0138(6) 0.0205(6) 0.0004(5) 0.0015(5) -0.0025(5) C16 0.0619(17) 0.0264(11) 0.0378(13) 0.0026(10) 0.0148(12) 0.0166(11) C17 0.0326(10) 0.0136(8) 0.0265(10) 0.0013(7) 0.0028(8) -0.0018(7) C18 0.0432(16) 0.0218(12) 0.142(3) 0.0072(17) 0.0161(19) -0.0094(12) O4 0.0244(7) 0.0178(6) 0.0167(6) -0.0032(5) 0.0033(5) 0.0010(5) C19 0.0434(13) 0.0319(11) 0.0269(11) -0.0074(9) 0.0057(9) -0.0156(10) C20 0.0261(9) 0.0205(9) 0.0174(8) -0.0018(7) -0.0011(7) -0.0011(7) C21 0.0459(14) 0.0402(13) 0.0230(10) -0.0060(9) 0.0117(10) -0.0136(11) O5 0.0152(6) 0.0228(7) 0.0248(7) 0.0027(5) 0.0036(5) 0.0019(5) C22 0.0254(10) 0.0381(13) 0.0344(12) -0.0063(10) 0.0015(9) -0.0090(9) C23 0.0171(8) 0.0240(9) 0.0277(10) 0.0019(8) 0.0037(7) -0.0021(7) C24 0.0293(11) 0.0375(12) 0.0305(11) 0.0005(9) 0.0122(9) -0.0067(9) Si2 0.0213(2) 0.0155(2) 0.0265(3) 0.0022(2) 0.0069(2) -0.00020(19) C4 0.0239(9) 0.0182(9) 0.0343(11) -0.0059(8) 0.0067(8) -0.0027(7) C5 0.0228(9) 0.0267(10) 0.0329(11) -0.0025(8) 0.0053(8) -0.0022(8) C6 0.0336(12) 0.0258(11) 0.0474(14) 0.0138(10) 0.0124(10) -0.0003(9) Si3 0.0263(3) 0.0255(3) 0.0171(2) 0.0005(2) 0.0078(2) 0.0058(2) C7 0.0377(12) 0.0248(10) 0.0280(10) -0.0028(8) 0.0048(9) 0.0118(9) C8 0.0317(11) 0.0504(15) 0.0308(11) -0.0040(11) 0.0164(9) 0.0036(11) C9 0.0400(12) 0.0408(13) 0.0176(9) 0.0030(9) 0.0085(9) 0.0074(10) O6 0.0251(7) 0.0174(6) 0.0157(6) -0.0020(5) 0.0015(5) 0.0005(5) C25 0.0316(12) 0.0431(14) 0.0378(13) -0.0176(11) 0.0067(10) -0.0106(10) C26 0.0332(10) 0.0193(9) 0.0190(9) -0.0014(7) -0.0045(8) -0.0057(8) C27 0.0433(13) 0.0319(12) 0.0299(11) -0.0135(9) -0.0049(10) 0.0057(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 O1 1.9337(14) . ? W1 O2 1.9409(13) . ? W1 O3 1.9444(14) . ? W1 W2 2.3435(4) . ? W1 P 2.5594(7) . ? W2 O5 1.8791(14) . ? W2 O4 1.8805(13) . ? W2 N1 1.9993(16) . ? W2 P 2.7739(9) . ? P O6 1.6257(14) . ? P N1 1.6699(16) . ? P N2 1.7015(17) . ? N1 Si1 1.7615(16) . ? Si1 C2 1.863(2) . ? Si1 C3 1.864(2) . ? Si1 C1 1.867(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? N2 Si2 1.7712(17) . ? N2 Si3 1.7804(17) . ? O1 C11 1.438(2) . ? C10 C11 1.519(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.514(3) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? O2 C14 1.421(2) . ? C13 C14 1.520(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.514(3) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? O3 C17 1.436(2) . ? C16 C17 1.507(3) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.500(3) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? O4 C20 1.435(2) . ? C19 C20 1.513(3) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.515(3) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? O5 C23 1.438(2) . ? C22 C23 1.512(3) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.517(3) . ? C23 H23 1.0000 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? Si2 C4 1.856(2) . ? Si2 C6 1.867(2) . ? Si2 C5 1.873(2) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? Si3 C7 1.867(2) . ? Si3 C9 1.869(2) . ? Si3 C8 1.877(2) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? O6 C26 1.453(2) . ? C25 C26 1.506(3) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.518(3) . ? C26 H26 1.0000 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 W1 O2 91.94(6) . . ? O1 W1 O3 148.10(6) . . ? O2 W1 O3 90.74(6) . . ? O1 W1 W2 103.85(4) . . ? O2 W1 W2 114.54(4) . . ? O3 W1 W2 103.84(5) . . ? O1 W1 P 86.84(5) . . ? O2 W1 P 176.70(4) . . ? O3 W1 P 88.68(4) . . ? W2 W1 P 68.75(2) . . ? O5 W2 O4 109.83(6) . . ? O5 W2 N1 117.08(7) . . ? O4 W2 N1 117.28(6) . . ? O5 W2 W1 104.66(5) . . ? O4 W2 W1 110.24(5) . . ? N1 W2 W1 95.90(5) . . ? O5 W2 P 121.88(5) . . ? O4 W2 P 128.28(4) . . ? N1 W2 P 36.61(5) . . ? W1 W2 P 59.308(16) . . ? O6 P N1 105.02(8) . . ? O6 P N2 95.57(8) . . ? N1 P N2 110.04(8) . . ? O6 P W1 123.59(6) . . ? N1 P W1 97.48(6) . . ? N2 P W1 123.96(6) . . ? O6 P W2 125.95(6) . . ? N1 P W2 45.57(5) . . ? N2 P W2 133.64(6) . . ? W1 P W2 51.943(18) . . ? P N1 Si1 137.48(10) . . ? P N1 W2 97.82(7) . . ? Si1 N1 W2 123.26(8) . . ? N1 Si1 C2 109.98(9) . . ? N1 Si1 C3 107.68(9) . . ? C2 Si1 C3 111.86(11) . . ? N1 Si1 C1 110.42(9) . . ? C2 Si1 C1 110.16(11) . . ? C3 Si1 C1 106.67(11) . . ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? P N2 Si2 123.96(9) . . ? P N2 Si3 116.89(9) . . ? Si2 N2 Si3 119.11(9) . . ? C11 O1 W1 120.63(12) . . ? C11 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C11 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O1 C11 C12 107.86(17) . . ? O1 C11 C10 109.94(16) . . ? C12 C11 C10 112.85(17) . . ? O1 C11 H11 108.7 . . ? C12 C11 H11 108.7 . . ? C10 C11 H11 108.7 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 O2 W1 134.72(12) . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O2 C14 C15 109.30(19) . . ? O2 C14 C13 109.45(16) . . ? C15 C14 C13 111.18(18) . . ? O2 C14 H14 109.0 . . ? C15 C14 H14 109.0 . . ? C13 C14 H14 109.0 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 O3 W1 123.49(12) . . ? C17 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C17 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O3 C17 C18 108.34(19) . . ? O3 C17 C16 110.49(17) . . ? C18 C17 C16 112.4(2) . . ? O3 C17 H17 108.5 . . ? C18 C17 H17 108.5 . . ? C16 C17 H17 108.5 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 O4 W2 140.02(12) . . ? C20 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C20 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O4 C20 C19 109.54(17) . . ? O4 C20 C21 108.94(17) . . ? C19 C20 C21 110.70(18) . . ? O4 C20 H20 109.2 . . ? C19 C20 H20 109.2 . . ? C21 C20 H20 109.2 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 O5 W2 135.55(12) . . ? C23 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C23 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O5 C23 C22 109.27(17) . . ? O5 C23 C24 107.61(17) . . ? C22 C23 C24 112.51(18) . . ? O5 C23 H23 109.1 . . ? C22 C23 H23 109.1 . . ? C24 C23 H23 109.1 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N2 Si2 C4 112.93(9) . . ? N2 Si2 C6 108.52(10) . . ? C4 Si2 C6 108.85(11) . . ? N2 Si2 C5 113.87(9) . . ? C4 Si2 C5 104.10(10) . . ? C6 Si2 C5 108.36(11) . . ? Si2 C4 H4A 109.5 . . ? Si2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 Si3 C7 111.09(9) . . ? N2 Si3 C9 113.24(9) . . ? C7 Si3 C9 113.15(11) . . ? N2 Si3 C8 111.84(10) . . ? C7 Si3 C8 103.59(12) . . ? C9 Si3 C8 103.27(11) . . ? Si3 C7 H7A 109.5 . . ? Si3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si3 C8 H8A 109.5 . . ? Si3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si3 C9 H9A 109.5 . . ? Si3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C26 O6 P 126.56(12) . . ? C26 C25 H25A 109.5 . . ? C26 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C26 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O6 C26 C25 111.19(17) . . ? O6 C26 C27 106.33(18) . . ? C25 C26 C27 111.15(18) . . ? O6 C26 H26 109.4 . . ? C25 C26 H26 109.4 . . ? C27 C26 H26 109.4 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 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 O1 W1 W2 O5 160.36(6) . . . . ? O2 W1 W2 O5 61.68(7) . . . . ? O3 W1 W2 O5 -35.62(6) . . . . ? P W1 W2 O5 -118.66(5) . . . . ? O1 W1 W2 O4 42.32(6) . . . . ? O2 W1 W2 O4 -56.36(6) . . . . ? O3 W1 W2 O4 -153.66(6) . . . . ? P W1 W2 O4 123.30(5) . . . . ? O1 W1 W2 N1 -79.63(6) . . . . ? O2 W1 W2 N1 -178.31(6) . . . . ? O3 W1 W2 N1 84.38(6) . . . . ? P W1 W2 N1 1.35(5) . . . . ? O1 W1 W2 P -80.98(5) . . . . ? O2 W1 W2 P -179.66(5) . . . . ? O3 W1 W2 P 83.04(5) . . . . ? O1 W1 P O6 -141.79(8) . . . . ? O3 W1 P O6 6.61(7) . . . . ? W2 W1 P O6 112.02(7) . . . . ? O1 W1 P N1 104.57(7) . . . . ? O3 W1 P N1 -107.03(7) . . . . ? W2 W1 P N1 -1.62(6) . . . . ? O1 W1 P N2 -15.77(8) . . . . ? O3 W1 P N2 132.63(8) . . . . ? W2 W1 P N2 -121.96(7) . . . . ? O1 W1 P W2 106.19(4) . . . . ? O3 W1 P W2 -105.41(4) . . . . ? O5 W2 P O6 -18.77(8) . . . . ? O4 W2 P O6 160.01(8) . . . . ? N1 W2 P O6 74.77(10) . . . . ? W1 W2 P O6 -107.47(7) . . . . ? O5 W2 P N1 -93.55(9) . . . . ? O4 W2 P N1 85.23(10) . . . . ? W1 W2 P N1 177.75(8) . . . . ? O5 W2 P N2 -167.77(9) . . . . ? O4 W2 P N2 11.01(10) . . . . ? N1 W2 P N2 -74.23(11) . . . . ? W1 W2 P N2 103.53(8) . . . . ? O5 W2 P W1 88.70(6) . . . . ? O4 W2 P W1 -92.52(6) . . . . ? N1 W2 P W1 -177.75(8) . . . . ? O6 P N1 Si1 39.67(16) . . . . ? N2 P N1 Si1 -62.15(16) . . . . ? W1 P N1 Si1 167.48(13) . . . . ? W2 P N1 Si1 165.69(19) . . . . ? O6 P N1 W2 -126.02(7) . . . . ? N2 P N1 W2 132.15(8) . . . . ? W1 P N1 W2 1.79(6) . . . . ? O5 W2 N1 P 107.84(8) . . . . ? O4 W2 N1 P -118.34(7) . . . . ? W1 W2 N1 P -1.94(7) . . . . ? O5 W2 N1 Si1 -60.64(11) . . . . ? O4 W2 N1 Si1 73.18(11) . . . . ? W1 W2 N1 Si1 -170.43(9) . . . . ? P W2 N1 Si1 -168.48(15) . . . . ? P N1 Si1 C2 -1.03(18) . . . . ? W2 N1 Si1 C2 161.95(11) . . . . ? P N1 Si1 C3 -123.15(15) . . . . ? W2 N1 Si1 C3 39.83(13) . . . . ? P N1 Si1 C1 120.75(15) . . . . ? W2 N1 Si1 C1 -76.27(13) . . . . ? O6 P N2 Si2 -154.40(11) . . . . ? N1 P N2 Si2 -46.18(13) . . . . ? W1 P N2 Si2 68.20(12) . . . . ? W2 P N2 Si2 0.83(15) . . . . ? O6 P N2 Si3 27.84(10) . . . . ? N1 P N2 Si3 136.07(10) . . . . ? W1 P N2 Si3 -109.55(9) . . . . ? W2 P N2 Si3 -176.93(4) . . . . ? O2 W1 O1 C11 -42.60(14) . . . . ? O3 W1 O1 C11 51.92(18) . . . . ? W2 W1 O1 C11 -158.47(12) . . . . ? P W1 O1 C11 134.33(13) . . . . ? W1 O1 C11 C12 152.47(13) . . . . ? W1 O1 C11 C10 -84.09(17) . . . . ? O1 W1 O2 C14 -101.05(17) . . . . ? O3 W1 O2 C14 110.74(17) . . . . ? W2 W1 O2 C14 5.14(18) . . . . ? W1 O2 C14 C15 -127.32(17) . . . . ? W1 O2 C14 C13 110.71(18) . . . . ? O1 W1 O3 C17 -53.62(19) . . . . ? O2 W1 O3 C17 41.25(15) . . . . ? W2 W1 O3 C17 156.78(13) . . . . ? P W1 O3 C17 -135.50(14) . . . . ? W1 O3 C17 C18 -143.1(2) . . . . ? W1 O3 C17 C16 93.4(2) . . . . ? O5 W2 O4 C20 -102.80(19) . . . . ? N1 W2 O4 C20 120.27(19) . . . . ? W1 W2 O4 C20 12.0(2) . . . . ? P W2 O4 C20 78.3(2) . . . . ? W2 O4 C20 C19 -136.69(17) . . . . ? W2 O4 C20 C21 102.1(2) . . . . ? O4 W2 O5 C23 97.78(18) . . . . ? N1 W2 O5 C23 -125.19(17) . . . . ? W1 W2 O5 C23 -20.53(18) . . . . ? P W2 O5 C23 -83.23(18) . . . . ? W2 O5 C23 C22 128.73(17) . . . . ? W2 O5 C23 C24 -108.83(19) . . . . ? P N2 Si2 C4 -3.78(15) . . . . ? Si3 N2 Si2 C4 173.93(10) . . . . ? P N2 Si2 C6 117.00(13) . . . . ? Si3 N2 Si2 C6 -65.30(13) . . . . ? P N2 Si2 C5 -122.24(12) . . . . ? Si3 N2 Si2 C5 55.47(13) . . . . ? P N2 Si3 C7 48.29(13) . . . . ? Si2 N2 Si3 C7 -129.58(11) . . . . ? P N2 Si3 C9 -80.33(13) . . . . ? Si2 N2 Si3 C9 101.81(13) . . . . ? P N2 Si3 C8 163.50(11) . . . . ? Si2 N2 Si3 C8 -14.37(14) . . . . ? N1 P O6 C26 88.57(16) . . . . ? N2 P O6 C26 -158.93(16) . . . . ? W1 P O6 C26 -21.31(17) . . . . ? W2 P O6 C26 43.06(17) . . . . ? P O6 C26 C25 -75.9(2) . . . . ? P O6 C26 C27 162.96(14) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C4 H4A O1 0.98 2.41 3.271(3) 145.9 . C9 H9C O6 0.98 2.47 3.047(3) 117.2 . C11 H11 O2 1.00 2.41 3.037(2) 120.5 . C17 H17 O2 1.00 2.43 3.055(3) 119.6 . C26 H26 O3 1.00 2.29 3.085(3) 135.4 . _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.87 _refine_diff_density_min -0.78 _refine_diff_density_rms 0.124 #===================================================================== data_anat3abs #TrackingRef '- C1DT10099H_ccdc_807550_807553_cif.txt' _database_code_depnum_ccdc_archive 'CCDC 807551' #TrackingRef 'Kovalenko_ChemCommun.cif' #===================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H69 Mo2 N2 O6 P Si3' _chemical_formula_sum 'C27 H69 Mo2 N2 O6 P Si3' _chemical_formula_weight 824.96 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' Si Si 0.0817 0.0704 '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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 11.643(3) _cell_length_b 16.741(4) _cell_length_c 21.756(6) _cell_angle_alpha 90.00 _cell_angle_beta 99.96(3) _cell_angle_gamma 90.00 _cell_volume 4176.7(19) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 17496 _cell_measurement_theta_min 4.28 _cell_measurement_theta_max 26.50 _exptl_crystal_description plate _exptl_crystal_colour 'red brown' _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.312 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1736 _exptl_absorpt_coefficient_mu 0.759 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.868 _exptl_absorpt_correction_T_max 0.969 _exptl_absorpt_process_details ; CrysAlis RED (Oxford Diffraction, 1995-2003) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; 'Oxford Xcalibur PX \k-geometry diffractometer with CCD area detector' ; _diffrn_measurement_method '\w and \f' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51763 _diffrn_reflns_av_R_equivalents 0.1081 _diffrn_reflns_av_sigmaI/netI 0.1163 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 4.28 _diffrn_reflns_theta_max 26.50 _reflns_number_total 8632 _reflns_number_gt 6314 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 1995-2003)' _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 1995-2003)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 1995-2003)' _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^)+(0.038P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8632 _refine_ls_number_parameters 391 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1298 _refine_ls_R_factor_gt 0.0807 _refine_ls_wR_factor_ref 0.1238 _refine_ls_wR_factor_gt 0.1104 _refine_ls_goodness_of_fit_ref 1.156 _refine_ls_restrained_S_all 1.156 _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 0.53588(4) 0.32192(3) 0.23712(2) 0.01475(14) Uani 1 1 d . . . Mo2 Mo 0.41922(4) 0.21316(3) 0.21999(2) 0.01526(14) Uani 1 1 d . . . P P 0.54947(13) 0.25924(8) 0.12841(7) 0.0153(3) Uani 1 1 d . . . N1 N 0.4597(4) 0.1845(3) 0.1365(2) 0.0148(10) Uani 1 1 d . . . Si1 Si 0.38176(15) 0.11105(9) 0.08815(8) 0.0210(4) Uani 1 1 d . . . C1 C 0.4266(6) 0.0088(3) 0.1168(3) 0.0328(17) Uani 1 1 d . . . H1A H 0.5084 -0.0001 0.1132 0.049 Uiso 1 1 calc R . . H1B H 0.3775 -0.0309 0.0916 0.049 Uiso 1 1 calc R . . H1C H 0.4176 0.0037 0.1605 0.049 Uiso 1 1 calc R . . C2 C 0.4071(6) 0.1227(4) 0.0071(3) 0.0274(15) Uani 1 1 d . . . H2A H 0.4910 0.1208 0.0065 0.041 Uiso 1 1 calc R . . H2B H 0.3757 0.1742 -0.0095 0.041 Uiso 1 1 calc R . . H2C H 0.3680 0.0794 -0.0187 0.041 Uiso 1 1 calc R . . C3 C 0.2247(5) 0.1214(4) 0.0931(3) 0.0280(16) Uani 1 1 d . . . H3A H 0.2135 0.1116 0.1360 0.042 Uiso 1 1 calc R . . H3B H 0.1793 0.0825 0.0652 0.042 Uiso 1 1 calc R . . H3C H 0.1984 0.1755 0.0805 0.042 Uiso 1 1 calc R . . N2 N 0.6734(4) 0.2246(3) 0.1065(2) 0.0174(11) Uani 1 1 d . . . Si2 Si 0.75242(15) 0.14025(9) 0.14007(8) 0.0215(4) Uani 1 1 d . . . C4 C 0.6909(5) 0.0962(3) 0.2056(3) 0.0240(15) Uani 1 1 d . . . H4A H 0.6905 0.1366 0.2382 0.036 Uiso 1 1 calc R . . H4B H 0.7388 0.0507 0.2229 0.036 Uiso 1 1 calc R . . H4C H 0.6110 0.0782 0.1904 0.036 Uiso 1 1 calc R . . C5 C 0.9075(5) 0.1629(3) 0.1748(3) 0.0266(15) Uani 1 1 d . . . H5A H 0.9115 0.2148 0.1960 0.040 Uiso 1 1 calc R . . H5B H 0.9547 0.1647 0.1417 0.040 Uiso 1 1 calc R . . H5C H 0.9375 0.1212 0.2050 0.040 Uiso 1 1 calc R . . C6 C 0.7500(6) 0.0632(4) 0.0774(3) 0.0331(17) Uani 1 1 d . . . H6A H 0.7912 0.0838 0.0451 0.050 Uiso 1 1 calc R . . H6B H 0.6690 0.0512 0.0589 0.050 Uiso 1 1 calc R . . H6C H 0.7885 0.0145 0.0955 0.050 Uiso 1 1 calc R . . Si3 Si 0.72721(15) 0.27923(10) 0.04713(8) 0.0215(4) Uani 1 1 d . . . C7 C 0.7317(6) 0.3883(3) 0.0642(3) 0.0256(15) Uani 1 1 d . . . H7A H 0.6562 0.4054 0.0738 0.038 Uiso 1 1 calc R . . H7B H 0.7480 0.4177 0.0277 0.038 Uiso 1 1 calc R . . H7C H 0.7931 0.3993 0.1000 0.038 Uiso 1 1 calc R . . C8 C 0.8828(5) 0.2550(4) 0.0444(3) 0.0328(16) Uani 1 1 d . . . H8A H 0.9321 0.2730 0.0831 0.049 Uiso 1 1 calc R . . H8B H 0.9067 0.2822 0.0087 0.049 Uiso 1 1 calc R . . H8C H 0.8914 0.1972 0.0400 0.049 Uiso 1 1 calc R . . C9 C 0.6497(6) 0.2548(4) -0.0331(3) 0.0324(16) Uani 1 1 d . . . H9A H 0.5657 0.2627 -0.0353 0.049 Uiso 1 1 calc R . . H9B H 0.6649 0.1990 -0.0427 0.049 Uiso 1 1 calc R . . H9C H 0.6779 0.2898 -0.0634 0.049 Uiso 1 1 calc R . . O1 O 0.6892(3) 0.2758(2) 0.26422(17) 0.0198(9) Uani 1 1 d . . . C10 C 0.8364(6) 0.3733(4) 0.2525(3) 0.0301(16) Uani 1 1 d . . . H10A H 0.7788 0.4096 0.2291 0.045 Uiso 1 1 calc R . . H10B H 0.8665 0.3374 0.2234 0.045 Uiso 1 1 calc R . . H10C H 0.9008 0.4044 0.2758 0.045 Uiso 1 1 calc R . . C11 C 0.7798(5) 0.3249(4) 0.2972(3) 0.0249(14) Uani 1 1 d . . . H11 H 0.7436 0.3629 0.3238 0.030 Uiso 1 1 calc R . . C12 C 0.8622(6) 0.2720(4) 0.3399(3) 0.0347(17) Uani 1 1 d . . . H12A H 0.8189 0.2426 0.3675 0.052 Uiso 1 1 calc R . . H12B H 0.9224 0.3048 0.3651 0.052 Uiso 1 1 calc R . . H12C H 0.8991 0.2341 0.3150 0.052 Uiso 1 1 calc R . . O2 O 0.5327(3) 0.3724(2) 0.31683(17) 0.0213(10) Uani 1 1 d . . . C13 C 0.5822(5) 0.3374(4) 0.4249(3) 0.0271(15) Uani 1 1 d . . . H13A H 0.6271 0.2918 0.4137 0.041 Uiso 1 1 calc R . . H13B H 0.5487 0.3242 0.4620 0.041 Uiso 1 1 calc R . . H13C H 0.6336 0.3839 0.4338 0.041 Uiso 1 1 calc R . . C14 C 0.4851(5) 0.3567(4) 0.3711(3) 0.0230(14) Uani 1 1 d . . . H14 H 0.4316 0.3096 0.3632 0.028 Uiso 1 1 calc R . . C15 C 0.4160(6) 0.4286(4) 0.3860(3) 0.0381(18) Uani 1 1 d . . . H15A H 0.3588 0.4431 0.3491 0.057 Uiso 1 1 calc R . . H15B H 0.4691 0.4736 0.3978 0.057 Uiso 1 1 calc R . . H15C H 0.3755 0.4158 0.4206 0.057 Uiso 1 1 calc R . . O3 O 0.4404(3) 0.4057(2) 0.19188(17) 0.0191(9) Uani 1 1 d . . . C16 C 0.5427(7) 0.5244(4) 0.1672(3) 0.043(2) Uani 1 1 d . . . H16A H 0.6166 0.4950 0.1740 0.064 Uiso 1 1 calc R . . H16B H 0.5574 0.5806 0.1786 0.064 Uiso 1 1 calc R . . H16C H 0.5065 0.5207 0.1232 0.064 Uiso 1 1 calc R . . C17 C 0.4624(5) 0.4890(3) 0.2070(3) 0.0226(14) Uani 1 1 d . . . H17 H 0.5005 0.4930 0.2518 0.027 Uiso 1 1 calc R . . C18 C 0.3475(7) 0.5308(4) 0.1989(5) 0.077(3) Uani 1 1 d . . . H18A H 0.2993 0.5070 0.2268 0.116 Uiso 1 1 calc R . . H18B H 0.3078 0.5254 0.1556 0.116 Uiso 1 1 calc R . . H18C H 0.3599 0.5876 0.2091 0.116 Uiso 1 1 calc R . . O4 O 0.4629(3) 0.1393(2) 0.28549(17) 0.0181(9) Uani 1 1 d . . . C19 C 0.6040(6) 0.0596(4) 0.3521(3) 0.0331(17) Uani 1 1 d . . . H19A H 0.6564 0.0615 0.3214 0.050 Uiso 1 1 calc R . . H19B H 0.5528 0.0129 0.3439 0.050 Uiso 1 1 calc R . . H19C H 0.6501 0.0557 0.3941 0.050 Uiso 1 1 calc R . . C20 C 0.5311(5) 0.1345(3) 0.3471(3) 0.0210(14) Uani 1 1 d . . . H20 H 0.5835 0.1821 0.3547 0.025 Uiso 1 1 calc R . . C21 C 0.4501(6) 0.1339(4) 0.3937(3) 0.043(2) Uani 1 1 d . . . H21A H 0.4021 0.1823 0.3887 0.064 Uiso 1 1 calc R . . H21B H 0.4956 0.1321 0.4360 0.064 Uiso 1 1 calc R . . H21C H 0.3996 0.0867 0.3868 0.064 Uiso 1 1 calc R . . O5 O 0.2691(3) 0.2536(2) 0.22018(17) 0.0197(9) Uani 1 1 d . . . C22 C 0.1329(5) 0.3609(4) 0.1932(3) 0.0323(16) Uani 1 1 d . . . H22A H 0.1727 0.3757 0.1587 0.048 Uiso 1 1 calc R . . H22B H 0.0989 0.4087 0.2089 0.048 Uiso 1 1 calc R . . H22C H 0.0708 0.3224 0.1784 0.048 Uiso 1 1 calc R . . C23 C 0.2196(5) 0.3236(4) 0.2452(3) 0.0222(14) Uani 1 1 d . . . H23 H 0.2832 0.3628 0.2600 0.027 Uiso 1 1 calc R . . C24 C 0.1649(5) 0.2971(4) 0.2994(3) 0.0293(16) Uani 1 1 d . . . H24A H 0.2239 0.2709 0.3305 0.044 Uiso 1 1 calc R . . H24B H 0.1016 0.2595 0.2848 0.044 Uiso 1 1 calc R . . H24C H 0.1337 0.3436 0.3183 0.044 Uiso 1 1 calc R . . O6 O 0.4980(3) 0.3004(2) 0.06203(17) 0.0190(9) Uani 1 1 d . . . C25 C 0.2897(5) 0.3332(4) 0.0543(3) 0.0308(16) Uani 1 1 d . . . H25A H 0.2895 0.3100 0.0956 0.046 Uiso 1 1 calc R . . H25B H 0.2682 0.2922 0.0222 0.046 Uiso 1 1 calc R . . H25C H 0.2334 0.3772 0.0472 0.046 Uiso 1 1 calc R . . C26 C 0.4106(5) 0.3647(3) 0.0508(3) 0.0224(14) Uani 1 1 d . . . H26 H 0.4316 0.4076 0.0827 0.027 Uiso 1 1 calc R . . C27 C 0.4180(6) 0.3975(4) -0.0132(3) 0.0339(17) Uani 1 1 d . . . H27A H 0.4981 0.4148 -0.0142 0.051 Uiso 1 1 calc R . . H27B H 0.3651 0.4432 -0.0222 0.051 Uiso 1 1 calc R . . H27C H 0.3956 0.3559 -0.0446 0.051 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 0.0155(3) 0.0135(3) 0.0150(3) -0.0006(2) 0.0018(2) -0.0001(2) Mo2 0.0152(3) 0.0144(3) 0.0163(3) 0.0011(2) 0.0032(2) -0.0003(2) P 0.0165(9) 0.0128(8) 0.0167(8) -0.0012(6) 0.0030(7) -0.0021(6) N1 0.017(3) 0.016(3) 0.013(2) 0.002(2) 0.006(2) 0.0008(19) Si1 0.0243(10) 0.0160(9) 0.0219(10) -0.0023(7) 0.0017(8) -0.0057(7) C1 0.030(4) 0.020(4) 0.048(4) -0.006(3) 0.004(3) -0.010(3) C2 0.028(4) 0.027(4) 0.024(4) -0.008(3) -0.003(3) -0.006(3) C3 0.030(4) 0.028(4) 0.025(4) 0.000(3) -0.001(3) -0.007(3) N2 0.018(3) 0.017(3) 0.018(3) -0.002(2) 0.005(2) -0.001(2) Si2 0.0219(10) 0.0152(9) 0.0282(10) -0.0001(7) 0.0068(8) 0.0018(7) C4 0.018(4) 0.015(3) 0.038(4) 0.005(3) 0.005(3) -0.002(2) C5 0.030(4) 0.017(4) 0.034(4) 0.004(3) 0.009(3) 0.002(3) C6 0.036(4) 0.023(4) 0.043(4) -0.007(3) 0.013(4) 0.004(3) Si3 0.0249(10) 0.0243(10) 0.0168(9) -0.0012(7) 0.0080(8) -0.0051(7) C7 0.029(4) 0.024(4) 0.024(4) 0.004(3) 0.007(3) -0.009(3) C8 0.037(4) 0.036(4) 0.030(4) 0.008(3) 0.017(3) -0.004(3) C9 0.041(4) 0.031(4) 0.028(4) -0.005(3) 0.016(3) -0.006(3) O1 0.012(2) 0.024(2) 0.021(2) 0.0004(18) -0.0028(18) 0.0007(17) C10 0.026(4) 0.024(4) 0.040(4) 0.001(3) 0.005(3) -0.004(3) C11 0.016(3) 0.030(4) 0.026(4) -0.006(3) -0.003(3) 0.000(3) C12 0.023(4) 0.047(5) 0.031(4) 0.005(3) -0.003(3) 0.000(3) O2 0.027(3) 0.022(2) 0.014(2) -0.0023(17) 0.0004(19) -0.0008(18) C13 0.033(4) 0.029(4) 0.020(3) 0.000(3) 0.005(3) -0.011(3) C14 0.021(4) 0.025(4) 0.023(4) -0.003(3) 0.005(3) 0.000(3) C15 0.028(4) 0.051(5) 0.034(4) -0.012(3) 0.004(3) 0.006(3) O3 0.021(2) 0.011(2) 0.024(2) 0.0013(17) -0.0024(19) 0.0029(16) C16 0.066(6) 0.020(4) 0.045(5) -0.010(3) 0.019(4) -0.020(3) C17 0.032(4) 0.009(3) 0.026(4) -0.001(3) 0.003(3) 0.001(3) C18 0.055(6) 0.014(4) 0.167(10) -0.013(5) 0.030(6) -0.002(4) O4 0.025(2) 0.015(2) 0.016(2) 0.0052(16) 0.0075(19) -0.0001(17) C19 0.037(4) 0.036(4) 0.027(4) 0.008(3) 0.006(3) 0.011(3) C20 0.029(4) 0.019(3) 0.013(3) 0.002(2) -0.003(3) 0.002(3) C21 0.054(5) 0.047(5) 0.030(4) 0.017(3) 0.015(4) 0.023(4) O5 0.017(2) 0.018(2) 0.023(2) -0.0031(17) 0.0028(18) 0.0009(17) C22 0.022(4) 0.037(4) 0.038(4) 0.007(3) 0.004(3) 0.008(3) C23 0.018(3) 0.029(4) 0.021(3) -0.006(3) 0.005(3) 0.000(3) C24 0.024(4) 0.036(4) 0.029(4) -0.002(3) 0.009(3) 0.007(3) O6 0.021(2) 0.017(2) 0.018(2) 0.0025(16) 0.0029(19) -0.0006(17) C25 0.029(4) 0.030(4) 0.031(4) 0.014(3) 0.002(3) 0.009(3) C26 0.032(4) 0.013(3) 0.020(3) -0.001(3) -0.002(3) 0.003(3) C27 0.042(5) 0.026(4) 0.031(4) 0.012(3) -0.001(3) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O2 1.935(4) . ? Mo1 O1 1.940(4) . ? Mo1 O3 1.948(4) . ? Mo1 Mo2 2.2636(8) . ? Mo1 P 2.6171(17) . ? Mo2 O5 1.875(4) . ? Mo2 O4 1.888(4) . ? Mo2 N1 2.013(4) . ? Mo2 P 2.8124(17) . ? P O6 1.619(4) . ? P N1 1.659(5) . ? P N2 1.698(5) . ? N1 Si1 1.764(5) . ? Si1 C2 1.847(6) . ? Si1 C3 1.858(6) . ? Si1 C1 1.864(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? N2 Si2 1.773(5) . ? N2 Si3 1.782(5) . ? Si2 C4 1.855(6) . ? Si2 C5 1.872(6) . ? Si2 C6 1.873(6) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? Si3 C7 1.863(6) . ? Si3 C9 1.866(6) . ? Si3 C8 1.868(6) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? O1 C11 1.430(7) . ? C10 C11 1.502(8) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.503(8) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? O2 C14 1.413(7) . ? C13 C14 1.514(8) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.515(8) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? O3 C17 1.444(6) . ? C16 C17 1.502(8) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.494(9) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? O4 C20 1.437(6) . ? C19 C20 1.507(8) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.500(9) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? O5 C23 1.453(6) . ? C22 C23 1.514(8) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.501(8) . ? C23 H23 1.0000 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? O6 C26 1.472(6) . ? C25 C26 1.517(8) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.513(8) . ? C26 H26 1.0000 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Mo1 O1 93.48(16) . . ? O2 Mo1 O3 92.33(16) . . ? O1 Mo1 O3 148.70(16) . . ? O2 Mo1 Mo2 113.23(12) . . ? O1 Mo1 Mo2 102.95(11) . . ? O3 Mo1 Mo2 102.87(11) . . ? O2 Mo1 P 176.81(12) . . ? O1 Mo1 P 85.34(12) . . ? O3 Mo1 P 87.16(12) . . ? Mo2 Mo1 P 69.94(4) . . ? O5 Mo2 O4 111.34(16) . . ? O5 Mo2 N1 116.88(17) . . ? O4 Mo2 N1 116.78(17) . . ? O5 Mo2 Mo1 104.02(11) . . ? O4 Mo2 Mo1 109.07(12) . . ? N1 Mo2 Mo1 96.48(13) . . ? O5 Mo2 P 121.31(12) . . ? O4 Mo2 P 127.33(12) . . ? Mo1 Mo2 P 60.94(4) . . ? O6 P N1 105.8(2) . . ? O6 P N2 95.5(2) . . ? N1 P N2 110.7(2) . . ? O6 P Mo1 124.38(15) . . ? N1 P Mo1 93.98(16) . . ? N2 P Mo1 125.28(17) . . ? O6 P Mo2 125.94(16) . . ? N2 P Mo2 133.94(17) . . ? Mo1 P Mo2 49.12(3) . . ? P N1 Si1 137.0(3) . . ? P N1 Mo2 99.5(2) . . ? Si1 N1 Mo2 121.8(2) . . ? N1 Si1 C2 110.1(2) . . ? N1 Si1 C3 108.1(2) . . ? C2 Si1 C3 111.5(3) . . ? N1 Si1 C1 110.8(3) . . ? C2 Si1 C1 109.5(3) . . ? C3 Si1 C1 106.7(3) . . ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? P N2 Si2 124.2(3) . . ? P N2 Si3 116.8(3) . . ? Si2 N2 Si3 119.0(3) . . ? N2 Si2 C4 113.0(2) . . ? N2 Si2 C5 113.6(2) . . ? C4 Si2 C5 104.1(3) . . ? N2 Si2 C6 107.9(3) . . ? C4 Si2 C6 109.1(3) . . ? C5 Si2 C6 109.0(3) . . ? Si2 C4 H4A 109.5 . . ? Si2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 Si3 C7 111.1(2) . . ? N2 Si3 C9 113.1(3) . . ? C7 Si3 C9 113.2(3) . . ? N2 Si3 C8 112.1(3) . . ? C7 Si3 C8 103.0(3) . . ? C9 Si3 C8 103.7(3) . . ? Si3 C7 H7A 109.5 . . ? Si3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si3 C8 H8A 109.5 . . ? Si3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si3 C9 H9A 109.5 . . ? Si3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 O1 Mo1 118.9(3) . . ? C11 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C11 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O1 C11 C10 110.7(5) . . ? O1 C11 C12 107.9(5) . . ? C10 C11 C12 114.4(5) . . ? O1 C11 H11 107.9 . . ? C10 C11 H11 107.9 . . ? C12 C11 H11 107.9 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 O2 Mo1 137.7(3) . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O2 C14 C13 109.7(5) . . ? O2 C14 C15 109.2(5) . . ? C13 C14 C15 110.9(5) . . ? O2 C14 H14 109.0 . . ? C13 C14 H14 109.0 . . ? C15 C14 H14 109.0 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 O3 Mo1 121.1(3) . . ? C17 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C17 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O3 C17 C18 107.8(5) . . ? O3 C17 C16 110.7(5) . . ? C18 C17 C16 112.4(6) . . ? O3 C17 H17 108.6 . . ? C18 C17 H17 108.6 . . ? C16 C17 H17 108.6 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 O4 Mo2 140.7(3) . . ? C20 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C20 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O4 C20 C21 108.6(5) . . ? O4 C20 C19 109.1(5) . . ? C21 C20 C19 111.0(5) . . ? O4 C20 H20 109.4 . . ? C21 C20 H20 109.4 . . ? C19 C20 H20 109.4 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 O5 Mo2 136.3(3) . . ? C23 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C23 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O5 C23 C24 107.8(5) . . ? O5 C23 C22 108.0(5) . . ? C24 C23 C22 112.9(5) . . ? O5 C23 H23 109.3 . . ? C24 C23 H23 109.3 . . ? C22 C23 H23 109.3 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 O6 P 126.7(3) . . ? C26 C25 H25A 109.5 . . ? C26 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C26 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O6 C26 C27 105.8(5) . . ? O6 C26 C25 111.0(4) . . ? C27 C26 C25 111.9(5) . . ? O6 C26 H26 109.4 . . ? C27 C26 H26 109.4 . . ? C25 C26 H26 109.4 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 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 O1 Mo1 Mo2 O5 161.65(17) . . . . ? O3 Mo1 Mo2 O5 -36.19(17) . . . . ? P Mo1 Mo2 O5 -118.29(13) . . . . ? O1 Mo1 Mo2 O4 42.75(17) . . . . ? O3 Mo1 Mo2 O4 -155.09(17) . . . . ? P Mo1 Mo2 O4 122.81(13) . . . . ? O1 Mo1 Mo2 N1 -78.52(17) . . . . ? O3 Mo1 Mo2 N1 83.64(17) . . . . ? P Mo1 Mo2 N1 1.54(13) . . . . ? O1 Mo1 Mo2 P -80.06(12) . . . . ? O3 Mo1 Mo2 P 82.10(12) . . . . ? O1 Mo1 P O6 -144.0(2) . . . . ? O3 Mo1 P O6 5.6(2) . . . . ? Mo2 Mo1 P O6 110.38(19) . . . . ? O1 Mo1 P N1 103.75(19) . . . . ? O3 Mo1 P N1 -106.66(19) . . . . ? Mo2 Mo1 P N1 -1.86(16) . . . . ? O1 Mo1 P N2 -15.2(2) . . . . ? O3 Mo1 P N2 134.4(2) . . . . ? Mo2 Mo1 P N2 -120.8(2) . . . . ? O1 Mo1 P Mo2 105.61(11) . . . . ? O3 Mo1 P Mo2 -104.80(11) . . . . ? O6 P N1 Si1 39.3(4) . . . . ? N2 P N1 Si1 -63.0(4) . . . . ? Mo1 P N1 Si1 166.8(4) . . . . ? Mo2 P N1 Si1 164.8(5) . . . . ? O6 P N1 Mo2 -125.5(2) . . . . ? N2 P N1 Mo2 132.2(2) . . . . ? Mo1 P N1 Mo2 1.99(17) . . . . ? O5 Mo2 N1 P 107.0(2) . . . . ? O4 Mo2 N1 P -117.5(2) . . . . ? Mo1 Mo2 N1 P -2.31(19) . . . . ? O5 Mo2 N1 Si1 -60.8(3) . . . . ? O4 Mo2 N1 Si1 74.7(3) . . . . ? Mo1 Mo2 N1 Si1 -170.1(2) . . . . ? P Mo2 N1 Si1 -167.8(4) . . . . ? P N1 Si1 C2 -0.9(5) . . . . ? Mo2 N1 Si1 C2 161.3(3) . . . . ? P N1 Si1 C3 -122.9(4) . . . . ? Mo2 N1 Si1 C3 39.3(3) . . . . ? P N1 Si1 C1 120.4(4) . . . . ? Mo2 N1 Si1 C1 -77.3(4) . . . . ? O6 P N2 Si2 -153.7(3) . . . . ? N1 P N2 Si2 -44.5(4) . . . . ? Mo1 P N2 Si2 66.5(3) . . . . ? Mo2 P N2 Si2 2.1(4) . . . . ? O6 P N2 Si3 27.8(3) . . . . ? N1 P N2 Si3 137.0(3) . . . . ? Mo1 P N2 Si3 -112.0(2) . . . . ? Mo2 P N2 Si3 -176.42(12) . . . . ? P N2 Si2 C4 -3.5(4) . . . . ? Si3 N2 Si2 C4 175.0(3) . . . . ? P N2 Si2 C5 -121.9(3) . . . . ? Si3 N2 Si2 C5 56.6(4) . . . . ? P N2 Si2 C6 117.2(3) . . . . ? Si3 N2 Si2 C6 -64.3(4) . . . . ? P N2 Si3 C7 48.1(4) . . . . ? Si2 N2 Si3 C7 -130.5(3) . . . . ? P N2 Si3 C9 -80.5(3) . . . . ? Si2 N2 Si3 C9 100.9(3) . . . . ? P N2 Si3 C8 162.7(3) . . . . ? Si2 N2 Si3 C8 -15.9(4) . . . . ? O2 Mo1 O1 C11 -46.3(4) . . . . ? O3 Mo1 O1 C11 54.0(5) . . . . ? Mo2 Mo1 O1 C11 -161.1(4) . . . . ? P Mo1 O1 C11 130.7(4) . . . . ? Mo1 O1 C11 C10 -83.1(5) . . . . ? Mo1 O1 C11 C12 151.0(4) . . . . ? O1 Mo1 O2 C14 -98.5(5) . . . . ? O3 Mo1 O2 C14 112.2(5) . . . . ? Mo2 Mo1 O2 C14 7.2(5) . . . . ? Mo1 O2 C14 C13 110.6(5) . . . . ? Mo1 O2 C14 C15 -127.6(5) . . . . ? O2 Mo1 O3 C17 43.9(4) . . . . ? O1 Mo1 O3 C17 -56.7(5) . . . . ? Mo2 Mo1 O3 C17 158.4(4) . . . . ? P Mo1 O3 C17 -132.9(4) . . . . ? Mo1 O3 C17 C18 -144.1(5) . . . . ? Mo1 O3 C17 C16 92.6(5) . . . . ? O5 Mo2 O4 C20 -99.9(5) . . . . ? N1 Mo2 O4 C20 122.3(5) . . . . ? Mo1 Mo2 O4 C20 14.3(6) . . . . ? P Mo2 O4 C20 81.8(6) . . . . ? Mo2 O4 C20 C21 104.4(6) . . . . ? Mo2 O4 C20 C19 -134.6(5) . . . . ? O4 Mo2 O5 C23 94.9(5) . . . . ? N1 Mo2 O5 C23 -127.3(5) . . . . ? Mo1 Mo2 O5 C23 -22.4(5) . . . . ? P Mo2 O5 C23 -86.7(5) . . . . ? Mo2 O5 C23 C24 -107.4(5) . . . . ? Mo2 O5 C23 C22 130.3(5) . . . . ? N1 P O6 C26 88.3(4) . . . . ? N2 P O6 C26 -158.3(4) . . . . ? Mo1 P O6 C26 -18.1(5) . . . . ? Mo2 P O6 C26 43.0(5) . . . . ? P O6 C26 C27 164.2(4) . . . . ? P O6 C26 C25 -74.3(6) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.76 _refine_diff_density_min -0.56 _refine_diff_density_rms 0.124 #===================================================================== data_anat6abs #TrackingRef '- C1DT10099H_ccdc_807550_807553_cif.txt' _database_code_depnum_ccdc_archive 'CCDC 807552' #TrackingRef 'Kovalenko_ChemCommun.cif' #===================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H69 Mo2 N2 O6 P S Si2' _chemical_formula_weight 840.94 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' Si Si 0.0817 0.0704 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.439(3) _cell_length_b 17.008(5) _cell_length_c 25.776(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4138(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4 _cell_measurement_theta_min 55 _cell_measurement_theta_max 10655 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.350 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1768 _exptl_absorpt_coefficient_mu 0.789 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.858 _exptl_absorpt_correction_T_max 0.941 _exptl_absorpt_process_details 'CrysAlis RED (Oxford Diffraction, 1995-2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KUMA KM4 CCD kappa-geometry diffractometer' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53107 _diffrn_reflns_av_R_equivalents 0.1102 _diffrn_reflns_av_sigmaI/netI 0.1334 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 28.58 _reflns_number_total 10070 _reflns_number_gt 7195 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 1995-2003)' _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 1995-2003)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 1995-2003)' _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^)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _chemical_absolute_configuration ad _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.44(3) _refine_ls_number_reflns 10070 _refine_ls_number_parameters 401 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0776 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.0470 _refine_ls_wR_factor_gt 0.0435 _refine_ls_goodness_of_fit_ref 0.898 _refine_ls_restrained_S_all 0.898 _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 0.48053(3) 0.53197(2) 0.153239(12) 0.01431(9) Uani 1 1 d . . . Mo2 Mo 0.26302(3) 0.50755(2) 0.123716(14) 0.01416(8) Uani 1 1 d . . . P P 0.42878(8) 0.52528(8) 0.01361(4) 0.0152(3) Uani 1 1 d . . . S S 0.59288(8) 0.53555(7) 0.06220(4) 0.0166(3) Uani 1 1 d . . . Si1 Si 0.53573(10) 0.50862(7) -0.09396(3) 0.0193(3) Uani 1 1 d . . . C4 C 0.6918(4) 0.5719(2) -0.07854(15) 0.0244(11) Uani 1 1 d . . . H4A H 0.6659 0.6098 -0.0515 0.037 Uiso 1 1 calc R . . H4B H 0.7214 0.6002 -0.1098 0.037 Uiso 1 1 calc R . . H4C H 0.7700 0.5389 -0.0662 0.037 Uiso 1 1 calc R . . C5 C 0.3986(4) 0.5621(2) -0.13233(16) 0.0322(12) Uani 1 1 d . . . H5A H 0.3268 0.5247 -0.1445 0.048 Uiso 1 1 calc R . . H5B H 0.4433 0.5875 -0.1622 0.048 Uiso 1 1 calc R . . H5C H 0.3535 0.6020 -0.1104 0.048 Uiso 1 1 calc R . . C6 C 0.5995(4) 0.4320(2) -0.14037(15) 0.0272(12) Uani 1 1 d . . . H6A H 0.6661 0.3969 -0.1227 0.041 Uiso 1 1 calc R . . H6B H 0.6472 0.4575 -0.1697 0.041 Uiso 1 1 calc R . . H6C H 0.5186 0.4015 -0.1531 0.041 Uiso 1 1 calc R . . Si2 Si 0.51981(11) 0.36571(7) -0.01968(4) 0.0198(3) Uani 1 1 d . . . C7 C 0.4375(4) 0.2985(2) -0.06853(15) 0.0260(11) Uani 1 1 d . . . H7A H 0.3481 0.3212 -0.0808 0.039 Uiso 1 1 calc R . . H7B H 0.4191 0.2472 -0.0525 0.039 Uiso 1 1 calc R . . H7C H 0.5022 0.2917 -0.0979 0.039 Uiso 1 1 calc R . . C8 C 0.4643(4) 0.3342(2) 0.04583(14) 0.0248(11) Uani 1 1 d . . . H8A H 0.5032 0.3705 0.0717 0.037 Uiso 1 1 calc R . . H8B H 0.4995 0.2810 0.0526 0.037 Uiso 1 1 calc R . . H8C H 0.3606 0.3344 0.0480 0.037 Uiso 1 1 calc R . . C9 C 0.7181(3) 0.3582(2) -0.01987(16) 0.0273(11) Uani 1 1 d . . . H9A H 0.7551 0.3788 -0.0527 0.041 Uiso 1 1 calc R . . H9B H 0.7461 0.3031 -0.0160 0.041 Uiso 1 1 calc R . . H9C H 0.7568 0.3890 0.0090 0.041 Uiso 1 1 calc R . . N2 N 0.4701(3) 0.46628(19) -0.03507(10) 0.0136(7) Uani 1 1 d . . . N1 N 0.2821(2) 0.5042(2) 0.04477(10) 0.0137(7) Uani 1 1 d . . . C10 C 0.1400(3) 0.4863(3) 0.01654(14) 0.0190(11) Uani 1 1 d . . . C1 C 0.1277(4) 0.5252(3) -0.03659(15) 0.0443(15) Uani 1 1 d . . . H1A H 0.0332 0.5153 -0.0509 0.066 Uiso 1 1 calc R . . H1B H 0.1996 0.5034 -0.0599 0.066 Uiso 1 1 calc R . . H1C H 0.1423 0.5820 -0.0330 0.066 Uiso 1 1 calc R . . C2 C 0.1252(4) 0.3974(3) 0.0101(2) 0.0409(15) Uani 1 1 d . . . H2A H 0.1380 0.3717 0.0438 0.061 Uiso 1 1 calc R . . H2B H 0.1974 0.3783 -0.0142 0.061 Uiso 1 1 calc R . . H2C H 0.0308 0.3851 -0.0035 0.061 Uiso 1 1 calc R . . C3 C 0.0181(3) 0.5157(3) 0.05087(12) 0.0315(12) Uani 1 1 d . . . H3A H -0.0712 0.5121 0.0316 0.047 Uiso 1 1 calc R . . H3B H 0.0355 0.5705 0.0607 0.047 Uiso 1 1 calc R . . H3C H 0.0123 0.4831 0.0822 0.047 Uiso 1 1 calc R . . O1 O 0.5678(2) 0.42866(15) 0.15507(10) 0.0187(7) Uani 1 1 d . . . C11 C 0.7102(4) 0.3156(3) 0.17201(18) 0.0373(14) Uani 1 1 d . . . H11A H 0.6877 0.3154 0.2091 0.056 Uiso 1 1 calc R . . H11B H 0.8046 0.2931 0.1667 0.056 Uiso 1 1 calc R . . H11C H 0.6399 0.2841 0.1532 0.056 Uiso 1 1 calc R . . C12 C 0.7076(3) 0.4000(2) 0.15176(17) 0.0232(10) Uani 1 1 d . . . H12 H 0.7332 0.3980 0.1141 0.028 Uiso 1 1 calc R . . C13 C 0.8143(4) 0.4525(3) 0.17825(16) 0.0373(14) Uani 1 1 d . . . H13A H 0.8095 0.5053 0.1632 0.056 Uiso 1 1 calc R . . H13B H 0.9097 0.4310 0.1733 0.056 Uiso 1 1 calc R . . H13C H 0.7930 0.4552 0.2154 0.056 Uiso 1 1 calc R . . O2 O 0.4772(2) 0.64567(14) 0.14469(10) 0.0198(7) Uani 1 1 d . . . C14 C 0.7140(4) 0.6842(3) 0.17137(19) 0.0437(15) Uani 1 1 d . . . H14A H 0.6843 0.6787 0.2076 0.065 Uiso 1 1 calc R . . H14B H 0.7817 0.7276 0.1684 0.065 Uiso 1 1 calc R . . H14C H 0.7588 0.6353 0.1598 0.065 Uiso 1 1 calc R . . C15 C 0.5868(3) 0.7010(2) 0.13819(15) 0.0200(11) Uani 1 1 d . . . H15 H 0.6178 0.6988 0.1011 0.024 Uiso 1 1 calc R . . C16 C 0.5290(4) 0.7820(2) 0.1481(2) 0.0614(17) Uani 1 1 d . . . H16A H 0.4487 0.7918 0.1249 0.092 Uiso 1 1 calc R . . H16B H 0.6033 0.8210 0.1417 0.092 Uiso 1 1 calc R . . H16C H 0.4975 0.7858 0.1842 0.092 Uiso 1 1 calc R . . O3 O 0.4285(2) 0.53304(18) 0.22582(9) 0.0192(7) Uani 1 1 d . . . C17 C 0.4684(5) 0.6129(3) 0.30093(16) 0.0390(13) Uani 1 1 d . . . H17A H 0.4621 0.6603 0.2794 0.058 Uiso 1 1 calc R . . H17B H 0.5329 0.6225 0.3300 0.058 Uiso 1 1 calc R . . H17C H 0.3742 0.5996 0.3143 0.058 Uiso 1 1 calc R . . C18 C 0.5239(4) 0.5454(2) 0.26859(13) 0.0202(10) Uani 1 1 d . . . H18 H 0.6198 0.5592 0.2549 0.024 Uiso 1 1 calc R . . C19 C 0.5333(4) 0.4702(3) 0.29909(15) 0.0362(12) Uani 1 1 d . . . H19A H 0.4388 0.4556 0.3116 0.054 Uiso 1 1 calc R . . H19B H 0.5967 0.4778 0.3288 0.054 Uiso 1 1 calc R . . H19C H 0.5704 0.4283 0.2768 0.054 Uiso 1 1 calc R . . O4 O 0.2100(2) 0.40898(15) 0.15083(10) 0.0154(6) Uani 1 1 d . . . C20 C 0.2311(5) 0.2727(2) 0.17126(16) 0.0404(13) Uani 1 1 d . . . H20A H 0.1290 0.2672 0.1653 0.061 Uiso 1 1 calc R . . H20B H 0.2613 0.2349 0.1977 0.061 Uiso 1 1 calc R . . H20C H 0.2823 0.2625 0.1389 0.061 Uiso 1 1 calc R . . C21 C 0.2629(4) 0.3554(2) 0.18969(14) 0.0181(10) Uani 1 1 d . . . H21 H 0.3678 0.3621 0.1931 0.022 Uiso 1 1 calc R . . C22 C 0.1930(4) 0.3745(3) 0.24102(16) 0.0316(13) Uani 1 1 d . . . H22A H 0.2161 0.4286 0.2510 0.047 Uiso 1 1 calc R . . H22B H 0.2276 0.3382 0.2677 0.047 Uiso 1 1 calc R . . H22C H 0.0901 0.3690 0.2376 0.047 Uiso 1 1 calc R . . O5 O 0.1569(2) 0.59066(16) 0.15309(12) 0.0181(6) Uani 1 1 d . . . C23 C 0.0868(4) 0.6241(2) 0.23979(15) 0.0236(11) Uani 1 1 d . . . H23A H -0.0116 0.6162 0.2288 0.035 Uiso 1 1 calc R . . H23B H 0.0903 0.6654 0.2663 0.035 Uiso 1 1 calc R . . H23C H 0.1241 0.5750 0.2542 0.035 Uiso 1 1 calc R . . C24 C 0.1765(4) 0.6488(3) 0.19302(15) 0.0193(11) Uani 1 1 d . . . H24 H 0.2787 0.6507 0.2032 0.023 Uiso 1 1 calc R . . C25 C 0.1319(4) 0.7277(3) 0.17236(18) 0.0308(13) Uani 1 1 d . . . H25A H 0.1915 0.7418 0.1426 0.046 Uiso 1 1 calc R . . H25B H 0.1425 0.7675 0.1996 0.046 Uiso 1 1 calc R . . H25C H 0.0326 0.7254 0.1614 0.046 Uiso 1 1 calc R . . O6 O 0.4070(2) 0.60461(16) -0.01913(10) 0.0149(7) Uani 1 1 d . . . C26 C 0.2982(6) 0.7039(3) 0.0369(2) 0.0648(19) Uani 1 1 d . . . H26A H 0.2090 0.6983 0.0178 0.097 Uiso 1 1 calc R . . H26B H 0.3072 0.7581 0.0495 0.097 Uiso 1 1 calc R . . H26C H 0.2987 0.6677 0.0665 0.097 Uiso 1 1 calc R . . C27 C 0.4186(4) 0.6854(3) 0.00208(17) 0.0288(12) Uani 1 1 d . . . H27 H 0.5102 0.6915 0.0212 0.035 Uiso 1 1 calc R . . C28 C 0.4176(5) 0.7381(3) -0.04581(17) 0.0413(14) Uani 1 1 d . . . H28A H 0.4899 0.7200 -0.0704 0.062 Uiso 1 1 calc R . . H28B H 0.4382 0.7924 -0.0355 0.062 Uiso 1 1 calc R . . H28C H 0.3242 0.7358 -0.0623 0.062 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 0.01303(14) 0.0159(2) 0.01397(16) -0.00064(18) -0.00136(14) 0.00004(15) Mo2 0.01223(13) 0.0171(2) 0.01316(13) 0.00075(18) 0.00004(14) -0.00055(15) P 0.0118(4) 0.0187(8) 0.0151(5) 0.0023(6) 0.0001(4) 0.0007(5) S 0.0116(4) 0.0222(8) 0.0159(5) 0.0002(5) -0.0006(4) -0.0011(5) Si1 0.0203(5) 0.0244(8) 0.0131(5) 0.0006(5) 0.0002(4) -0.0012(6) C4 0.020(2) 0.031(3) 0.022(2) 0.001(2) 0.0063(18) -0.0058(19) C5 0.033(2) 0.046(4) 0.018(3) 0.008(2) -0.0035(19) -0.008(2) C6 0.037(2) 0.027(3) 0.018(3) -0.002(2) 0.0028(18) -0.006(2) Si2 0.0177(5) 0.0212(8) 0.0207(6) -0.0023(6) -0.0006(5) -0.0015(6) C7 0.025(2) 0.023(3) 0.030(3) -0.005(2) 0.0029(19) -0.004(2) C8 0.030(2) 0.014(3) 0.030(3) 0.002(2) -0.002(2) 0.001(2) C9 0.021(2) 0.026(3) 0.035(3) 0.001(2) 0.0013(19) 0.006(2) N2 0.0120(13) 0.012(2) 0.0170(15) -0.0051(16) -0.0014(13) 0.0003(16) N1 0.0113(12) 0.017(2) 0.0122(14) 0.0018(17) -0.0012(11) -0.0002(15) C10 0.0108(16) 0.030(4) 0.016(2) -0.001(2) -0.0027(15) -0.003(2) C1 0.0191(18) 0.088(5) 0.026(2) 0.014(3) -0.0078(16) -0.006(3) C2 0.020(2) 0.051(4) 0.052(4) -0.009(3) -0.011(2) -0.007(2) C3 0.0154(16) 0.055(4) 0.024(2) -0.005(2) -0.0110(17) -0.005(2) O1 0.0126(11) 0.0211(19) 0.0224(15) 0.0024(15) 0.0033(12) 0.0059(11) C11 0.031(3) 0.033(4) 0.048(4) 0.013(3) 0.002(2) 0.017(2) C12 0.0178(18) 0.027(3) 0.025(2) 0.003(2) 0.0030(19) 0.0063(19) C13 0.026(2) 0.044(4) 0.042(3) -0.003(3) -0.009(2) 0.003(2) O2 0.0165(12) 0.0098(17) 0.0331(17) -0.0039(13) 0.0086(12) -0.0030(13) C14 0.039(3) 0.034(4) 0.058(4) -0.006(3) -0.013(3) -0.014(2) C15 0.0220(19) 0.017(3) 0.021(3) -0.002(2) 0.0033(17) -0.0080(19) C16 0.033(2) 0.021(3) 0.131(5) -0.006(4) -0.008(3) -0.001(2) O3 0.0224(12) 0.021(2) 0.0139(14) 0.0014(15) -0.0028(10) 0.0027(14) C17 0.042(3) 0.047(4) 0.027(3) -0.016(3) -0.004(2) -0.002(3) C18 0.0221(18) 0.019(3) 0.019(2) 0.004(2) -0.0043(18) -0.002(2) C19 0.031(2) 0.043(3) 0.034(2) 0.012(3) -0.005(2) -0.004(3) O4 0.0207(13) 0.0138(17) 0.0116(14) 0.0052(14) -0.0022(12) -0.0080(12) C20 0.076(4) 0.017(3) 0.028(3) 0.007(2) 0.000(3) -0.001(3) C21 0.0190(19) 0.019(3) 0.016(2) 0.002(2) 0.0012(18) -0.003(2) C22 0.041(3) 0.035(4) 0.019(2) 0.004(2) 0.005(2) 0.006(2) O5 0.0145(12) 0.0203(19) 0.0196(16) -0.0040(16) 0.0030(13) 0.0069(12) C23 0.028(2) 0.024(3) 0.019(2) -0.003(2) -0.0007(19) 0.005(2) C24 0.0214(19) 0.019(3) 0.017(2) -0.010(2) -0.0008(18) 0.002(2) C25 0.028(2) 0.022(3) 0.042(3) 0.002(3) 0.007(2) 0.005(2) O6 0.0141(13) 0.0085(19) 0.0219(16) 0.0056(14) -0.0023(12) 0.0024(12) C26 0.109(5) 0.024(4) 0.062(4) 0.003(3) 0.054(3) 0.019(4) C27 0.040(3) 0.017(3) 0.030(3) -0.003(2) -0.009(2) 0.011(2) C28 0.051(3) 0.030(4) 0.042(3) 0.007(3) 0.005(3) -0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O3 1.934(2) . ? Mo1 O1 1.941(2) . ? Mo1 O2 1.947(2) . ? Mo1 Mo2 2.2287(7) . ? Mo1 S 2.5759(11) . ? Mo2 O4 1.884(3) . ? Mo2 O5 1.891(2) . ? Mo2 N1 2.044(3) . ? P O6 1.605(3) . ? P N1 1.640(3) . ? P N2 1.653(3) . ? P S 1.9996(13) . ? Si1 N2 1.791(3) . ? Si1 C5 1.865(4) . ? Si1 C4 1.867(4) . ? Si1 C6 1.868(4) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? Si2 N2 1.818(3) . ? Si2 C8 1.848(4) . ? Si2 C7 1.870(4) . ? Si2 C9 1.876(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? N1 C10 1.556(4) . ? C10 C1 1.526(5) . ? C10 C2 1.528(6) . ? C10 C3 1.535(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? O1 C12 1.409(4) . ? C11 C12 1.527(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.510(5) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? O2 C15 1.409(4) . ? C14 C15 1.501(5) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.503(5) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? O3 C18 1.438(4) . ? C17 C18 1.512(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.503(5) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? O4 C21 1.444(4) . ? C20 C21 1.515(5) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.514(5) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? O5 C24 1.439(4) . ? C23 C24 1.532(5) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.505(5) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? O6 C27 1.482(5) . ? C26 C27 1.483(6) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.526(6) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Mo1 O1 95.32(12) . . ? O3 Mo1 O2 95.51(12) . . ? O1 Mo1 O2 155.35(9) . . ? O3 Mo1 Mo2 95.64(7) . . ? O1 Mo1 Mo2 103.33(7) . . ? O2 Mo1 Mo2 97.55(7) . . ? O3 Mo1 S 170.20(7) . . ? O1 Mo1 S 82.46(8) . . ? O2 Mo1 S 83.12(8) . . ? Mo2 Mo1 S 94.16(3) . . ? O4 Mo2 O5 112.08(10) . . ? O4 Mo2 N1 111.58(13) . . ? O5 Mo2 N1 117.81(13) . . ? O4 Mo2 Mo1 106.50(7) . . ? O5 Mo2 Mo1 102.25(7) . . ? N1 Mo2 Mo1 105.30(7) . . ? O6 P N1 109.49(14) . . ? O6 P N2 98.13(15) . . ? N1 P N2 115.97(16) . . ? O6 P S 110.79(11) . . ? N1 P S 111.47(11) . . ? N2 P S 110.23(10) . . ? P S Mo1 104.46(5) . . ? N2 Si1 C5 113.90(15) . . ? N2 Si1 C4 108.93(16) . . ? C5 Si1 C4 112.32(17) . . ? N2 Si1 C6 111.95(17) . . ? C5 Si1 C6 102.93(18) . . ? C4 Si1 C6 106.49(16) . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 Si2 C8 113.52(16) . . ? N2 Si2 C7 108.75(16) . . ? C8 Si2 C7 108.66(18) . . ? N2 Si2 C9 108.72(16) . . ? C8 Si2 C9 105.42(18) . . ? C7 Si2 C9 111.80(19) . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si2 C8 H8A 109.5 . . ? Si2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si2 C9 H9A 109.5 . . ? Si2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? P N2 Si1 118.74(19) . . ? P N2 Si2 117.81(16) . . ? Si1 N2 Si2 118.30(16) . . ? C10 N1 P 122.8(2) . . ? C10 N1 Mo2 113.27(18) . . ? P N1 Mo2 123.78(14) . . ? C1 C10 C2 109.0(4) . . ? C1 C10 C3 108.6(3) . . ? C2 C10 C3 108.4(3) . . ? C1 C10 N1 113.6(3) . . ? C2 C10 N1 108.8(3) . . ? C3 C10 N1 108.2(3) . . ? C10 C1 H1A 109.5 . . ? C10 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C10 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C10 C2 H2A 109.5 . . ? C10 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C10 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C10 C3 H3A 109.5 . . ? C10 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C10 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C12 O1 Mo1 135.2(2) . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O1 C12 C13 113.1(3) . . ? O1 C12 C11 108.7(3) . . ? C13 C12 C11 113.0(3) . . ? O1 C12 H12 107.3 . . ? C13 C12 H12 107.3 . . ? C11 C12 H12 107.3 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 O2 Mo1 131.7(2) . . ? C15 C14 H14A 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C15 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O2 C15 C14 113.1(3) . . ? O2 C15 C16 109.0(3) . . ? C14 C15 C16 111.6(4) . . ? O2 C15 H15 107.7 . . ? C14 C15 H15 107.7 . . ? C16 C15 H15 107.7 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 O3 Mo1 125.7(2) . . ? C18 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C18 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O3 C18 C19 108.3(3) . . ? O3 C18 C17 108.5(3) . . ? C19 C18 C17 112.2(3) . . ? O3 C18 H18 109.3 . . ? C19 C18 H18 109.3 . . ? C17 C18 H18 109.3 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 O4 Mo2 136.7(2) . . ? C21 C20 H20A 109.5 . . ? C21 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C21 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O4 C21 C22 108.7(3) . . ? O4 C21 C20 107.5(3) . . ? C22 C21 C20 112.7(3) . . ? O4 C21 H21 109.3 . . ? C22 C21 H21 109.3 . . ? C20 C21 H21 109.3 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 O5 Mo2 137.0(2) . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C24 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O5 C24 C25 108.9(3) . . ? O5 C24 C23 107.6(3) . . ? C25 C24 C23 111.6(3) . . ? O5 C24 H24 109.6 . . ? C25 C24 H24 109.6 . . ? C23 C24 H24 109.6 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 O6 P 125.2(2) . . ? C27 C26 H26A 109.5 . . ? C27 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C27 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O6 C27 C26 111.4(4) . . ? O6 C27 C28 104.3(3) . . ? C26 C27 C28 111.1(4) . . ? O6 C27 H27 110.0 . . ? C26 C27 H27 110.0 . . ? C28 C27 H27 110.0 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 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 O3 Mo1 Mo2 O4 -62.15(12) . . . . ? O1 Mo1 Mo2 O4 34.69(12) . . . . ? O2 Mo1 Mo2 O4 -158.49(11) . . . . ? S Mo1 Mo2 O4 117.92(9) . . . . ? O3 Mo1 Mo2 O5 55.58(13) . . . . ? O1 Mo1 Mo2 O5 152.43(12) . . . . ? O2 Mo1 Mo2 O5 -40.75(12) . . . . ? S Mo1 Mo2 O5 -124.35(10) . . . . ? O3 Mo1 Mo2 N1 179.25(14) . . . . ? O1 Mo1 Mo2 N1 -83.91(13) . . . . ? O2 Mo1 Mo2 N1 82.91(13) . . . . ? S Mo1 Mo2 N1 -0.68(11) . . . . ? O6 P S Mo1 113.27(11) . . . . ? N1 P S Mo1 -8.93(15) . . . . ? N2 P S Mo1 -139.20(12) . . . . ? O1 Mo1 S P 108.07(9) . . . . ? O2 Mo1 S P -91.97(9) . . . . ? Mo2 Mo1 S P 5.15(6) . . . . ? O6 P N2 Si1 21.49(17) . . . . ? N1 P N2 Si1 137.88(17) . . . . ? S P N2 Si1 -94.28(15) . . . . ? O6 P N2 Si2 175.70(16) . . . . ? N1 P N2 Si2 -67.9(2) . . . . ? S P N2 Si2 59.93(18) . . . . ? C5 Si1 N2 P -71.7(2) . . . . ? C4 Si1 N2 P 54.5(2) . . . . ? C6 Si1 N2 P 172.03(16) . . . . ? C5 Si1 N2 Si2 134.21(18) . . . . ? C4 Si1 N2 Si2 -99.6(2) . . . . ? C6 Si1 N2 Si2 17.9(2) . . . . ? C8 Si2 N2 P 18.1(2) . . . . ? C7 Si2 N2 P 139.23(18) . . . . ? C9 Si2 N2 P -98.8(2) . . . . ? C8 Si2 N2 Si1 172.48(18) . . . . ? C7 Si2 N2 Si1 -66.4(2) . . . . ? C9 Si2 N2 Si1 55.5(2) . . . . ? O6 P N1 C10 62.0(4) . . . . ? N2 P N1 C10 -47.9(4) . . . . ? S P N1 C10 -175.1(3) . . . . ? O6 P N1 Mo2 -112.8(2) . . . . ? N2 P N1 Mo2 137.4(2) . . . . ? S P N1 Mo2 10.2(3) . . . . ? O4 Mo2 N1 C10 64.0(3) . . . . ? O5 Mo2 N1 C10 -67.7(3) . . . . ? Mo1 Mo2 N1 C10 179.1(3) . . . . ? O4 Mo2 N1 P -120.8(2) . . . . ? O5 Mo2 N1 P 107.4(2) . . . . ? Mo1 Mo2 N1 P -5.7(2) . . . . ? P N1 C10 C1 -26.9(5) . . . . ? Mo2 N1 C10 C1 148.3(3) . . . . ? P N1 C10 C2 94.8(4) . . . . ? Mo2 N1 C10 C2 -90.0(3) . . . . ? P N1 C10 C3 -147.6(3) . . . . ? Mo2 N1 C10 C3 27.6(4) . . . . ? O3 Mo1 O1 C12 -109.4(4) . . . . ? O2 Mo1 O1 C12 6.3(5) . . . . ? Mo2 Mo1 O1 C12 153.5(3) . . . . ? S Mo1 O1 C12 60.9(4) . . . . ? Mo1 O1 C12 C13 36.7(5) . . . . ? Mo1 O1 C12 C11 163.0(3) . . . . ? O3 Mo1 O2 C15 108.1(3) . . . . ? O1 Mo1 O2 C15 -7.6(5) . . . . ? Mo2 Mo1 O2 C15 -155.4(3) . . . . ? S Mo1 O2 C15 -62.1(3) . . . . ? Mo1 O2 C15 C14 -39.8(5) . . . . ? Mo1 O2 C15 C16 -164.5(3) . . . . ? O1 Mo1 O3 C18 75.2(3) . . . . ? O2 Mo1 O3 C18 -82.6(3) . . . . ? Mo2 Mo1 O3 C18 179.2(3) . . . . ? Mo1 O3 C18 C19 -112.9(3) . . . . ? Mo1 O3 C18 C17 125.1(3) . . . . ? O5 Mo2 O4 C21 -99.4(3) . . . . ? N1 Mo2 O4 C21 126.0(3) . . . . ? Mo1 Mo2 O4 C21 11.6(3) . . . . ? Mo2 O4 C21 C22 91.5(4) . . . . ? Mo2 O4 C21 C20 -146.3(3) . . . . ? O4 Mo2 O5 C24 99.6(4) . . . . ? N1 Mo2 O5 C24 -128.9(4) . . . . ? Mo1 Mo2 O5 C24 -14.1(4) . . . . ? Mo2 O5 C24 C25 132.6(3) . . . . ? Mo2 O5 C24 C23 -106.2(3) . . . . ? N1 P O6 C27 82.0(3) . . . . ? N2 P O6 C27 -156.7(3) . . . . ? S P O6 C27 -41.4(3) . . . . ? P O6 C27 C26 -70.7(4) . . . . ? P O6 C27 C28 169.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 28.58 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.58 _refine_diff_density_min -0.63 _refine_diff_density_rms 0.093 #===================================================================== data_anat1abs #TrackingRef '- C1DT10099H_ccdc_807550_807553_cif.txt' _database_code_depnum_ccdc_archive 'CCDC 807553' #TrackingRef 'Kovalenko_ChemCommun.cif' #===================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H78 Mo2 N3 O6 P Si4' _chemical_formula_sum 'C30 H78 Mo2 N3 O6 P Si4' _chemical_formula_weight 912.16 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' Si Si 0.0817 0.0704 '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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.760(3) _cell_length_b 13.424(4) _cell_length_c 16.339(5) _cell_angle_alpha 88.52(3) _cell_angle_beta 86.50(3) _cell_angle_gamma 64.50(3) _cell_volume 2323.8(12) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 30064 _cell_measurement_theta_min 4 _cell_measurement_theta_max 60 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.304 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 964 _exptl_absorpt_coefficient_mu 0.714 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.7632 _exptl_absorpt_correction_T_max 0.8703 _exptl_absorpt_process_details ; CrysAlis RED (Oxford Diffraction, 1995-2003) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; 'Oxford Xcalibur PX \k-geometry diffractometer with CCD area detector' ; _diffrn_measurement_method '\w and \f' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35863 _diffrn_reflns_av_R_equivalents 0.0352 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 4.68 _diffrn_reflns_theta_max 30.00 _reflns_number_total 13203 _reflns_number_gt 10678 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 1995-2003)' _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 1995-2003)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 1995-2003)' _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^)+(0.0688P)^2^+0.6707P] 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 13203 _refine_ls_number_parameters 439 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0559 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.1191 _refine_ls_wR_factor_gt 0.1128 _refine_ls_goodness_of_fit_ref 1.133 _refine_ls_restrained_S_all 1.133 _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 0.437744(19) 0.198022(17) 0.176532(12) 0.01740(6) Uani 1 1 d . . . Mo2 Mo 0.406956(18) 0.301813(16) 0.288886(11) 0.01422(6) Uani 1 1 d . . . P P 0.26059(5) 0.52853(5) 0.24560(3) 0.01389(12) Uani 1 1 d . . . N2 N 0.19869(19) 0.64877(17) 0.29619(12) 0.0172(4) Uani 1 1 d . . . Si3 Si 0.21722(7) 0.65183(6) 0.40359(4) 0.02125(14) Uani 1 1 d . . . C7 C 0.3009(3) 0.5103(2) 0.44502(15) 0.0260(5) Uani 1 1 d . . . H7A H 0.2577 0.4656 0.4304 0.039 Uiso 1 1 calc R . . H7B H 0.3012 0.5137 0.5048 0.039 Uiso 1 1 calc R . . H7C H 0.3879 0.4768 0.4217 0.039 Uiso 1 1 calc R . . C8 C 0.0597(3) 0.7163(3) 0.46249(18) 0.0331(6) Uani 1 1 d . . . H8A H -0.0068 0.7542 0.4243 0.050 Uiso 1 1 calc R . . H8B H 0.0606 0.7696 0.5020 0.050 Uiso 1 1 calc R . . H8C H 0.0435 0.6587 0.4917 0.050 Uiso 1 1 calc R . . C9 C 0.3112(3) 0.7305(2) 0.42538(18) 0.0289(6) Uani 1 1 d . . . H9A H 0.3679 0.7261 0.3777 0.043 Uiso 1 1 calc R . . H9B H 0.3609 0.6984 0.4732 0.043 Uiso 1 1 calc R . . H9C H 0.2537 0.8079 0.4365 0.043 Uiso 1 1 calc R . . Si2 Si 0.10543(7) 0.77562(6) 0.24610(5) 0.02308(15) Uani 1 1 d . . . C4 C 0.0744(3) 0.8953(2) 0.3155(2) 0.0359(7) Uani 1 1 d . . . H4A H 0.0400 0.8835 0.3691 0.054 Uiso 1 1 calc R . . H4B H 0.0135 0.9636 0.2912 0.054 Uiso 1 1 calc R . . H4C H 0.1534 0.9013 0.3223 0.054 Uiso 1 1 calc R . . C5 C 0.1756(3) 0.8129(2) 0.15103(19) 0.0330(6) Uani 1 1 d . . . H5A H 0.2514 0.8209 0.1642 0.049 Uiso 1 1 calc R . . H5B H 0.1140 0.8827 0.1292 0.049 Uiso 1 1 calc R . . H5C H 0.1981 0.7546 0.1100 0.049 Uiso 1 1 calc R . . C6 C -0.0511(3) 0.7832(3) 0.2230(2) 0.0347(7) Uani 1 1 d . . . H6A H -0.0406 0.7331 0.1776 0.052 Uiso 1 1 calc R . . H6B H -0.1071 0.8589 0.2075 0.052 Uiso 1 1 calc R . . H6C H -0.0881 0.7615 0.2716 0.052 Uiso 1 1 calc R . . N3 N 0.21472(19) 0.43545(17) 0.27423(12) 0.0166(4) Uani 1 1 d . . . Si4 Si 0.06626(6) 0.43653(6) 0.28078(4) 0.01815(13) Uani 1 1 d . . . C41 C -0.0231(2) 0.4904(2) 0.18593(17) 0.0260(5) Uani 1 1 d . . . H41A H -0.0303 0.5648 0.1740 0.039 Uiso 1 1 calc R . . H41B H -0.1076 0.4932 0.1946 0.039 Uiso 1 1 calc R . . H41C H 0.0219 0.4415 0.1397 0.039 Uiso 1 1 calc R . . C43 C 0.0756(3) 0.2959(2) 0.29942(18) 0.0276(6) Uani 1 1 d . . . H43A H 0.1414 0.2432 0.2623 0.041 Uiso 1 1 calc R . . H43B H -0.0058 0.2960 0.2894 0.041 Uiso 1 1 calc R . . H43C H 0.0962 0.2744 0.3564 0.041 Uiso 1 1 calc R . . C42 C -0.0337(3) 0.5260(2) 0.36813(17) 0.0276(6) Uani 1 1 d . . . H42A H 0.0099 0.5008 0.4191 0.041 Uiso 1 1 calc R . . H42B H -0.1147 0.5213 0.3732 0.041 Uiso 1 1 calc R . . H42C H -0.0485 0.6027 0.3576 0.041 Uiso 1 1 calc R . . N1 N 0.41003(18) 0.45849(16) 0.24863(11) 0.0146(4) Uani 1 1 d . . . Si1 Si 0.53686(6) 0.49314(5) 0.23853(4) 0.01571(13) Uani 1 1 d . . . C1 C 0.4902(3) 0.6347(2) 0.19485(17) 0.0248(5) Uani 1 1 d . . . H1A H 0.4532 0.6395 0.1419 0.037 Uiso 1 1 calc R . . H1B H 0.5649 0.6494 0.1871 0.037 Uiso 1 1 calc R . . H1C H 0.4281 0.6894 0.2327 0.037 Uiso 1 1 calc R . . C2 C 0.6029(2) 0.4918(2) 0.33991(15) 0.0226(5) Uani 1 1 d . . . H2A H 0.5445 0.5558 0.3722 0.034 Uiso 1 1 calc R . . H2B H 0.6845 0.4950 0.3313 0.034 Uiso 1 1 calc R . . H2C H 0.6145 0.4239 0.3694 0.034 Uiso 1 1 calc R . . C3 C 0.6650(2) 0.3961(2) 0.16771(15) 0.0208(5) Uani 1 1 d . . . H3A H 0.6827 0.3199 0.1829 0.031 Uiso 1 1 calc R . . H3B H 0.7414 0.4075 0.1717 0.031 Uiso 1 1 calc R . . H3C H 0.6381 0.4099 0.1113 0.031 Uiso 1 1 calc R . . O6 O 0.21426(16) 0.57954(14) 0.15780(10) 0.0176(3) Uani 1 1 d . . . C27 C 0.2351(2) 0.5132(2) 0.08375(14) 0.0210(5) Uani 1 1 d . . . H27 H 0.2192 0.4470 0.0970 0.025 Uiso 1 1 calc R . . C26 C 0.1388(3) 0.5886(3) 0.02448(16) 0.0307(6) Uani 1 1 d . . . H26A H 0.0539 0.6158 0.0510 0.046 Uiso 1 1 calc R . . H26B H 0.1432 0.5471 -0.0250 0.046 Uiso 1 1 calc R . . H26C H 0.1577 0.6513 0.0095 0.046 Uiso 1 1 calc R . . C28 C 0.3691(2) 0.4772(2) 0.04843(15) 0.0219(5) Uani 1 1 d . . . H28A H 0.3847 0.5424 0.0371 0.033 Uiso 1 1 calc R . . H28B H 0.3807 0.4362 -0.0026 0.033 Uiso 1 1 calc R . . H28C H 0.4283 0.4297 0.0880 0.033 Uiso 1 1 calc R . . O4 O 0.57383(15) 0.25566(14) 0.32513(10) 0.0180(3) Uani 1 1 d . . . C21 C 0.6962(2) 0.1658(2) 0.31199(15) 0.0210(5) Uani 1 1 d . . . H21 H 0.7093 0.1425 0.2532 0.025 Uiso 1 1 calc R . . C22 C 0.7042(3) 0.0695(2) 0.3664(2) 0.0307(6) Uani 1 1 d . . . H22A H 0.6943 0.0915 0.4241 0.046 Uiso 1 1 calc R . . H22B H 0.7864 0.0066 0.3561 0.046 Uiso 1 1 calc R . . H22C H 0.6369 0.0485 0.3541 0.046 Uiso 1 1 calc R . . C20 C 0.7967(2) 0.2023(2) 0.33279(19) 0.0281(6) Uani 1 1 d . . . H20A H 0.7936 0.2619 0.2957 0.042 Uiso 1 1 calc R . . H20B H 0.8801 0.1397 0.3265 0.042 Uiso 1 1 calc R . . H20C H 0.7814 0.2288 0.3896 0.042 Uiso 1 1 calc R . . O5 O 0.34705(16) 0.21590(15) 0.36037(11) 0.0218(4) Uani 1 1 d . . . C24 C 0.3099(3) 0.2293(2) 0.44646(16) 0.0261(5) Uani 1 1 d . . . H24 H 0.2323 0.3001 0.4548 0.031 Uiso 1 1 calc R . . C23 C 0.4130(3) 0.2323(3) 0.49699(17) 0.0339(7) Uani 1 1 d . . . H23A H 0.4840 0.1589 0.4973 0.051 Uiso 1 1 calc R . . H23B H 0.3795 0.2544 0.5534 0.051 Uiso 1 1 calc R . . H23C H 0.4419 0.2856 0.4729 0.051 Uiso 1 1 calc R . . C25 C 0.2787(3) 0.1344(3) 0.4733(2) 0.0376(7) Uani 1 1 d . . . H25A H 0.2133 0.1331 0.4395 0.056 Uiso 1 1 calc R . . H25B H 0.2480 0.1441 0.5310 0.056 Uiso 1 1 calc R . . H25C H 0.3547 0.0646 0.4667 0.056 Uiso 1 1 calc R . . O3 O 0.47486(19) 0.05283(15) 0.20919(12) 0.0260(4) Uani 1 1 d . . . C18 C 0.4776(3) -0.0197(2) 0.27515(18) 0.0283(6) Uani 1 1 d . . . H18 H 0.4852 0.0127 0.3278 0.034 Uiso 1 1 calc R . . C19 C 0.5928(3) -0.1282(3) 0.2592(2) 0.0416(8) Uani 1 1 d . . . H19A H 0.5883 -0.1574 0.2058 0.062 Uiso 1 1 calc R . . H19B H 0.5953 -0.1812 0.3023 0.062 Uiso 1 1 calc R . . H19C H 0.6692 -0.1161 0.2593 0.062 Uiso 1 1 calc R . . C17 C 0.3564(3) -0.0336(3) 0.2792(2) 0.0422(8) Uani 1 1 d . . . H17A H 0.2844 0.0387 0.2870 0.063 Uiso 1 1 calc R . . H17B H 0.3567 -0.0819 0.3252 0.063 Uiso 1 1 calc R . . H17C H 0.3497 -0.0664 0.2279 0.063 Uiso 1 1 calc R . . O1 O 0.27635(17) 0.26319(15) 0.12935(11) 0.0239(4) Uani 1 1 d . . . C12 C 0.2576(3) 0.2037(2) 0.06278(18) 0.0303(6) Uani 1 1 d . . . H12 H 0.3359 0.1339 0.0527 0.036 Uiso 1 1 calc R . . C11 C 0.1492(3) 0.1747(3) 0.0879(2) 0.0400(8) Uani 1 1 d . . . H11A H 0.1690 0.1293 0.1376 0.060 Uiso 1 1 calc R . . H11B H 0.1363 0.1334 0.0435 0.060 Uiso 1 1 calc R . . H11C H 0.0721 0.2426 0.0987 0.060 Uiso 1 1 calc R . . C13 C 0.2333(3) 0.2741(3) -0.01448(19) 0.0389(7) Uani 1 1 d . . . H13A H 0.1579 0.3437 -0.0047 0.058 Uiso 1 1 calc R . . H13B H 0.2202 0.2343 -0.0597 0.058 Uiso 1 1 calc R . . H13C H 0.3061 0.2898 -0.0288 0.058 Uiso 1 1 calc R . . O2 O 0.57864(17) 0.21529(15) 0.12506(11) 0.0221(4) Uani 1 1 d . . . C15 C 0.6531(3) 0.1658(2) 0.05223(17) 0.0280(6) Uani 1 1 d . . . H15 H 0.6574 0.2265 0.0173 0.034 Uiso 1 1 calc R . . C14 C 0.5983(3) 0.1063(3) 0.0025(2) 0.0396(8) Uani 1 1 d . . . H14A H 0.5849 0.0509 0.0368 0.059 Uiso 1 1 calc R . . H14B H 0.6568 0.0698 -0.0442 0.059 Uiso 1 1 calc R . . H14C H 0.5175 0.1593 -0.0176 0.059 Uiso 1 1 calc R . . C16 C 0.7857(3) 0.0915(3) 0.0748(2) 0.0424(8) Uani 1 1 d . . . H16A H 0.8174 0.1328 0.1081 0.064 Uiso 1 1 calc R . . H16B H 0.8402 0.0649 0.0248 0.064 Uiso 1 1 calc R . . H16C H 0.7855 0.0284 0.1064 0.064 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 0.01719(10) 0.01785(11) 0.01911(10) -0.00234(7) -0.00067(7) -0.00929(8) Mo2 0.01378(10) 0.01663(10) 0.01376(10) 0.00117(7) -0.00086(7) -0.00800(8) P 0.0138(3) 0.0171(3) 0.0113(2) 0.0006(2) -0.00083(19) -0.0072(2) N2 0.0167(9) 0.0191(10) 0.0149(9) -0.0021(7) 0.0012(7) -0.0069(8) Si3 0.0228(3) 0.0272(4) 0.0169(3) -0.0065(3) 0.0034(3) -0.0139(3) C7 0.0327(14) 0.0361(15) 0.0138(11) -0.0001(10) -0.0035(10) -0.0187(12) C8 0.0324(15) 0.0452(17) 0.0261(14) -0.0133(12) 0.0112(11) -0.0217(14) C9 0.0281(13) 0.0317(14) 0.0302(14) -0.0128(11) 0.0044(11) -0.0161(12) Si2 0.0180(3) 0.0182(3) 0.0299(4) 0.0021(3) 0.0001(3) -0.0051(3) C4 0.0262(14) 0.0206(13) 0.055(2) -0.0094(13) 0.0054(13) -0.0047(11) C5 0.0331(15) 0.0267(14) 0.0363(15) 0.0107(11) -0.0011(12) -0.0110(12) C6 0.0212(13) 0.0278(15) 0.0528(19) 0.0070(13) -0.0091(12) -0.0079(12) N3 0.0167(9) 0.0190(10) 0.0159(9) -0.0014(7) 0.0002(7) -0.0094(8) Si4 0.0145(3) 0.0239(3) 0.0183(3) -0.0007(2) -0.0002(2) -0.0105(3) C41 0.0193(12) 0.0332(14) 0.0273(13) 0.0005(11) -0.0060(10) -0.0124(11) C43 0.0228(12) 0.0286(14) 0.0368(15) 0.0012(11) -0.0012(11) -0.0162(11) C42 0.0203(12) 0.0367(15) 0.0281(13) -0.0033(11) 0.0042(10) -0.0150(11) N1 0.0137(8) 0.0166(9) 0.0127(8) 0.0014(7) -0.0018(7) -0.0059(7) Si1 0.0153(3) 0.0193(3) 0.0155(3) 0.0002(2) -0.0005(2) -0.0103(3) C1 0.0283(13) 0.0199(12) 0.0289(13) 0.0024(10) 0.0015(10) -0.0134(11) C2 0.0205(11) 0.0278(13) 0.0225(12) -0.0020(10) -0.0046(9) -0.0125(10) C3 0.0177(11) 0.0251(12) 0.0193(11) -0.0006(9) 0.0019(9) -0.0092(10) O6 0.0181(8) 0.0218(8) 0.0123(7) 0.0006(6) -0.0023(6) -0.0078(7) C27 0.0204(11) 0.0297(13) 0.0130(10) -0.0022(9) -0.0030(8) -0.0106(10) C26 0.0246(13) 0.0476(18) 0.0162(11) 0.0036(11) -0.0042(10) -0.0118(12) C28 0.0187(11) 0.0299(13) 0.0152(10) 0.0007(9) 0.0000(9) -0.0087(10) O4 0.0150(8) 0.0207(8) 0.0173(8) 0.0009(6) -0.0026(6) -0.0066(7) C21 0.0172(11) 0.0216(12) 0.0210(11) -0.0002(9) -0.0027(9) -0.0050(9) C22 0.0206(12) 0.0225(13) 0.0492(17) 0.0088(12) -0.0048(12) -0.0096(11) C20 0.0155(11) 0.0268(14) 0.0413(16) 0.0054(11) -0.0037(10) -0.0086(10) O5 0.0196(8) 0.0241(9) 0.0215(8) 0.0047(7) 0.0023(7) -0.0099(7) C24 0.0260(13) 0.0270(13) 0.0227(12) 0.0068(10) 0.0048(10) -0.0101(11) C23 0.0342(15) 0.0425(17) 0.0212(13) 0.0092(12) -0.0015(11) -0.0134(14) C25 0.0326(15) 0.0337(16) 0.0410(17) 0.0130(13) 0.0122(13) -0.0116(13) O3 0.0309(10) 0.0171(9) 0.0327(10) -0.0027(7) 0.0013(8) -0.0132(8) C18 0.0307(14) 0.0207(13) 0.0354(15) 0.0032(11) -0.0021(11) -0.0130(11) C19 0.0362(17) 0.0267(15) 0.051(2) 0.0044(14) 0.0016(14) -0.0039(13) C17 0.0376(17) 0.0383(18) 0.061(2) 0.0035(15) -0.0018(15) -0.0262(15) O1 0.0225(9) 0.0262(9) 0.0247(9) -0.0084(7) -0.0058(7) -0.0108(8) C12 0.0266(13) 0.0326(15) 0.0335(14) -0.0146(12) -0.0049(11) -0.0131(12) C11 0.0340(16) 0.0405(18) 0.0513(19) -0.0198(15) -0.0033(14) -0.0202(14) C13 0.0400(17) 0.0489(19) 0.0283(15) -0.0106(13) -0.0106(13) -0.0178(15) O2 0.0227(9) 0.0262(9) 0.0201(8) -0.0056(7) 0.0051(7) -0.0134(8) C15 0.0302(14) 0.0312(14) 0.0222(12) -0.0042(10) 0.0066(10) -0.0136(12) C14 0.0376(17) 0.051(2) 0.0324(15) -0.0212(14) 0.0083(13) -0.0212(15) C16 0.0312(16) 0.052(2) 0.0317(16) -0.0100(14) 0.0036(12) -0.0058(15) _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 O3 1.875(2) . ? Mo1 O2 1.9123(19) . ? Mo1 O1 1.9173(19) . ? Mo1 Mo2 2.2492(9) . ? Mo2 O4 1.9136(18) . ? Mo2 O5 1.9287(18) . ? Mo2 N1 2.202(2) . ? Mo2 N3 2.222(2) . ? Mo2 P 2.8727(14) . ? P O6 1.5960(18) . ? P N1 1.600(2) . ? P N3 1.609(2) . ? P N2 1.674(2) . ? N2 Si3 1.785(2) . ? N2 Si2 1.789(2) . ? Si3 C7 1.855(3) . ? Si3 C9 1.880(3) . ? Si3 C8 1.885(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? Si2 C6 1.861(3) . ? Si2 C5 1.872(3) . ? Si2 C4 1.882(3) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? N3 Si4 1.736(2) . ? Si4 C43 1.861(3) . ? Si4 C41 1.875(3) . ? Si4 C42 1.879(3) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? N1 Si1 1.741(2) . ? Si1 C3 1.866(3) . ? Si1 C2 1.869(3) . ? Si1 C1 1.871(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? O6 C27 1.466(3) . ? C27 C28 1.515(3) . ? C27 C26 1.530(4) . ? C27 H27 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? O4 C21 1.433(3) . ? C21 C20 1.520(4) . ? C21 C22 1.523(4) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? O5 C24 1.440(3) . ? C24 C25 1.517(4) . ? C24 C23 1.523(4) . ? C24 H24 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? O3 C18 1.426(3) . ? C18 C17 1.512(4) . ? C18 C19 1.517(4) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? O1 C12 1.447(3) . ? C12 C11 1.517(4) . ? C12 C13 1.523(5) . ? C12 H12 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? O2 C15 1.427(3) . ? C15 C14 1.502(4) . ? C15 C16 1.508(4) . ? C15 H15 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Mo1 O2 113.80(9) . . ? O3 Mo1 O1 109.82(9) . . ? O2 Mo1 O1 120.54(9) . . ? O3 Mo1 Mo2 108.87(7) . . ? O2 Mo1 Mo2 99.07(6) . . ? O1 Mo1 Mo2 102.94(6) . . ? O4 Mo2 O5 100.69(8) . . ? O4 Mo2 N1 88.49(8) . . ? O5 Mo2 N1 152.33(7) . . ? O4 Mo2 N3 149.14(7) . . ? O5 Mo2 N3 93.57(8) . . ? N1 Mo2 N3 67.45(8) . . ? O4 Mo2 Mo1 103.24(6) . . ? O5 Mo2 Mo1 95.72(6) . . ? N1 Mo2 Mo1 107.61(5) . . ? N3 Mo2 Mo1 102.37(6) . . ? O4 Mo2 P 119.91(6) . . ? O5 Mo2 P 124.91(6) . . ? N1 Mo2 P 33.57(5) . . ? N3 Mo2 P 33.87(6) . . ? Mo1 Mo2 P 108.03(3) . . ? O6 P N1 114.37(10) . . ? O6 P N3 113.21(10) . . ? N1 P N3 99.87(11) . . ? O6 P N2 96.15(10) . . ? N1 P N2 115.93(11) . . ? N3 P N2 118.27(11) . . ? O6 P Mo2 128.66(7) . . ? N1 P Mo2 49.55(8) . . ? N3 P Mo2 50.32(8) . . ? N2 P Mo2 135.18(8) . . ? P N2 Si3 120.21(12) . . ? P N2 Si2 121.34(12) . . ? Si3 N2 Si2 118.35(12) . . ? N2 Si3 C7 111.11(11) . . ? N2 Si3 C9 110.93(12) . . ? C7 Si3 C9 107.81(14) . . ? N2 Si3 C8 111.33(13) . . ? C7 Si3 C8 106.37(14) . . ? C9 Si3 C8 109.12(13) . . ? Si3 C7 H7A 109.5 . . ? Si3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si3 C8 H8A 109.5 . . ? Si3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si3 C9 H9A 109.5 . . ? Si3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 Si2 C6 111.16(13) . . ? N2 Si2 C5 117.97(12) . . ? C6 Si2 C5 108.32(15) . . ? N2 Si2 C4 109.81(13) . . ? C6 Si2 C4 106.84(15) . . ? C5 Si2 C4 101.87(15) . . ? Si2 C4 H4A 109.5 . . ? Si2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? P N3 Si4 131.53(13) . . ? P N3 Mo2 95.81(10) . . ? Si4 N3 Mo2 132.37(11) . . ? N3 Si4 C43 111.72(12) . . ? N3 Si4 C41 113.32(12) . . ? C43 Si4 C41 106.89(13) . . ? N3 Si4 C42 110.77(11) . . ? C43 Si4 C42 107.01(13) . . ? C41 Si4 C42 106.79(13) . . ? Si4 C41 H41A 109.5 . . ? Si4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? Si4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? Si4 C43 H43A 109.5 . . ? Si4 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? Si4 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? Si4 C42 H42A 109.5 . . ? Si4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? Si4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? P N1 Si1 133.43(13) . . ? P N1 Mo2 96.87(10) . . ? Si1 N1 Mo2 129.17(10) . . ? N1 Si1 C3 111.09(11) . . ? N1 Si1 C2 111.35(11) . . ? C3 Si1 C2 108.87(12) . . ? N1 Si1 C1 111.94(12) . . ? C3 Si1 C1 106.58(12) . . ? C2 Si1 C1 106.79(13) . . ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C27 O6 P 123.86(15) . . ? O6 C27 C28 110.1(2) . . ? O6 C27 C26 105.3(2) . . ? C28 C27 C26 111.5(2) . . ? O6 C27 H27 110.0 . . ? C28 C27 H27 110.0 . . ? C26 C27 H27 110.0 . . ? C27 C26 H26A 109.5 . . ? C27 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C27 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C21 O4 Mo2 138.48(15) . . ? O4 C21 C20 109.6(2) . . ? O4 C21 C22 109.0(2) . . ? C20 C21 C22 110.0(2) . . ? O4 C21 H21 109.4 . . ? C20 C21 H21 109.4 . . ? C22 C21 H21 109.4 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C20 H20A 109.5 . . ? C21 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C21 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C24 O5 Mo2 129.83(17) . . ? O5 C24 C25 107.9(2) . . ? O5 C24 C23 111.7(2) . . ? C25 C24 C23 110.7(2) . . ? O5 C24 H24 108.8 . . ? C25 C24 H24 108.8 . . ? C23 C24 H24 108.8 . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C24 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C18 O3 Mo1 146.85(17) . . ? O3 C18 C17 108.9(2) . . ? O3 C18 C19 107.4(2) . . ? C17 C18 C19 112.1(3) . . ? O3 C18 H18 109.4 . . ? C17 C18 H18 109.4 . . ? C19 C18 H18 109.4 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C18 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C12 O1 Mo1 116.91(16) . . ? O1 C12 C11 108.7(2) . . ? O1 C12 C13 109.2(2) . . ? C11 C12 C13 112.4(3) . . ? O1 C12 H12 108.8 . . ? C11 C12 H12 108.8 . . ? C13 C12 H12 108.8 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 O2 Mo1 129.97(17) . . ? O2 C15 C14 113.6(2) . . ? O2 C15 C16 108.9(2) . . ? C14 C15 C16 111.9(3) . . ? O2 C15 H15 107.4 . . ? C14 C15 H15 107.4 . . ? C16 C15 H15 107.4 . . ? C15 C14 H14A 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C15 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 2.810 _refine_diff_density_min -0.725 _refine_diff_density_rms 0.121