#Supplementary Material for Dalton Transactions #This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Kovalenko, Oleksandr' 'Boldog, Ishtvan' 'Kinzhybalo, Vasyl' 'Lis, Tadeusz' 'Brusilovets, Anatolii' _publ_contact_author_name 'Kovalenko, Oleksandr' _publ_contact_author_email kovalenko.chem@gmail.com _publ_section_title ; Reactions of trialkoxynitridomolybdenum with low coordinated phosphorus compounds containing a P=N double bond ; # Attachment '- ANAT.cif' #===================================================================== data_5ab _database_code_depnum_ccdc_archive 'CCDC 781902' #TrackingRef '- ANAT.cif' #===================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H54 Mo N3 O3 P Si3' _chemical_formula_sum 'C21 H54 Mo N3 O3 P Si3' _chemical_formula_weight 607.85 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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.865(3) _cell_length_b 17.714(5) _cell_length_c 20.325(6) _cell_angle_alpha 70.65(3) _cell_angle_beta 77.37(3) _cell_angle_gamma 88.48(3) _cell_volume 3266.0(17) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 30428 _cell_measurement_theta_min 4 _cell_measurement_theta_max 33 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.236 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 0.584 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.897 _exptl_absorpt_correction_T_max 0.917 _exptl_absorpt_process_details 'CrysAlis RED; Oxford-Diffraction Poland, 2003' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Xcalibur PX kappa-geometry diffractometer with Onyx CCD camera' _diffrn_measurement_method 'omega and phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 78806 _diffrn_reflns_av_R_equivalents 0.0763 _diffrn_reflns_av_sigmaI/netI 0.1019 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 4.16 _diffrn_reflns_theta_max 32.59 _reflns_number_total 23295 _reflns_number_gt 12600 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD; Oxford-Diffraction Poland, 2003' _computing_cell_refinement 'CrysAlis RED; Oxford-Diffraction Poland, 2003' _computing_data_reduction 'CrysAlis RED; Oxford-Diffraction Poland, 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^)+(0.02P)^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 23295 _refine_ls_number_parameters 623 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1086 _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_ref 0.0792 _refine_ls_wR_factor_gt 0.0703 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1A Mo 0.96390(2) 0.569930(12) 0.336392(11) 0.01838(6) Uani 0.9658(7) 1 d P . . Mo1B Mo 0.9964(7) 0.5406(4) 0.2930(4) 0.031(2) Uiso 0.0342(7) 1 d P . . P1 P 0.85484(6) 0.69165(3) 0.21336(3) 0.01869(13) Uani 1 1 d . . . Si1 Si 0.82063(6) 0.73738(4) 0.34660(3) 0.02383(15) Uani 1 1 d . . . Si2 Si 1.14238(7) 0.78052(4) 0.14234(4) 0.02446(15) Uani 1 1 d . . . Si3 Si 0.87320(7) 0.83769(4) 0.08970(4) 0.02740(16) Uani 1 1 d . . . O1 O 0.84283(15) 0.48270(9) 0.35130(8) 0.0252(4) Uani 1 1 d . . . O2 O 1.14907(15) 0.55357(9) 0.30005(8) 0.0259(4) Uani 1 1 d . . . O3 O 0.93630(14) 0.60952(8) 0.20697(8) 0.0195(3) Uani 1 1 d . . . N1 N 0.95948(18) 0.57070(11) 0.41781(10) 0.0251(5) Uani 1 1 d . . . N2 N 0.89777(17) 0.67887(10) 0.29364(9) 0.0180(4) Uani 1 1 d . . . N3 N 0.96042(17) 0.76890(10) 0.15015(10) 0.0199(4) Uani 1 1 d . . . C11 C 0.7651(2) 0.41921(13) 0.41270(12) 0.0244(5) Uani 1 1 d . . . C12 C 0.8630(2) 0.37581(14) 0.45986(13) 0.0323(6) Uani 1 1 d . . . H12A H 0.9392 0.3554 0.4316 0.048 Uiso 1 1 calc R . . H12B H 0.8117 0.3310 0.4999 0.048 Uiso 1 1 calc R . . H12C H 0.9010 0.4131 0.4784 0.048 Uiso 1 1 calc R . . C13 C 0.6496(2) 0.45539(16) 0.45334(14) 0.0394(7) Uani 1 1 d . . . H13A H 0.6899 0.4901 0.4737 0.059 Uiso 1 1 calc R . . H13B H 0.5906 0.4125 0.4920 0.059 Uiso 1 1 calc R . . H13C H 0.5933 0.4870 0.4207 0.059 Uiso 1 1 calc R . . C14 C 0.7061(3) 0.36317(15) 0.38199(15) 0.0463(8) Uani 1 1 d . . . H14A H 0.6493 0.3932 0.3489 0.069 Uiso 1 1 calc R . . H14B H 0.6484 0.3200 0.4210 0.069 Uiso 1 1 calc R . . H14C H 0.7826 0.3402 0.3563 0.069 Uiso 1 1 calc R . . C21 C 1.2739(2) 0.53370(15) 0.32846(14) 0.0292(6) Uani 1 1 d . . . C22 C 1.3258(3) 0.60808(16) 0.33877(17) 0.0491(8) Uani 1 1 d . . . H22A H 1.3495 0.6512 0.2925 0.074 Uiso 1 1 calc R . . H22B H 1.4084 0.5960 0.3591 0.074 Uiso 1 1 calc R . . H22C H 1.2527 0.6250 0.3714 0.074 Uiso 1 1 calc R . . C23 C 1.3759(3) 0.50927(19) 0.27232(15) 0.0483(8) Uani 1 1 d . . . H23A H 1.3360 0.4631 0.2655 0.072 Uiso 1 1 calc R . . H23B H 1.4629 0.4949 0.2882 0.072 Uiso 1 1 calc R . . H23C H 1.3948 0.5541 0.2270 0.072 Uiso 1 1 calc R . . C24 C 1.2407(2) 0.46458(15) 0.39892(13) 0.0329(6) Uani 1 1 d . . . H24A H 1.1720 0.4806 0.4340 0.049 Uiso 1 1 calc R . . H24B H 1.3258 0.4504 0.4167 0.049 Uiso 1 1 calc R . . H24C H 1.2029 0.4182 0.3915 0.049 Uiso 1 1 calc R . . C31 C 0.9373(2) 0.75655(15) 0.40010(13) 0.0333(6) Uani 1 1 d . . . H31A H 0.9614 0.7054 0.4318 0.050 Uiso 1 1 calc R . . H31B H 0.8898 0.7883 0.4289 0.050 Uiso 1 1 calc R . . H31C H 1.0222 0.7861 0.3680 0.050 Uiso 1 1 calc R . . C32 C 0.6574(2) 0.68559(14) 0.40824(13) 0.0318(6) Uani 1 1 d . . . H32A H 0.5944 0.6756 0.3805 0.048 Uiso 1 1 calc R . . H32B H 0.6129 0.7193 0.4357 0.048 Uiso 1 1 calc R . . H32C H 0.6788 0.6345 0.4411 0.048 Uiso 1 1 calc R . . C33 C 0.7778(3) 0.83595(14) 0.28684(13) 0.0348(6) Uani 1 1 d . . . H33A H 0.8633 0.8643 0.2543 0.052 Uiso 1 1 calc R . . H33B H 0.7335 0.8681 0.3159 0.052 Uiso 1 1 calc R . . H33C H 0.7140 0.8272 0.2590 0.052 Uiso 1 1 calc R . . C41 C 1.2379(2) 0.69395(16) 0.12777(15) 0.0385(7) Uani 1 1 d . . . H41A H 1.1998 0.6449 0.1670 0.058 Uiso 1 1 calc R . . H41B H 1.3366 0.7020 0.1262 0.058 Uiso 1 1 calc R . . H41C H 1.2278 0.6892 0.0824 0.058 Uiso 1 1 calc R . . C42 C 1.1810(2) 0.79780(15) 0.22169(13) 0.0310(6) Uani 1 1 d . . . H42A H 1.1252 0.8410 0.2316 0.046 Uiso 1 1 calc R . . H42B H 1.2800 0.8129 0.2122 0.046 Uiso 1 1 calc R . . H42C H 1.1581 0.7486 0.2631 0.046 Uiso 1 1 calc R . . C43 C 1.2240(3) 0.86936(16) 0.06444(14) 0.0411(7) Uani 1 1 d . . . H43A H 1.2114 0.8627 0.0201 0.062 Uiso 1 1 calc R . . H43B H 1.3235 0.8740 0.0628 0.062 Uiso 1 1 calc R . . H43C H 1.1798 0.9179 0.0696 0.062 Uiso 1 1 calc R . . C51 C 0.6835(2) 0.81004(16) 0.11045(15) 0.0374(6) Uani 1 1 d . . . H51A H 0.6709 0.7565 0.1078 0.056 Uiso 1 1 calc R . . H51B H 0.6394 0.8490 0.0757 0.056 Uiso 1 1 calc R . . H51C H 0.6407 0.8101 0.1587 0.056 Uiso 1 1 calc R . . C52 C 0.8875(3) 0.94077(14) 0.09359(15) 0.0392(7) Uani 1 1 d . . . H52A H 0.8434 0.9408 0.1417 0.059 Uiso 1 1 calc R . . H52B H 0.8408 0.9776 0.0587 0.059 Uiso 1 1 calc R . . H52C H 0.9859 0.9581 0.0824 0.059 Uiso 1 1 calc R . . C53 C 0.9418(3) 0.84042(16) -0.00445(14) 0.0381(7) Uani 1 1 d . . . H53A H 1.0349 0.8670 -0.0224 0.057 Uiso 1 1 calc R . . H53B H 0.8796 0.8702 -0.0345 0.057 Uiso 1 1 calc R . . H53C H 0.9468 0.7856 -0.0058 0.057 Uiso 1 1 calc R . . C61 C 0.8957(2) 0.56296(13) 0.16461(13) 0.0242(5) Uani 1 1 d . . . C62 C 0.7415(2) 0.53815(14) 0.19187(14) 0.0312(6) Uani 1 1 d . . . H62A H 0.7224 0.5090 0.2434 0.047 Uiso 1 1 calc R . . H62B H 0.7161 0.5035 0.1671 0.047 Uiso 1 1 calc R . . H62C H 0.6867 0.5860 0.1826 0.047 Uiso 1 1 calc R . . C63 C 0.9295(3) 0.61147(16) 0.08682(14) 0.0361(6) Uani 1 1 d . . . H63A H 0.8740 0.6590 0.0786 0.054 Uiso 1 1 calc R . . H63B H 0.9080 0.5791 0.0592 0.054 Uiso 1 1 calc R . . H63C H 1.0286 0.6280 0.0716 0.054 Uiso 1 1 calc R . . C64 C 0.9835(3) 0.48971(15) 0.18164(16) 0.0398(7) Uani 1 1 d . . . H64A H 1.0822 0.5071 0.1682 0.060 Uiso 1 1 calc R . . H64B H 0.9671 0.4554 0.1547 0.060 Uiso 1 1 calc R . . H64C H 0.9578 0.4596 0.2330 0.060 Uiso 1 1 calc R . . Mo2A Mo 0.47905(2) 0.070808(12) 0.330874(11) 0.01846(7) Uani 0.9652(8) 1 d P . . Mo2B Mo 0.5210(7) 0.0548(4) 0.2853(4) 0.038(2) Uiso 0.0348(8) 1 d P . . P2 P 0.34382(6) 0.18338(4) 0.21084(3) 0.01943(13) Uani 1 1 d . . . Si12 Si 0.26817(7) 0.21068(4) 0.35311(4) 0.02401(15) Uani 1 1 d . . . Si22 Si 0.61181(7) 0.29359(4) 0.14604(4) 0.02487(15) Uani 1 1 d . . . Si32 Si 0.33981(7) 0.33454(4) 0.09392(4) 0.02736(16) Uani 1 1 d . . . O12 O 0.40178(15) -0.02819(9) 0.33800(8) 0.0252(4) Uani 1 1 d . . . O22 O 0.67261(15) 0.07885(10) 0.29704(9) 0.0280(4) Uani 1 1 d . . . O32 O 0.44770(14) 0.11037(9) 0.19996(8) 0.0204(3) Uani 1 1 d . . . N12 N 0.45767(18) 0.06804(11) 0.41473(10) 0.0246(4) Uani 1 1 d . . . N22 N 0.37644(17) 0.16925(11) 0.29352(10) 0.0194(4) Uani 1 1 d . . . N32 N 0.43524(18) 0.26900(11) 0.15209(10) 0.0208(4) Uani 1 1 d . . . C15 C 0.3458(2) -0.10182(13) 0.39454(12) 0.0250(5) Uani 1 1 d . . . C16 C 0.4366(3) -0.12623(14) 0.44851(13) 0.0352(6) Uani 1 1 d . . . H16A H 0.4393 -0.0843 0.4698 0.053 Uiso 1 1 calc R . . H16B H 0.5311 -0.1337 0.4246 0.053 Uiso 1 1 calc R . . H16C H 0.3984 -0.1765 0.4861 0.053 Uiso 1 1 calc R . . C17 C 0.1990(3) -0.08869(16) 0.42925(15) 0.0429(7) Uani 1 1 d . . . H17A H 0.1439 -0.0701 0.3927 0.064 Uiso 1 1 calc R . . H17B H 0.2013 -0.0483 0.4523 0.064 Uiso 1 1 calc R . . H17C H 0.1567 -0.1392 0.4652 0.064 Uiso 1 1 calc R . . C18 C 0.3466(3) -0.16406(14) 0.35775(14) 0.0341(6) Uani 1 1 d . . . H18A H 0.4420 -0.1691 0.3334 0.051 Uiso 1 1 calc R . . H18B H 0.2880 -0.1473 0.3227 0.051 Uiso 1 1 calc R . . H18C H 0.3103 -0.2159 0.3935 0.051 Uiso 1 1 calc R . . C25 C 0.7926(2) 0.07928(14) 0.32836(13) 0.0261(5) Uani 1 1 d . . . C26 C 0.7949(3) 0.15508(15) 0.34734(16) 0.0415(7) Uani 1 1 d . . . H26A H 0.7078 0.1571 0.3807 0.062 Uiso 1 1 calc R . . H26B H 0.8053 0.2019 0.3038 0.062 Uiso 1 1 calc R . . H26C H 0.8733 0.1552 0.3697 0.062 Uiso 1 1 calc R . . C27 C 0.9190(2) 0.07733(18) 0.27098(15) 0.0458(7) Uani 1 1 d . . . H27A H 0.9229 0.1247 0.2284 0.069 Uiso 1 1 calc R . . H27B H 0.9123 0.0288 0.2585 0.069 Uiso 1 1 calc R . . H27C H 1.0035 0.0772 0.2890 0.069 Uiso 1 1 calc R . . C28 C 0.7817(2) 0.00529(15) 0.39406(14) 0.0346(6) Uani 1 1 d . . . H28A H 0.7744 -0.0427 0.3809 0.052 Uiso 1 1 calc R . . H28B H 0.6990 0.0071 0.4303 0.052 Uiso 1 1 calc R . . H28C H 0.8648 0.0036 0.4135 0.052 Uiso 1 1 calc R . . C34 C 0.3721(2) 0.25339(15) 0.39927(14) 0.0330(6) Uani 1 1 d . . . H34A H 0.4287 0.3001 0.3645 0.049 Uiso 1 1 calc R . . H34B H 0.4330 0.2129 0.4215 0.049 Uiso 1 1 calc R . . H34C H 0.3095 0.2697 0.4362 0.049 Uiso 1 1 calc R . . C35 C 0.1410(2) 0.13330(15) 0.42180(13) 0.0335(6) Uani 1 1 d . . . H35A H 0.1891 0.0969 0.4562 0.050 Uiso 1 1 calc R . . H35B H 0.0982 0.1029 0.3985 0.050 Uiso 1 1 calc R . . H35C H 0.0688 0.1594 0.4468 0.050 Uiso 1 1 calc R . . C36 C 0.1667(3) 0.29102(15) 0.30263(13) 0.0349(6) Uani 1 1 d . . . H36A H 0.1050 0.2676 0.2819 0.052 Uiso 1 1 calc R . . H36B H 0.2308 0.3315 0.2642 0.052 Uiso 1 1 calc R . . H36C H 0.1110 0.3161 0.3352 0.052 Uiso 1 1 calc R . . C44 C 0.7285(2) 0.21466(15) 0.13139(14) 0.0354(6) Uani 1 1 d . . . H44A H 0.7220 0.2067 0.0867 0.053 Uiso 1 1 calc R . . H44B H 0.7009 0.1645 0.1713 0.053 Uiso 1 1 calc R . . H44C H 0.8245 0.2309 0.1284 0.053 Uiso 1 1 calc R . . C45 C 0.6275(2) 0.31740(15) 0.22680(13) 0.0325(6) Uani 1 1 d . . . H45A H 0.6015 0.2695 0.2693 0.049 Uiso 1 1 calc R . . H45B H 0.5655 0.3602 0.2321 0.049 Uiso 1 1 calc R . . H45C H 0.7237 0.3351 0.2216 0.049 Uiso 1 1 calc R . . C46 C 0.6842(3) 0.38483(15) 0.06796(14) 0.0392(7) Uani 1 1 d . . . H46A H 0.6307 0.4310 0.0723 0.059 Uiso 1 1 calc R . . H46B H 0.6779 0.3761 0.0235 0.059 Uiso 1 1 calc R . . H46C H 0.7817 0.3951 0.0671 0.059 Uiso 1 1 calc R . . C54 C 0.1534(2) 0.29932(16) 0.11403(14) 0.0347(6) Uani 1 1 d . . . H54A H 0.1073 0.2989 0.1621 0.052 Uiso 1 1 calc R . . H54B H 0.1484 0.2451 0.1118 0.052 Uiso 1 1 calc R . . H54C H 0.1067 0.3356 0.0788 0.052 Uiso 1 1 calc R . . C55 C 0.3390(3) 0.43624(15) 0.10221(16) 0.0419(7) Uani 1 1 d . . . H55A H 0.4336 0.4608 0.0849 0.063 Uiso 1 1 calc R . . H55B H 0.3053 0.4318 0.1525 0.063 Uiso 1 1 calc R . . H55C H 0.2776 0.4696 0.0737 0.063 Uiso 1 1 calc R . . C56 C 0.4124(3) 0.34369(16) -0.00176(13) 0.0380(7) Uani 1 1 d . . . H56A H 0.4081 0.2909 -0.0072 0.057 Uiso 1 1 calc R . . H56B H 0.5094 0.3643 -0.0159 0.057 Uiso 1 1 calc R . . H56C H 0.3578 0.3806 -0.0322 0.057 Uiso 1 1 calc R . . C65 C 0.4215(2) 0.06448(14) 0.15421(14) 0.0260(6) Uani 1 1 d . . . C66 C 0.2791(3) 0.02060(15) 0.18657(14) 0.0353(6) Uani 1 1 d . . . H66A H 0.2068 0.0598 0.1857 0.053 Uiso 1 1 calc R . . H66B H 0.2754 -0.0133 0.2361 0.053 Uiso 1 1 calc R . . H66C H 0.2635 -0.0128 0.1587 0.053 Uiso 1 1 calc R . . C67 C 0.4315(3) 0.11884(15) 0.07972(14) 0.0346(6) Uani 1 1 d . . . H67A H 0.5208 0.1497 0.0624 0.052 Uiso 1 1 calc R . . H67B H 0.3554 0.1556 0.0786 0.052 Uiso 1 1 calc R . . H67C H 0.4250 0.0871 0.0490 0.052 Uiso 1 1 calc R . . C68 C 0.5382(3) 0.00536(16) 0.15941(15) 0.0411(7) Uani 1 1 d . . . H68A H 0.5326 -0.0264 0.2097 0.062 Uiso 1 1 calc R . . H68B H 0.6285 0.0350 0.1392 0.062 Uiso 1 1 calc R . . H68C H 0.5279 -0.0304 0.1327 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 Mo1A 0.01910(11) 0.01836(11) 0.01898(12) -0.00674(9) -0.00569(8) -0.00264(8) P1 0.0197(3) 0.0184(3) 0.0186(3) -0.0065(3) -0.0047(2) -0.0018(2) Si1 0.0264(3) 0.0241(3) 0.0217(3) -0.0099(3) -0.0028(3) -0.0029(3) Si2 0.0250(3) 0.0261(4) 0.0213(4) -0.0076(3) -0.0025(3) -0.0084(3) Si3 0.0346(4) 0.0230(4) 0.0221(4) -0.0039(3) -0.0069(3) 0.0021(3) O1 0.0266(8) 0.0228(9) 0.0247(9) -0.0036(7) -0.0086(7) -0.0057(7) O2 0.0196(8) 0.0349(10) 0.0245(9) -0.0109(8) -0.0066(7) 0.0029(7) O3 0.0219(8) 0.0174(8) 0.0215(9) -0.0090(7) -0.0056(6) -0.0020(6) N1 0.0251(10) 0.0260(11) 0.0255(12) -0.0088(9) -0.0075(8) -0.0039(8) N2 0.0205(9) 0.0178(9) 0.0168(10) -0.0073(8) -0.0035(7) -0.0025(7) N3 0.0233(9) 0.0180(10) 0.0178(10) -0.0056(8) -0.0033(8) 0.0001(8) C11 0.0282(12) 0.0188(12) 0.0233(13) -0.0009(10) -0.0078(10) -0.0091(10) C12 0.0351(14) 0.0264(13) 0.0310(15) -0.0022(11) -0.0092(11) -0.0056(11) C13 0.0287(13) 0.0390(16) 0.0411(17) -0.0062(13) 0.0011(12) -0.0069(12) C14 0.0657(19) 0.0324(15) 0.0410(17) -0.0026(13) -0.0245(14) -0.0227(14) C21 0.0194(11) 0.0348(14) 0.0373(15) -0.0142(12) -0.0111(10) 0.0029(10) C22 0.0482(17) 0.0365(17) 0.065(2) -0.0066(15) -0.0317(15) -0.0093(13) C23 0.0282(14) 0.070(2) 0.0437(18) -0.0193(16) -0.0039(13) 0.0129(14) C24 0.0285(13) 0.0366(15) 0.0345(15) -0.0101(12) -0.0122(11) 0.0047(11) C31 0.0368(14) 0.0377(15) 0.0328(15) -0.0208(13) -0.0082(11) -0.0030(12) C32 0.0334(13) 0.0293(14) 0.0321(15) -0.0119(12) -0.0030(11) -0.0035(11) C33 0.0454(15) 0.0286(14) 0.0291(14) -0.0133(12) 0.0005(12) -0.0018(12) C41 0.0229(13) 0.0479(17) 0.0474(18) -0.0221(15) -0.0025(12) -0.0057(11) C42 0.0299(13) 0.0345(15) 0.0281(14) -0.0102(12) -0.0043(11) -0.0118(11) C43 0.0367(15) 0.0449(17) 0.0312(16) -0.0009(13) -0.0027(12) -0.0135(13) C51 0.0377(15) 0.0386(16) 0.0364(17) -0.0075(13) -0.0177(12) 0.0067(12) C52 0.0466(16) 0.0243(14) 0.0389(17) -0.0059(12) -0.0012(13) 0.0039(12) C53 0.0475(16) 0.0398(16) 0.0267(15) -0.0092(13) -0.0107(12) 0.0043(13) C61 0.0273(12) 0.0199(12) 0.0317(14) -0.0153(11) -0.0089(10) -0.0010(9) C62 0.0362(14) 0.0258(13) 0.0351(15) -0.0114(12) -0.0123(11) -0.0063(11) C63 0.0405(15) 0.0392(16) 0.0356(16) -0.0205(14) -0.0095(12) -0.0068(12) C64 0.0478(16) 0.0355(16) 0.0484(18) -0.0274(14) -0.0158(14) 0.0072(13) Mo2A 0.01844(11) 0.01936(12) 0.01903(13) -0.00718(9) -0.00548(8) -0.00269(8) P2 0.0196(3) 0.0209(3) 0.0191(3) -0.0075(3) -0.0052(2) -0.0011(2) Si12 0.0248(3) 0.0274(4) 0.0221(3) -0.0113(3) -0.0050(3) 0.0007(3) Si22 0.0266(3) 0.0243(4) 0.0223(4) -0.0052(3) -0.0055(3) -0.0076(3) Si32 0.0311(4) 0.0273(4) 0.0217(4) -0.0049(3) -0.0070(3) 0.0030(3) O12 0.0298(9) 0.0211(8) 0.0240(9) -0.0036(7) -0.0095(7) -0.0075(7) O22 0.0196(8) 0.0370(10) 0.0270(10) -0.0085(8) -0.0080(7) 0.0011(7) O32 0.0220(8) 0.0217(9) 0.0213(9) -0.0102(7) -0.0075(6) -0.0002(6) N12 0.0261(10) 0.0257(11) 0.0253(12) -0.0101(9) -0.0096(8) 0.0011(8) N22 0.0213(9) 0.0205(10) 0.0176(10) -0.0072(8) -0.0054(7) -0.0004(7) N32 0.0228(9) 0.0208(10) 0.0196(10) -0.0066(9) -0.0063(8) -0.0006(8) C15 0.0274(12) 0.0200(12) 0.0245(13) -0.0041(10) -0.0037(10) -0.0098(9) C16 0.0533(17) 0.0236(13) 0.0280(14) -0.0028(11) -0.0155(12) -0.0096(12) C17 0.0379(15) 0.0322(15) 0.0486(19) -0.0074(14) 0.0020(13) -0.0069(12) C18 0.0440(15) 0.0256(13) 0.0328(15) -0.0082(11) -0.0100(12) -0.0082(11) C25 0.0185(11) 0.0306(14) 0.0296(14) -0.0076(11) -0.0096(10) -0.0006(10) C26 0.0331(14) 0.0329(15) 0.066(2) -0.0169(15) -0.0252(14) 0.0008(12) C27 0.0225(13) 0.067(2) 0.0429(18) -0.0137(16) -0.0045(12) 0.0007(13) C28 0.0260(13) 0.0389(16) 0.0397(16) -0.0118(13) -0.0106(11) 0.0015(11) C34 0.0352(14) 0.0344(15) 0.0365(15) -0.0200(13) -0.0100(11) 0.0025(11) C35 0.0254(13) 0.0426(16) 0.0290(14) -0.0090(12) -0.0035(10) 0.0017(11) C36 0.0405(15) 0.0363(15) 0.0287(14) -0.0144(12) -0.0047(11) 0.0065(12) C44 0.0239(13) 0.0423(16) 0.0386(16) -0.0139(13) -0.0024(11) -0.0033(11) C45 0.0354(14) 0.0343(15) 0.0291(14) -0.0095(12) -0.0096(11) -0.0118(11) C46 0.0380(15) 0.0397(16) 0.0337(16) -0.0039(13) -0.0064(12) -0.0139(12) C54 0.0325(14) 0.0441(17) 0.0267(15) -0.0074(13) -0.0122(11) 0.0050(12) C55 0.0443(16) 0.0318(15) 0.0433(18) -0.0074(14) -0.0055(13) 0.0057(12) C56 0.0437(16) 0.0461(17) 0.0220(15) -0.0064(13) -0.0106(12) 0.0032(13) C65 0.0259(12) 0.0250(13) 0.0353(15) -0.0216(12) -0.0054(10) -0.0001(10) C66 0.0484(16) 0.0279(14) 0.0348(16) -0.0135(12) -0.0139(12) -0.0079(12) C67 0.0445(15) 0.0375(16) 0.0271(15) -0.0179(13) -0.0075(12) 0.0008(12) C68 0.0524(17) 0.0368(16) 0.0451(18) -0.0245(14) -0.0176(14) 0.0129(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1A N1 1.650(2) . ? Mo1A O2 1.8681(16) . ? Mo1A O1 1.8803(16) . ? Mo1A N2 1.9936(19) . ? Mo1A O3 2.5624(17) . ? P1 O3 1.6724(16) . ? P1 N3 1.713(2) . ? P1 N2 1.7163(19) . ? Si1 N2 1.7753(18) . ? Si1 C31 1.853(2) . ? Si1 C32 1.854(2) . ? Si1 C33 1.866(3) . ? Si2 N3 1.7785(19) . ? Si2 C41 1.852(3) . ? Si2 C42 1.855(2) . ? Si2 C43 1.868(3) . ? Si3 N3 1.775(2) . ? Si3 C52 1.864(2) . ? Si3 C51 1.867(3) . ? Si3 C53 1.870(3) . ? O1 C11 1.452(3) . ? O2 C21 1.459(3) . ? O3 C61 1.490(2) . ? C11 C13 1.514(3) . ? C11 C14 1.521(3) . ? C11 C12 1.523(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C21 C23 1.518(3) . ? C21 C22 1.519(3) . ? C21 C24 1.521(3) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C61 C63 1.495(3) . ? C61 C62 1.523(3) . ? C61 C64 1.526(3) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? Mo2A N12 1.655(2) . ? Mo2A O22 1.8746(16) . ? Mo2A O12 1.8792(15) . ? Mo2A N22 2.0018(19) . ? Mo2A O32 2.6038(17) . ? P2 O32 1.6708(16) . ? P2 N32 1.715(2) . ? P2 N22 1.716(2) . ? Si12 N22 1.7686(19) . ? Si12 C34 1.854(2) . ? Si12 C35 1.860(3) . ? Si12 C36 1.867(3) . ? Si22 N32 1.7748(19) . ? Si22 C44 1.847(3) . ? Si22 C45 1.863(2) . ? Si22 C46 1.872(3) . ? Si32 N32 1.775(2) . ? Si32 C55 1.864(3) . ? Si32 C54 1.872(2) . ? Si32 C56 1.873(3) . ? O12 C15 1.447(3) . ? O22 C25 1.462(3) . ? O32 C65 1.486(2) . ? C15 C16 1.513(3) . ? C15 C17 1.514(3) . ? C15 C18 1.522(3) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C25 C28 1.516(3) . ? C25 C26 1.517(3) . ? C25 C27 1.519(3) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C65 C67 1.484(3) . ? C65 C66 1.525(3) . ? C65 C68 1.532(3) . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 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 N1 Mo1A O2 105.02(8) . . ? N1 Mo1A O1 103.94(8) . . ? O2 Mo1A O1 112.79(7) . . ? N1 Mo1A N2 99.78(9) . . ? O2 Mo1A N2 116.15(8) . . ? O1 Mo1A N2 116.59(7) . . ? N1 Mo1A O3 162.49(7) . . ? O2 Mo1A O3 85.78(7) . . ? O1 Mo1A O3 83.81(7) . . ? N2 Mo1A O3 62.82(6) . . ? O3 P1 N3 104.00(9) . . ? O3 P1 N2 91.30(9) . . ? N3 P1 N2 107.16(9) . . ? N2 Si1 C31 112.44(10) . . ? N2 Si1 C32 109.75(10) . . ? C31 Si1 C32 108.70(12) . . ? N2 Si1 C33 109.13(10) . . ? C31 Si1 C33 108.17(12) . . ? C32 Si1 C33 108.56(12) . . ? N3 Si2 C41 112.62(10) . . ? N3 Si2 C42 111.71(10) . . ? C41 Si2 C42 109.34(13) . . ? N3 Si2 C43 112.28(11) . . ? C41 Si2 C43 105.21(13) . . ? C42 Si2 C43 105.22(12) . . ? N3 Si3 C52 111.36(12) . . ? N3 Si3 C51 111.95(11) . . ? C52 Si3 C51 106.61(12) . . ? N3 Si3 C53 111.85(11) . . ? C52 Si3 C53 109.06(13) . . ? C51 Si3 C53 105.71(13) . . ? C11 O1 Mo1A 136.20(14) . . ? C21 O2 Mo1A 136.04(14) . . ? C61 O3 P1 121.40(13) . . ? C61 O3 Mo1A 132.80(13) . . ? P1 O3 Mo1A 91.19(7) . . ? P1 N2 Si1 120.00(11) . . ? P1 N2 Mo1A 112.52(9) . . ? Si1 N2 Mo1A 122.19(10) . . ? P1 N3 Si3 114.04(10) . . ? P1 N3 Si2 124.52(11) . . ? Si3 N3 Si2 121.43(11) . . ? O1 C11 C13 108.92(19) . . ? O1 C11 C14 105.48(19) . . ? C13 C11 C14 110.9(2) . . ? O1 C11 C12 109.43(18) . . ? C13 C11 C12 111.2(2) . . ? C14 C11 C12 110.8(2) . . ? 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 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O2 C21 C23 105.2(2) . . ? O2 C21 C22 107.70(19) . . ? C23 C21 C22 112.3(2) . . ? O2 C21 C24 110.04(18) . . ? C23 C21 C24 110.5(2) . . ? C22 C21 C24 110.9(2) . . ? 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 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si1 C31 H31A 109.5 . . ? Si1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si1 C32 H32A 109.5 . . ? Si1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si1 C33 H33A 109.5 . . ? Si1 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si1 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si2 C41 H41A 109.5 . . ? Si2 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? Si2 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? Si2 C42 H42A 109.5 . . ? Si2 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? Si2 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? Si2 C43 H43A 109.5 . . ? Si2 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? Si2 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? Si3 C51 H51A 109.5 . . ? Si3 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? Si3 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? Si3 C52 H52A 109.5 . . ? Si3 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? Si3 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? Si3 C53 H53A 109.5 . . ? Si3 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? Si3 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? O3 C61 C63 110.10(18) . . ? O3 C61 C62 109.15(18) . . ? C63 C61 C62 111.8(2) . . ? O3 C61 C64 102.76(18) . . ? C63 C61 C64 112.2(2) . . ? C62 C61 C64 110.5(2) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? N12 Mo2A O22 103.99(8) . . ? N12 Mo2A O12 104.50(9) . . ? O22 Mo2A O12 111.92(7) . . ? N12 Mo2A N22 99.02(9) . . ? O22 Mo2A N22 116.52(8) . . ? O12 Mo2A N22 117.99(7) . . ? N12 Mo2A O32 160.44(7) . . ? O22 Mo2A O32 89.72(7) . . ? O12 Mo2A O32 82.54(7) . . ? N22 Mo2A O32 61.97(6) . . ? O32 P2 N32 103.59(9) . . ? O32 P2 N22 91.54(9) . . ? N32 P2 N22 107.77(9) . . ? N22 Si12 C34 111.08(10) . . ? N22 Si12 C35 110.85(11) . . ? C34 Si12 C35 108.53(12) . . ? N22 Si12 C36 109.59(11) . . ? C34 Si12 C36 109.30(12) . . ? C35 Si12 C36 107.40(12) . . ? N32 Si22 C44 112.44(10) . . ? N32 Si22 C45 109.68(10) . . ? C44 Si22 C45 112.07(12) . . ? N32 Si22 C46 113.16(11) . . ? C44 Si22 C46 103.60(12) . . ? C45 Si22 C46 105.61(12) . . ? N32 Si32 C55 110.92(12) . . ? N32 Si32 C54 112.58(11) . . ? C55 Si32 C54 106.44(12) . . ? N32 Si32 C56 111.80(11) . . ? C55 Si32 C56 108.87(13) . . ? C54 Si32 C56 105.95(12) . . ? C15 O12 Mo2A 136.96(14) . . ? C25 O22 Mo2A 135.15(14) . . ? C65 O32 P2 119.99(13) . . ? C65 O32 Mo2A 134.24(13) . . ? P2 O32 Mo2A 91.28(7) . . ? P2 N22 Si12 120.11(11) . . ? P2 N22 Mo2A 114.20(9) . . ? Si12 N22 Mo2A 120.50(10) . . ? P2 N32 Si22 125.00(12) . . ? P2 N32 Si32 114.71(10) . . ? Si22 N32 Si32 120.28(11) . . ? O12 C15 C16 110.27(17) . . ? O12 C15 C17 108.32(19) . . ? C16 C15 C17 111.2(2) . . ? O12 C15 C18 105.42(18) . . ? C16 C15 C18 110.3(2) . . ? C17 C15 C18 111.11(19) . . ? 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 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O22 C25 C28 109.24(18) . . ? O22 C25 C26 108.74(19) . . ? C28 C25 C26 111.1(2) . . ? O22 C25 C27 105.53(19) . . ? C28 C25 C27 110.5(2) . . ? C26 C25 C27 111.6(2) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si12 C34 H34A 109.5 . . ? Si12 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si12 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si12 C35 H35A 109.5 . . ? Si12 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si12 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Si12 C36 H36A 109.5 . . ? Si12 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? Si12 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? Si22 C44 H44A 109.5 . . ? Si22 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? Si22 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? Si22 C45 H45A 109.5 . . ? Si22 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? Si22 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? Si22 C46 H46A 109.5 . . ? Si22 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? Si22 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? Si32 C54 H54A 109.5 . . ? Si32 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? Si32 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? Si32 C55 H55A 109.5 . . ? Si32 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? Si32 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? Si32 C56 H56A 109.5 . . ? Si32 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? Si32 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C67 C65 O32 110.35(19) . . ? C67 C65 C66 111.8(2) . . ? O32 C65 C66 108.77(18) . . ? C67 C65 C68 111.9(2) . . ? O32 C65 C68 102.50(18) . . ? C66 C65 C68 111.1(2) . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C65 C67 H67A 109.5 . . ? C65 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C65 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C65 C68 H68A 109.5 . . ? C65 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C65 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 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 N1 Mo1A O1 C11 -6.1(2) . . . . ? O2 Mo1A O1 C11 107.1(2) . . . . ? N2 Mo1A O1 C11 -114.8(2) . . . . ? O3 Mo1A O1 C11 -170.1(2) . . . . ? N1 Mo1A O2 C21 8.4(2) . . . . ? O1 Mo1A O2 C21 -104.1(2) . . . . ? N2 Mo1A O2 C21 117.6(2) . . . . ? O3 Mo1A O2 C21 174.4(2) . . . . ? N3 P1 O3 C61 -97.56(16) . . . . ? N2 P1 O3 C61 154.40(15) . . . . ? N3 P1 O3 Mo1A 118.46(8) . . . . ? N2 P1 O3 Mo1A 10.42(7) . . . . ? N1 Mo1A O3 C61 -140.2(2) . . . . ? O2 Mo1A O3 C61 90.77(17) . . . . ? O1 Mo1A O3 C61 -22.72(16) . . . . ? N2 Mo1A O3 C61 -146.91(17) . . . . ? N1 Mo1A O3 P1 -3.4(2) . . . . ? O2 Mo1A O3 P1 -132.39(7) . . . . ? O1 Mo1A O3 P1 114.11(7) . . . . ? N2 Mo1A O3 P1 -10.08(6) . . . . ? O3 P1 N2 Si1 -169.43(10) . . . . ? N3 P1 N2 Si1 85.48(12) . . . . ? O3 P1 N2 Mo1A -14.57(9) . . . . ? N3 P1 N2 Mo1A -119.66(10) . . . . ? C31 Si1 N2 P1 -149.25(12) . . . . ? C32 Si1 N2 P1 89.63(14) . . . . ? C33 Si1 N2 P1 -29.22(14) . . . . ? C31 Si1 N2 Mo1A 58.38(14) . . . . ? C32 Si1 N2 Mo1A -62.74(14) . . . . ? C33 Si1 N2 Mo1A 178.41(11) . . . . ? N1 Mo1A N2 P1 -167.32(9) . . . . ? O2 Mo1A N2 P1 80.49(10) . . . . ? O1 Mo1A N2 P1 -56.25(11) . . . . ? O3 Mo1A N2 P1 10.63(7) . . . . ? N1 Mo1A N2 Si1 -13.09(12) . . . . ? O2 Mo1A N2 Si1 -125.28(10) . . . . ? O1 Mo1A N2 Si1 97.99(11) . . . . ? O3 Mo1A N2 Si1 164.86(12) . . . . ? O3 P1 N3 Si3 127.60(10) . . . . ? N2 P1 N3 Si3 -136.58(10) . . . . ? O3 P1 N3 Si2 -51.02(14) . . . . ? N2 P1 N3 Si2 44.80(14) . . . . ? C52 Si3 N3 P1 120.13(12) . . . . ? C51 Si3 N3 P1 0.89(15) . . . . ? C53 Si3 N3 P1 -117.55(13) . . . . ? C52 Si3 N3 Si2 -61.20(15) . . . . ? C51 Si3 N3 Si2 179.56(12) . . . . ? C53 Si3 N3 Si2 61.12(15) . . . . ? C41 Si2 N3 P1 58.80(16) . . . . ? C42 Si2 N3 P1 -64.71(15) . . . . ? C43 Si2 N3 P1 177.35(13) . . . . ? C41 Si2 N3 Si3 -119.72(14) . . . . ? C42 Si2 N3 Si3 116.76(13) . . . . ? C43 Si2 N3 Si3 -1.18(16) . . . . ? Mo1A O1 C11 C13 69.0(3) . . . . ? Mo1A O1 C11 C14 -171.92(16) . . . . ? Mo1A O1 C11 C12 -52.7(3) . . . . ? Mo1A O2 C21 C23 165.66(17) . . . . ? Mo1A O2 C21 C22 -74.4(3) . . . . ? Mo1A O2 C21 C24 46.6(3) . . . . ? P1 O3 C61 C63 67.0(2) . . . . ? Mo1A O3 C61 C63 -166.21(14) . . . . ? P1 O3 C61 C62 -56.0(2) . . . . ? Mo1A O3 C61 C62 70.7(2) . . . . ? P1 O3 C61 C64 -173.27(15) . . . . ? Mo1A O3 C61 C64 -46.5(2) . . . . ? N12 Mo2A O12 C15 -6.9(2) . . . . ? O22 Mo2A O12 C15 105.0(2) . . . . ? N22 Mo2A O12 C15 -115.6(2) . . . . ? O32 Mo2A O12 C15 -168.3(2) . . . . ? N12 Mo2A O22 C25 3.1(2) . . . . ? O12 Mo2A O22 C25 -109.1(2) . . . . ? N22 Mo2A O22 C25 110.9(2) . . . . ? O32 Mo2A O22 C25 169.0(2) . . . . ? N32 P2 O32 C65 -99.32(16) . . . . ? N22 P2 O32 C65 151.98(16) . . . . ? N32 P2 O32 Mo2A 115.73(8) . . . . ? N22 P2 O32 Mo2A 7.03(7) . . . . ? N12 Mo2A O32 C65 -128.3(2) . . . . ? O22 Mo2A O32 C65 96.59(17) . . . . ? O12 Mo2A O32 C65 -15.57(16) . . . . ? N22 Mo2A O32 C65 -142.86(18) . . . . ? N12 Mo2A O32 P2 7.7(2) . . . . ? O22 Mo2A O32 P2 -127.38(7) . . . . ? O12 Mo2A O32 P2 120.46(7) . . . . ? N22 Mo2A O32 P2 -6.82(7) . . . . ? O32 P2 N22 Si12 -164.70(11) . . . . ? N32 P2 N22 Si12 90.50(12) . . . . ? O32 P2 N22 Mo2A -10.05(10) . . . . ? N32 P2 N22 Mo2A -114.85(10) . . . . ? C34 Si12 N22 P2 -138.73(13) . . . . ? C35 Si12 N22 P2 100.52(14) . . . . ? C36 Si12 N22 P2 -17.85(15) . . . . ? C34 Si12 N22 Mo2A 68.22(14) . . . . ? C35 Si12 N22 Mo2A -52.53(14) . . . . ? C36 Si12 N22 Mo2A -170.91(11) . . . . ? N12 Mo2A N22 P2 -167.83(10) . . . . ? O22 Mo2A N22 P2 81.51(11) . . . . ? O12 Mo2A N22 P2 -56.02(12) . . . . ? O32 Mo2A N22 P2 7.28(7) . . . . ? N12 Mo2A N22 Si12 -13.28(12) . . . . ? O22 Mo2A N22 Si12 -123.94(10) . . . . ? O12 Mo2A N22 Si12 98.53(11) . . . . ? O32 Mo2A N22 Si12 161.83(12) . . . . ? O32 P2 N32 Si22 -50.26(14) . . . . ? N22 P2 N32 Si22 45.85(15) . . . . ? O32 P2 N32 Si32 128.97(10) . . . . ? N22 P2 N32 Si32 -134.91(10) . . . . ? C44 Si22 N32 P2 55.36(16) . . . . ? C45 Si22 N32 P2 -70.05(16) . . . . ? C46 Si22 N32 P2 172.31(13) . . . . ? C44 Si22 N32 Si32 -123.84(14) . . . . ? C45 Si22 N32 Si32 110.76(14) . . . . ? C46 Si22 N32 Si32 -6.88(16) . . . . ? C55 Si32 N32 P2 123.49(13) . . . . ? C54 Si32 N32 P2 4.34(15) . . . . ? C56 Si32 N32 P2 -114.79(13) . . . . ? C55 Si32 N32 Si22 -57.24(15) . . . . ? C54 Si32 N32 Si22 -176.38(12) . . . . ? C56 Si32 N32 Si22 64.48(15) . . . . ? Mo2A O12 C15 C16 -43.0(3) . . . . ? Mo2A O12 C15 C17 78.9(2) . . . . ? Mo2A O12 C15 C18 -162.09(16) . . . . ? Mo2A O22 C25 C28 54.3(3) . . . . ? Mo2A O22 C25 C26 -67.1(3) . . . . ? Mo2A O22 C25 C27 173.10(17) . . . . ? P2 O32 C65 C67 60.8(2) . . . . ? Mo2A O32 C65 C67 -172.50(13) . . . . ? P2 O32 C65 C66 -62.3(2) . . . . ? Mo2A O32 C65 C66 64.5(2) . . . . ? P2 O32 C65 C68 -179.93(15) . . . . ? Mo2A O32 C65 C68 -53.2(2) . . . . ? 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 C16 H16A N12 0.98 2.55 3.281(3) 131.4 . C24 H24A N1 0.98 2.61 3.334(3) 130.5 . C28 H28B N12 0.98 2.63 3.341(3) 130.0 . C31 H31A N1 0.98 2.50 3.198(3) 128.4 . C34 H34B N12 0.98 2.62 3.298(3) 126.7 . C41 H41A O2 0.98 2.59 3.495(4) 152.9 . C41 H41A O3 0.98 2.58 3.198(3) 121.4 . C44 H44B O22 0.98 2.46 3.364(3) 153.3 . C44 H44B O32 0.98 2.57 3.147(3) 117.5 . C64 H64C O1 0.98 2.58 3.386(3) 139.2 . C66 H66B O12 0.98 2.58 3.391(3) 140.0 . _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.04 _refine_diff_density_min -0.65 _refine_diff_density_rms 0.094 #===================================================================== data_5c _database_code_depnum_ccdc_archive 'CCDC 781903' #TrackingRef '- ANAT.cif' #===================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H54 Mo N3 O3 P Si3' _chemical_formula_sum 'C21 H54 Mo N3 O3 P Si3' _chemical_formula_weight 607.85 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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.082(4) _cell_length_b 10.356(4) _cell_length_c 18.523(7) _cell_angle_alpha 83.90(4) _cell_angle_beta 89.83(4) _cell_angle_gamma 61.91(5) _cell_volume 1694.1(14) _cell_formula_units_Z 2 _cell_measurement_temperature 250(2) _cell_measurement_reflns_used 15019 _cell_measurement_theta_min 4 _cell_measurement_theta_max 30 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.192 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 0.563 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.903 _exptl_absorpt_correction_T_max 0.950 _exptl_absorpt_process_details 'CrysAlis RED; Oxford-Diffraction Poland, 2003' _exptl_special_details ; ? ; _diffrn_ambient_temperature 250(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 'Xcalibur PX kappa-geometry diffractometer with Onyx CCD camera' _diffrn_measurement_method 'omega and phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36400 _diffrn_reflns_av_R_equivalents 0.0726 _diffrn_reflns_av_sigmaI/netI 0.0931 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 4.59 _diffrn_reflns_theta_max 30.07 _reflns_number_total 9881 _reflns_number_gt 5271 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD; Oxford-Diffraction Poland, 2003' _computing_cell_refinement 'CrysAlis RED; Oxford-Diffraction Poland, 2003' _computing_data_reduction 'CrysAlis RED; Oxford-Diffraction Poland, 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^)+(0.047P^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 9881 _refine_ls_number_parameters 312 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.1064 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.1208 _refine_ls_wR_factor_gt 0.1110 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.043 _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 Mo1A Mo 0.59091(3) 0.53129(3) 0.829234(15) 0.04287(11) Uani 0.9653(11) 1 d P . . Mo1B Mo 0.5261(11) 0.6328(11) 0.7849(6) 0.062(4) Uiso 0.0347(11) 1 d P . . P1 P 0.82817(9) 0.42068(9) 0.71215(4) 0.0423(2) Uani 1 1 d . . . Si1 Si 0.90910(12) 0.22353(13) 0.85415(6) 0.0689(3) Uani 1 1 d . . . Si2 Si 0.66848(11) 0.27245(10) 0.63977(5) 0.0515(3) Uani 1 1 d . . . Si3 Si 0.97692(12) 0.23986(12) 0.59554(6) 0.0646(3) Uani 1 1 d . . . O1 O 0.5987(3) 0.7045(3) 0.84037(12) 0.0649(7) Uani 1 1 d . A . O2 O 0.4067(2) 0.5672(2) 0.78900(12) 0.0564(6) Uani 1 1 d . . . O3 O 0.6637(2) 0.5743(2) 0.69822(10) 0.0396(5) Uani 1 1 d . . . N1 N 0.5986(3) 0.4558(3) 0.91296(14) 0.0572(7) Uani 1 1 d . . . N2 N 0.7742(3) 0.3698(3) 0.79344(13) 0.0434(6) Uani 1 1 d . . . N3 N 0.8199(3) 0.3115(3) 0.65064(13) 0.0445(6) Uani 1 1 d . . . C11 C 0.5932(6) 0.7903(5) 0.8987(2) 0.0834(13) Uani 1 1 d D . . C12A C 0.7337(11) 0.7045(12) 0.9457(6) 0.106(3) Uiso 0.50 1 d PD A 1 H12A H 0.8199 0.6713 0.9156 0.159 Uiso 0.50 1 calc PR A 1 H12B H 0.7317 0.6199 0.9726 0.159 Uiso 0.50 1 calc PR A 1 H12C H 0.7411 0.7665 0.9795 0.159 Uiso 0.50 1 calc PR A 1 C13A C 0.4501(8) 0.8134(8) 0.9439(4) 0.0562(18) Uiso 0.50 1 d PD A 1 H13A H 0.3609 0.8572 0.9112 0.084 Uiso 0.50 1 calc PR A 1 H13B H 0.4374 0.8782 0.9805 0.084 Uiso 0.50 1 calc PR A 1 H13C H 0.4651 0.7189 0.9674 0.084 Uiso 0.50 1 calc PR A 1 C14A C 0.5934(14) 0.9245(12) 0.8669(7) 0.122(4) Uiso 0.50 1 d PD A 1 H14A H 0.6843 0.8995 0.8409 0.183 Uiso 0.50 1 calc PR A 1 H14B H 0.5898 0.9831 0.9051 0.183 Uiso 0.50 1 calc PR A 1 H14C H 0.5061 0.9806 0.8334 0.183 Uiso 0.50 1 calc PR A 1 C12B C 0.7519(12) 0.7721(16) 0.9067(8) 0.146(5) Uiso 0.50 1 d PD A 2 H12D H 0.8196 0.6734 0.9293 0.219 Uiso 0.50 1 calc PR A 2 H12E H 0.7513 0.8437 0.9366 0.219 Uiso 0.50 1 calc PR A 2 H12F H 0.7857 0.7877 0.8590 0.219 Uiso 0.50 1 calc PR A 2 C13B C 0.5329(15) 0.7621(15) 0.9652(6) 0.137(5) Uiso 0.50 1 d PD A 2 H13D H 0.6034 0.6661 0.9898 0.206 Uiso 0.50 1 calc PR A 2 H13E H 0.4380 0.7638 0.9545 0.206 Uiso 0.50 1 calc PR A 2 H13F H 0.5167 0.8374 0.9963 0.206 Uiso 0.50 1 calc PR A 2 C14B C 0.5036(10) 0.9577(8) 0.8615(4) 0.067(2) Uiso 0.50 1 d PD A 2 H14D H 0.4042 0.9784 0.8439 0.101 Uiso 0.50 1 calc PR A 2 H14E H 0.5584 0.9724 0.8211 0.101 Uiso 0.50 1 calc PR A 2 H14F H 0.4940 1.0237 0.8970 0.101 Uiso 0.50 1 calc PR A 2 C21 C 0.2758(4) 0.5559(6) 0.8144(2) 0.0815(13) Uani 1 1 d . . . C22 C 0.3201(7) 0.3949(7) 0.8307(4) 0.148(3) Uani 1 1 d . . . H22A H 0.4040 0.3483 0.8666 0.222 Uiso 1 1 calc R . . H22B H 0.3497 0.3481 0.7865 0.222 Uiso 1 1 calc R . . H22C H 0.2354 0.3845 0.8495 0.222 Uiso 1 1 calc R . . C23 C 0.2255(5) 0.6321(6) 0.8831(3) 0.1149(18) Uani 1 1 d . . . H23A H 0.3093 0.5908 0.9189 0.172 Uiso 1 1 calc R . . H23B H 0.1437 0.6171 0.9026 0.172 Uiso 1 1 calc R . . H23C H 0.1913 0.7369 0.8713 0.172 Uiso 1 1 calc R . . C24 C 0.1567(6) 0.6336(10) 0.7532(3) 0.188(4) Uani 1 1 d . . . H24A H 0.1934 0.5868 0.7095 0.282 Uiso 1 1 calc R . . H24B H 0.1338 0.7362 0.7445 0.282 Uiso 1 1 calc R . . H24C H 0.0664 0.6278 0.7665 0.282 Uiso 1 1 calc R . . C31 C 0.9873(5) 0.2972(6) 0.9200(2) 0.1089(17) Uani 1 1 d . . . H31A H 0.9154 0.3393 0.9567 0.163 Uiso 1 1 calc R . . H31B H 1.0068 0.3729 0.8945 0.163 Uiso 1 1 calc R . . H31C H 1.0805 0.2180 0.9430 0.163 Uiso 1 1 calc R . . C32 C 1.0674(6) 0.0977(6) 0.8023(3) 0.142(2) Uani 1 1 d . . . H32A H 1.1423 0.0180 0.8356 0.213 Uiso 1 1 calc R . . H32B H 1.1129 0.1522 0.7765 0.213 Uiso 1 1 calc R . . H32C H 1.0296 0.0574 0.7676 0.213 Uiso 1 1 calc R . . C33 C 0.8279(5) 0.1156(5) 0.9054(2) 0.0999(16) Uani 1 1 d . . . H33A H 0.8051 0.1463 0.9536 0.150 Uiso 1 1 calc R . . H33B H 0.8999 0.0115 0.9095 0.150 Uiso 1 1 calc R . . H33C H 0.7362 0.1326 0.8798 0.150 Uiso 1 1 calc R . . C41 C 0.6915(5) 0.1653(5) 0.5609(2) 0.0834(12) Uani 1 1 d . . . H41A H 0.7806 0.0699 0.5701 0.125 Uiso 1 1 calc R . . H41B H 0.7020 0.2191 0.5170 0.125 Uiso 1 1 calc R . . H41C H 0.6037 0.1514 0.5547 0.125 Uiso 1 1 calc R . . C42 C 0.6587(5) 0.1575(5) 0.7206(2) 0.0834(13) Uani 1 1 d . . . H42A H 0.7547 0.0688 0.7301 0.125 Uiso 1 1 calc R . . H42B H 0.5804 0.1307 0.7120 0.125 Uiso 1 1 calc R . . H42C H 0.6358 0.2123 0.7623 0.125 Uiso 1 1 calc R . . C43 C 0.4852(4) 0.4398(4) 0.6198(2) 0.0714(11) Uani 1 1 d . . . H43A H 0.4072 0.4119 0.6134 0.107 Uiso 1 1 calc R . . H43B H 0.4897 0.4969 0.5757 0.107 Uiso 1 1 calc R . . H43C H 0.4626 0.4987 0.6600 0.107 Uiso 1 1 calc R . . C51 C 0.9202(5) 0.3122(5) 0.4974(2) 0.0872(13) Uani 1 1 d . . . H51A H 0.8662 0.4190 0.4923 0.131 Uiso 1 1 calc R . . H51B H 0.8556 0.2751 0.4798 0.131 Uiso 1 1 calc R . . H51C H 1.0093 0.2798 0.4694 0.131 Uiso 1 1 calc R . . C52 C 1.1224(4) 0.2926(6) 0.6198(2) 0.0950(14) Uani 1 1 d . . . H52A H 1.1616 0.2512 0.6694 0.143 Uiso 1 1 calc R . . H52B H 1.0777 0.3991 0.6158 0.143 Uiso 1 1 calc R . . H52C H 1.2038 0.2548 0.5870 0.143 Uiso 1 1 calc R . . C53 C 1.0704(5) 0.0341(4) 0.6065(3) 0.1042(16) Uani 1 1 d . . . H53A H 0.9971 0.0018 0.5963 0.156 Uiso 1 1 calc R . . H53B H 1.1122 -0.0035 0.6560 0.156 Uiso 1 1 calc R . . H53C H 1.1505 -0.0030 0.5730 0.156 Uiso 1 1 calc R . . C61 C 0.6519(4) 0.7065(3) 0.65155(17) 0.0501(8) Uani 1 1 d . . . C62 C 0.4856(5) 0.8190(4) 0.6572(2) 0.0824(13) Uani 1 1 d . . . H62A H 0.4634 0.9108 0.6278 0.124 Uiso 1 1 calc R . . H62B H 0.4664 0.8366 0.7075 0.124 Uiso 1 1 calc R . . H62C H 0.4220 0.7805 0.6399 0.124 Uiso 1 1 calc R . . C63 C 0.7554(5) 0.7553(4) 0.6834(2) 0.0747(11) Uani 1 1 d . . . H63A H 0.8591 0.6822 0.6789 0.112 Uiso 1 1 calc R . . H63B H 0.7365 0.7661 0.7344 0.112 Uiso 1 1 calc R . . H63C H 0.7374 0.8491 0.6576 0.112 Uiso 1 1 calc R . . C64 C 0.6862(4) 0.6724(4) 0.57447(19) 0.0692(10) Uani 1 1 d . . . H64A H 0.7909 0.5992 0.5729 0.104 Uiso 1 1 calc R . . H64B H 0.6676 0.7616 0.5436 0.104 Uiso 1 1 calc R . . H64C H 0.6221 0.6344 0.5573 0.104 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 Mo1A 0.0530(2) 0.04890(19) 0.03832(17) -0.00574(13) 0.00500(13) -0.03359(16) P1 0.0431(5) 0.0467(5) 0.0406(5) -0.0017(4) 0.0017(4) -0.0249(4) Si1 0.0619(7) 0.0780(7) 0.0505(6) 0.0145(5) -0.0085(5) -0.0242(6) Si2 0.0682(6) 0.0510(6) 0.0462(5) -0.0112(4) 0.0052(5) -0.0360(5) Si3 0.0596(7) 0.0669(7) 0.0563(6) -0.0131(5) 0.0166(5) -0.0198(5) O1 0.1029(19) 0.0727(16) 0.0520(14) -0.0236(12) 0.0238(13) -0.0654(15) O2 0.0468(13) 0.0747(16) 0.0525(14) -0.0080(12) 0.0063(10) -0.0326(12) O3 0.0459(12) 0.0371(11) 0.0373(11) 0.0001(9) 0.0020(9) -0.0219(10) N1 0.076(2) 0.0688(19) 0.0407(15) -0.0043(13) 0.0064(14) -0.0461(17) N2 0.0501(15) 0.0478(15) 0.0371(14) -0.0015(11) 0.0003(11) -0.0279(13) N3 0.0492(15) 0.0391(14) 0.0406(14) -0.0044(11) 0.0062(12) -0.0171(12) C11 0.150(4) 0.086(3) 0.060(2) -0.028(2) 0.031(3) -0.090(3) C21 0.049(2) 0.129(4) 0.079(3) -0.026(3) 0.016(2) -0.050(3) C22 0.141(5) 0.163(6) 0.214(7) -0.059(5) 0.080(5) -0.125(5) C23 0.062(3) 0.171(5) 0.104(4) -0.029(4) 0.031(3) -0.047(3) C24 0.063(3) 0.376(11) 0.114(5) -0.007(6) -0.005(3) -0.099(5) C31 0.092(3) 0.164(5) 0.074(3) 0.018(3) -0.030(3) -0.069(3) C32 0.104(4) 0.117(4) 0.088(4) 0.029(3) 0.004(3) 0.034(3) C33 0.116(4) 0.088(3) 0.085(3) 0.042(3) -0.025(3) -0.049(3) C41 0.109(3) 0.085(3) 0.073(3) -0.033(2) 0.007(2) -0.055(3) C42 0.124(4) 0.091(3) 0.071(3) -0.011(2) 0.012(2) -0.080(3) C43 0.062(2) 0.080(3) 0.082(3) -0.020(2) 0.000(2) -0.039(2) C51 0.107(3) 0.102(3) 0.056(3) -0.019(2) 0.027(2) -0.050(3) C52 0.070(3) 0.129(4) 0.086(3) -0.027(3) 0.038(2) -0.045(3) C53 0.103(4) 0.072(3) 0.097(4) -0.028(3) 0.013(3) -0.005(3) C61 0.065(2) 0.0381(18) 0.0467(19) 0.0021(14) 0.0013(16) -0.0254(17) C62 0.091(3) 0.046(2) 0.086(3) 0.006(2) 0.012(2) -0.015(2) C63 0.108(3) 0.065(2) 0.073(3) -0.004(2) 0.010(2) -0.061(2) C64 0.090(3) 0.063(2) 0.056(2) 0.0061(18) 0.002(2) -0.040(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1A N1 1.646(3) . ? Mo1A O2 1.855(2) . ? Mo1A O1 1.865(2) . ? Mo1A N2 1.992(3) . ? Mo1A O3 2.587(2) . ? P1 O3 1.667(2) . ? P1 N2 1.714(3) . ? P1 N3 1.716(3) . ? Si1 N2 1.765(3) . ? Si1 C33 1.858(4) . ? Si1 C31 1.860(5) . ? Si1 C32 1.862(5) . ? Si2 N3 1.771(3) . ? Si2 C42 1.844(4) . ? Si2 C43 1.846(4) . ? Si2 C41 1.877(4) . ? Si3 N3 1.773(3) . ? Si3 C52 1.860(5) . ? Si3 C53 1.868(4) . ? Si3 C51 1.872(4) . ? O1 C11 1.456(4) . ? O2 C21 1.451(4) . ? O3 C61 1.494(3) . ? C11 C13B 1.433(10) . ? C11 C14A 1.452(10) . ? C11 C12A 1.487(9) . ? C11 C12B 1.526(10) . ? C11 C13A 1.596(7) . ? C11 C14B 1.604(8) . ? C12A H12A 0.9700 . ? C12A H12B 0.9700 . ? C12A H12C 0.9700 . ? C13A H13A 0.9700 . ? C13A H13B 0.9700 . ? C13A H13C 0.9700 . ? C14A H14A 0.9700 . ? C14A H14B 0.9700 . ? C14A H14C 0.9700 . ? C12B H12D 0.9700 . ? C12B H12E 0.9700 . ? C12B H12F 0.9700 . ? C13B H13D 0.9700 . ? C13B H13E 0.9700 . ? C13B H13F 0.9700 . ? C14B H14D 0.9700 . ? C14B H14E 0.9700 . ? C14B H14F 0.9700 . ? C21 C22 1.504(7) . ? C21 C24 1.509(7) . ? C21 C23 1.527(6) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C33 H33C 0.9700 . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C41 H41C 0.9700 . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C42 H42C 0.9700 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C43 H43C 0.9700 . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C51 H51C 0.9700 . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C52 H52C 0.9700 . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C53 H53C 0.9700 . ? C61 C63 1.502(5) . ? C61 C64 1.507(5) . ? C61 C62 1.538(5) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C62 H62C 0.9700 . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C63 H63C 0.9700 . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C64 H64C 0.9700 . ? 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 N1 Mo1A O2 104.77(12) . . ? N1 Mo1A O1 104.37(12) . . ? O2 Mo1A O1 112.48(12) . . ? N1 Mo1A N2 99.32(13) . . ? O2 Mo1A N2 116.83(10) . . ? O1 Mo1A N2 116.44(11) . . ? N1 Mo1A O3 161.22(11) . . ? O2 Mo1A O3 87.24(9) . . ? O1 Mo1A O3 83.57(9) . . ? N2 Mo1A O3 62.07(9) . . ? O3 P1 N2 91.18(12) . . ? O3 P1 N3 104.21(12) . . ? N2 P1 N3 107.41(12) . . ? N2 Si1 C33 112.03(17) . . ? N2 Si1 C31 109.86(19) . . ? C33 Si1 C31 108.9(2) . . ? N2 Si1 C32 109.39(18) . . ? C33 Si1 C32 108.7(3) . . ? C31 Si1 C32 107.8(3) . . ? N3 Si2 C42 110.82(16) . . ? N3 Si2 C43 113.06(15) . . ? C42 Si2 C43 110.0(2) . . ? N3 Si2 C41 111.84(17) . . ? C42 Si2 C41 106.07(19) . . ? C43 Si2 C41 104.64(19) . . ? N3 Si3 C52 112.35(17) . . ? N3 Si3 C53 110.54(19) . . ? C52 Si3 C53 106.8(2) . . ? N3 Si3 C51 111.31(16) . . ? C52 Si3 C51 105.9(2) . . ? C53 Si3 C51 109.7(2) . . ? C11 O1 Mo1A 138.2(2) . . ? C21 O2 Mo1A 136.6(2) . . ? C61 O3 P1 120.44(18) . . ? C61 O3 Mo1A 133.77(17) . . ? P1 O3 Mo1A 91.21(9) . . ? P1 N2 Si1 119.75(15) . . ? P1 N2 Mo1A 113.72(13) . . ? Si1 N2 Mo1A 121.21(14) . . ? P1 N3 Si2 124.49(15) . . ? P1 N3 Si3 114.54(15) . . ? Si2 N3 Si3 120.96(15) . . ? C13B C11 O1 116.8(6) . . ? C14A C11 O1 108.3(6) . . ? C14A C11 C12A 107.2(7) . . ? O1 C11 C12A 108.1(5) . . ? C13B C11 C12B 115.0(9) . . ? O1 C11 C12B 105.0(6) . . ? C14A C11 C13A 115.5(6) . . ? O1 C11 C13A 107.3(4) . . ? C12A C11 C13A 110.3(6) . . ? C12B C11 C13A 142.5(7) . . ? C13B C11 C14B 113.9(7) . . ? O1 C11 C14B 103.7(4) . . ? C12B C11 C14B 100.6(7) . . ? C13A C11 C14B 90.0(5) . . ? C11 C12A H12A 109.5 . . ? C11 C12A H12B 109.5 . . ? C11 C12A H12C 109.5 . . ? C11 C13A H13A 109.5 . . ? C11 C13A H13B 109.5 . . ? C11 C13A H13C 109.5 . . ? C11 C14A H14A 109.5 . . ? C11 C14A H14B 109.5 . . ? C11 C14A H14C 109.5 . . ? C11 C12B H12D 109.5 . . ? C11 C12B H12E 109.5 . . ? H12D C12B H12E 109.5 . . ? C11 C12B H12F 109.5 . . ? H12D C12B H12F 109.5 . . ? H12E C12B H12F 109.5 . . ? C11 C13B H13D 109.5 . . ? C11 C13B H13E 109.5 . . ? H13D C13B H13E 109.5 . . ? C11 C13B H13F 109.5 . . ? H13D C13B H13F 109.5 . . ? H13E C13B H13F 109.5 . . ? C11 C14B H14D 109.5 . . ? C11 C14B H14E 109.5 . . ? H14D C14B H14E 109.5 . . ? C11 C14B H14F 109.5 . . ? H14D C14B H14F 109.5 . . ? H14E C14B H14F 109.5 . . ? O2 C21 C22 107.9(3) . . ? O2 C21 C24 105.4(4) . . ? C22 C21 C24 112.9(5) . . ? O2 C21 C23 109.3(3) . . ? C22 C21 C23 110.2(4) . . ? C24 C21 C23 110.9(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 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si1 C31 H31A 109.5 . . ? Si1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si1 C32 H32A 109.5 . . ? Si1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si1 C33 H33A 109.5 . . ? Si1 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si1 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si2 C41 H41A 109.5 . . ? Si2 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? Si2 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? Si2 C42 H42A 109.5 . . ? Si2 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? Si2 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? Si2 C43 H43A 109.5 . . ? Si2 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? Si2 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? Si3 C51 H51A 109.5 . . ? Si3 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? Si3 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? Si3 C52 H52A 109.5 . . ? Si3 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? Si3 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? Si3 C53 H53A 109.5 . . ? Si3 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? Si3 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? O3 C61 C63 109.2(3) . . ? O3 C61 C64 110.2(3) . . ? C63 C61 C64 112.2(3) . . ? O3 C61 C62 101.8(3) . . ? C63 C61 C62 111.6(3) . . ? C64 C61 C62 111.4(3) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 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 N1 Mo1A O1 C11 -8.3(4) . . . . ? O2 Mo1A O1 C11 104.7(4) . . . . ? N2 Mo1A O1 C11 -116.6(4) . . . . ? O3 Mo1A O1 C11 -171.0(4) . . . . ? N1 Mo1A O2 C21 5.9(4) . . . . ? O1 Mo1A O2 C21 -106.8(4) . . . . ? N2 Mo1A O2 C21 114.7(4) . . . . ? O3 Mo1A O2 C21 171.3(4) . . . . ? N2 P1 O3 C61 154.0(2) . . . . ? N3 P1 O3 C61 -97.7(2) . . . . ? N2 P1 O3 Mo1A 9.47(9) . . . . ? N3 P1 O3 Mo1A 117.77(10) . . . . ? N1 Mo1A O3 C61 -137.3(4) . . . . ? O2 Mo1A O3 C61 92.1(2) . . . . ? O1 Mo1A O3 C61 -20.9(2) . . . . ? N2 Mo1A O3 C61 -145.4(3) . . . . ? N1 Mo1A *3 P1 -1.1(3) . . . . ? O2 Mo1A O3 P1 -131.69(11) . . . . ? O1 Mo1A O3 P1 115.32(11) . . . . ? N2 Mo1A O3 P1 -9.21(9) . . . . ? O3 P1 N2 Si1 -168.06(15) . . . . ? N3 P1 N2 Si1 86.65(18) . . . . ? O3 P1 N2 Mo1A -13.49(13) . . . . ? N3 P1 N2 Mo1A -118.78(14) . . . . ? C33 Si1 N2 P1 -145.9(2) . . . . ? C31 Si1 N2 P1 92.9(2) . . . . ? C32 Si1 N2 P1 -25.3(3) . . . . ? C33 Si1 N2 Mo1A 61.4(2) . . . . ? C31 Si1 N2 Mo1A -59.7(2) . . . . ? C32 Si1 N2 Mo1A -177.9(3) . . . . ? N1 Mo1A N2 P1 -167.56(14) . . . . ? O2 Mo1A N2 P1 80.57(15) . . . . ? O1 Mo1A N2 P1 -56.31(16) . . . . ? O3 Mo1A N2 P1 9.79(10) . . . . ? N1 Mo1A N2 Si1 -13.40(18) . . . . ? O2 Mo1A N2 Si1 -125.27(15) . . . . ? O1 Mo1A N2 Si1 97.85(16) . . . . ? O3 Mo1A N2 Si1 163.95(17) . . . . ? O3 P1 N3 Si2 -50.48(18) . . . . ? N2 P1 N3 Si2 45.4(2) . . . . ? O3 P1 N3 Si3 128.56(13) . . . . ? N2 P1 N3 Si3 -135.60(14) . . . . ? C42 Si2 N3 P1 -67.7(2) . . . . ? C43 Si2 N3 P1 56.3(2) . . . . ? C41 Si2 N3 P1 174.17(19) . . . . ? C42 Si2 N3 Si3 113.3(2) . . . . ? C43 Si2 N3 Si3 -122.63(19) . . . . ? C41 Si2 N3 Si3 -4.8(2) . . . . ? C52 Si3 N3 P1 2.7(2) . . . . ? C53 Si3 N3 P1 121.9(2) . . . . ? C51 Si3 N3 P1 -116.0(2) . . . . ? C52 Si3 N3 Si2 -178.3(2) . . . . ? C53 Si3 N3 Si2 -59.0(2) . . . . ? C51 Si3 N3 Si2 63.1(2) . . . . ? Mo1A O1 C11 C13B -18.3(9) . . . . ? Mo1A O1 C11 C14A -175.3(6) . . . . ? Mo1A O1 C11 C12A 68.8(7) . . . . ? Mo1A O1 C11 C12B 110.4(7) . . . . ? Mo1A O1 C11 C13A -50.1(6) . . . . ? Mo1A O1 C11 C14B -144.5(4) . . . . ? Mo1A O2 C21 C22 -70.1(5) . . . . ? Mo1A O2 C21 C24 169.0(4) . . . . ? Mo1A O2 C21 C23 49.7(6) . . . . ? P1 O3 C61 C63 -59.8(3) . . . . ? Mo1A O3 C61 C63 66.9(3) . . . . ? P1 O3 C61 C64 63.9(3) . . . . ? Mo1A O3 C61 C64 -169.51(19) . . . . ? P1 O3 C61 C62 -177.8(2) . . . . ? Mo1A O3 C61 C62 -51.2(3) . . . . ? 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 C23 H23A N1 0.97 2.58 3.335(6) 134.6 . C42 H42C N2 0.97 2.70 3.326(5) 122.8 . C43 H43C O2 0.97 2.55 3.474(5) 158.8 . C63 H63B O1 0.97 2.60 3.414(5) 141.9 . _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.63 _refine_diff_density_min -0.60 _refine_diff_density_rms 0.071 #===================================================================== data_7 _database_code_depnum_ccdc_archive 'CCDC 781904' #TrackingRef '- ANAT.cif' #===================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H54 Mo N3 O3 P S Si2' _chemical_formula_sum 'C22 H54 Mo N3 O3 P S Si2' _chemical_formula_weight 623.83 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 MONOCLINIC _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.557(5) _cell_length_b 11.920(3) _cell_length_c 18.590(6) _cell_angle_alpha 90.00 _cell_angle_beta 109.73(3) _cell_angle_gamma 90.00 _cell_volume 3244.9(17) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 29485 _cell_measurement_theta_min 4 _cell_measurement_theta_max 33 _exptl_crystal_description parallelepiped _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.277 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 0.617 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.870 _exptl_absorpt_correction_T_max 0.934 _exptl_absorpt_process_details 'CrysAlis RED; Oxford-Diffraction Poland, 2003' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'Xcalibur PX kappa-geometry diffractometer with Onyx CCD camera' _diffrn_measurement_method 'omega and phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47426 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_sigmaI/netI 0.0542 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 4.71 _diffrn_reflns_theta_max 32.58 _reflns_number_total 11759 _reflns_number_gt 8196 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD; Oxford-Diffraction Poland, 2003' _computing_cell_refinement 'CrysAlis RED; Oxford-Diffraction Poland, 2003' _computing_data_reduction 'CrysAlis RED; Oxford-Diffraction Poland, 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^)+(0.027P)^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 11759 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0507 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0627 _refine_ls_wR_factor_gt 0.0604 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.004 _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 0.690376(9) 0.390444(10) 0.751641(7) 0.01365(3) Uani 1 1 d . . . S1 S 0.69950(2) 0.39844(3) 0.615759(19) 0.01535(7) Uani 1 1 d . . . P1 P 0.75826(3) 0.54751(3) 0.65233(2) 0.01284(7) Uani 1 1 d . . . Si1 Si 0.88191(3) 0.63510(3) 0.57175(2) 0.01721(9) Uani 1 1 d . . . Si2 Si 0.94536(3) 0.45426(3) 0.69553(2) 0.01737(9) Uani 1 1 d . . . O1 O 0.74971(7) 0.39210(8) 0.85873(5) 0.0184(2) Uani 1 1 d . . . O2 O 0.69142(7) 0.23421(8) 0.73596(5) 0.0162(2) Uani 1 1 d . . . O3 O 0.71122(7) 0.64782(8) 0.59692(5) 0.0161(2) Uani 1 1 d . . . N1 N 0.58230(9) 0.41999(10) 0.73686(7) 0.0200(3) Uani 1 1 d . . . N2 N 0.75111(8) 0.55087(9) 0.73615(6) 0.0142(2) Uani 1 1 d . . . N3 N 0.86319(8) 0.55875(9) 0.64829(6) 0.0139(2) Uani 1 1 d . . . C11 C 0.72951(12) 0.36272(13) 0.92700(8) 0.0229(3) Uani 1 1 d . . . C12 C 0.73086(14) 0.23620(14) 0.93143(10) 0.0373(5) Uani 1 1 d . . . H12A H 0.6809 0.2057 0.8882 0.056 Uiso 1 1 calc R . . H12B H 0.7233 0.2125 0.9794 0.056 Uiso 1 1 calc R . . H12C H 0.7893 0.2083 0.9295 0.056 Uiso 1 1 calc R . . C13 C 0.80523(14) 0.41254(17) 0.99398(10) 0.0430(5) Uani 1 1 d . . . H13A H 0.8645 0.3869 0.9926 0.064 Uiso 1 1 calc R . . H13B H 0.7978 0.3883 1.0419 0.064 Uiso 1 1 calc R . . H13C H 0.8023 0.4946 0.9907 0.064 Uiso 1 1 calc R . . C14 C 0.63622(14) 0.40774(17) 0.92306(11) 0.0405(5) Uani 1 1 d . . . H14A H 0.6377 0.4899 0.9237 0.061 Uiso 1 1 calc R . . H14B H 0.6213 0.3804 0.9671 0.061 Uiso 1 1 calc R . . H14C H 0.5898 0.3819 0.8758 0.061 Uiso 1 1 calc R . . C21 C 0.63082(11) 0.14014(12) 0.70705(8) 0.0186(3) Uani 1 1 d . . . C22 C 0.53795(12) 0.16204(14) 0.71223(12) 0.0348(4) Uani 1 1 d . . . H22A H 0.5440 0.1791 0.7653 0.052 Uiso 1 1 calc R . . H22B H 0.4995 0.0954 0.6952 0.052 Uiso 1 1 calc R . . H22C H 0.5098 0.2259 0.6796 0.052 Uiso 1 1 calc R . . C23 C 0.67597(12) 0.03937(13) 0.75516(10) 0.0324(4) Uani 1 1 d . . . H23A H 0.7371 0.0287 0.7522 0.049 Uiso 1 1 calc R . . H23B H 0.6391 -0.0278 0.7359 0.049 Uiso 1 1 calc R . . H23C H 0.6808 0.0523 0.8084 0.049 Uiso 1 1 calc R . . C24 C 0.62460(14) 0.12262(14) 0.62420(10) 0.0360(4) Uani 1 1 d . . . H24A H 0.5981 0.1895 0.5943 0.054 Uiso 1 1 calc R . . H24B H 0.5859 0.0575 0.6031 0.054 Uiso 1 1 calc R . . H24C H 0.6859 0.1096 0.6220 0.054 Uiso 1 1 calc R . . C31 C 0.78186(10) 0.64538(11) 0.79399(8) 0.0157(3) Uani 1 1 d . . . C32 C 0.70624(11) 0.66801(13) 0.82743(9) 0.0241(3) Uani 1 1 d . . . H32A H 0.6941 0.5996 0.8516 0.036 Uiso 1 1 calc R . . H32B H 0.6506 0.6911 0.7865 0.036 Uiso 1 1 calc R . . H32C H 0.7256 0.7278 0.8657 0.036 Uiso 1 1 calc R . . C33 C 0.79881(11) 0.75446(12) 0.75633(8) 0.0222(3) Uani 1 1 d . . . H33A H 0.8187 0.8136 0.7950 0.033 Uiso 1 1 calc R . . H33B H 0.7422 0.7776 0.7164 0.033 Uiso 1 1 calc R . . H33C H 0.8463 0.7415 0.7336 0.033 Uiso 1 1 calc R . . C34 C 0.86961(11) 0.61264(13) 0.85680(8) 0.0218(3) Uani 1 1 d . . . H34A H 0.8607 0.5413 0.8796 0.033 Uiso 1 1 calc R . . H34B H 0.8861 0.6711 0.8962 0.033 Uiso 1 1 calc R . . H34C H 0.9187 0.6044 0.8352 0.033 Uiso 1 1 calc R . . C41 C 0.85480(12) 0.78746(12) 0.57111(9) 0.0241(3) Uani 1 1 d . . . H41A H 0.7933 0.8012 0.5349 0.036 Uiso 1 1 calc R . . H41B H 0.8993 0.8307 0.5557 0.036 Uiso 1 1 calc R . . H41C H 0.8576 0.8107 0.6224 0.036 Uiso 1 1 calc R . . C42 C 1.00534(11) 0.63340(13) 0.58062(9) 0.0257(4) Uani 1 1 d . . . H42A H 1.0413 0.6725 0.6275 0.038 Uiso 1 1 calc R . . H42B H 1.0130 0.6713 0.5364 0.038 Uiso 1 1 calc R . . H42C H 1.0264 0.5556 0.5826 0.038 Uiso 1 1 calc R . . C43 C 0.81802(12) 0.56717(14) 0.47869(9) 0.0253(4) Uani 1 1 d . . . H43A H 0.8386 0.4894 0.4791 0.038 Uiso 1 1 calc R . . H43B H 0.8294 0.6082 0.4371 0.038 Uiso 1 1 calc R . . H43C H 0.7525 0.5682 0.4709 0.038 Uiso 1 1 calc R . . C51 C 0.95966(12) 0.35626(13) 0.62215(9) 0.0270(4) Uani 1 1 d . . . H51A H 0.9001 0.3253 0.5918 0.040 Uiso 1 1 calc R . . H51B H 1.0008 0.2950 0.6476 0.040 Uiso 1 1 calc R . . H51C H 0.9857 0.3970 0.5885 0.040 Uiso 1 1 calc R . . C52 C 0.91357(11) 0.36136(13) 0.76245(9) 0.0225(3) Uani 1 1 d . . . H52A H 0.8985 0.4071 0.8004 0.034 Uiso 1 1 calc R . . H52B H 0.9650 0.3118 0.7885 0.034 Uiso 1 1 calc R . . H52C H 0.8605 0.3160 0.7339 0.034 Uiso 1 1 calc R . . C53 C 1.05419(11) 0.52380(13) 0.75348(9) 0.0255(4) Uani 1 1 d . . . H53A H 1.0826 0.5585 0.7193 0.038 Uiso 1 1 calc R . . H53B H 1.0958 0.4678 0.7856 0.038 Uiso 1 1 calc R . . H53C H 1.0413 0.5816 0.7860 0.038 Uiso 1 1 calc R . . C61 C 0.61211(10) 0.67561(12) 0.55956(9) 0.0209(3) Uani 1 1 d . . . C62 C 0.61163(12) 0.80201(14) 0.54755(11) 0.0360(4) Uani 1 1 d . . . H62A H 0.6398 0.8393 0.5969 0.054 Uiso 1 1 calc R . . H62B H 0.5485 0.8281 0.5243 0.054 Uiso 1 1 calc R . . H62C H 0.6462 0.8199 0.5137 0.054 Uiso 1 1 calc R . . C63 C 0.55722(11) 0.64499(14) 0.61008(9) 0.0264(4) Uani 1 1 d . . . H63A H 0.5625 0.5642 0.6205 0.040 Uiso 1 1 calc R . . H63B H 0.4930 0.6645 0.5841 0.040 Uiso 1 1 calc R . . H63C H 0.5806 0.6864 0.6583 0.040 Uiso 1 1 calc R . . C64 C 0.57880(11) 0.61464(14) 0.48345(9) 0.0279(4) Uani 1 1 d . . . H64A H 0.6137 0.6401 0.4514 0.042 Uiso 1 1 calc R . . H64B H 0.5138 0.6307 0.4577 0.042 Uiso 1 1 calc R . . H64C H 0.5873 0.5337 0.4921 0.042 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 0.01605(6) 0.01250(6) 0.01427(6) 0.00022(5) 0.00756(5) -0.00103(5) S1 0.01966(18) 0.01346(16) 0.01391(16) -0.00109(13) 0.00695(14) -0.00225(14) P1 0.01386(18) 0.01183(16) 0.01339(17) 0.00115(13) 0.00535(14) 0.00083(13) Si1 0.0214(2) 0.0174(2) 0.0157(2) 0.00129(15) 0.00995(17) -0.00081(16) Si2 0.0164(2) 0.0170(2) 0.0194(2) 0.00210(15) 0.00704(17) 0.00371(16) O1 0.0242(6) 0.0187(5) 0.0141(5) 0.0007(4) 0.0089(4) -0.0035(4) O2 0.0182(5) 0.0132(5) 0.0183(5) 0.0001(4) 0.0074(4) -0.0014(4) O3 0.0148(5) 0.0148(5) 0.0174(5) 0.0034(4) 0.0036(4) 0.0013(4) N1 0.0206(7) 0.0173(6) 0.0247(7) -0.0008(5) 0.0111(6) -0.0006(5) N2 0.0169(6) 0.0123(5) 0.0150(6) -0.0017(4) 0.0075(5) -0.0015(5) N3 0.0138(6) 0.0149(6) 0.0148(6) 0.0020(4) 0.0072(5) 0.0013(5) C11 0.0321(9) 0.0255(8) 0.0138(7) 0.0014(6) 0.0111(7) -0.0045(7) C12 0.0616(14) 0.0282(9) 0.0277(9) 0.0048(7) 0.0225(9) -0.0067(9) C13 0.0578(14) 0.0522(13) 0.0185(9) -0.0039(8) 0.0123(9) -0.0224(10) C14 0.0497(13) 0.0523(12) 0.0312(10) 0.0093(8) 0.0289(10) 0.0064(10) C21 0.0231(8) 0.0126(7) 0.0205(8) -0.0021(5) 0.0080(6) -0.0041(6) C22 0.0243(9) 0.0252(9) 0.0580(12) -0.0084(8) 0.0180(9) -0.0068(7) C23 0.0398(11) 0.0148(7) 0.0385(10) 0.0051(7) 0.0080(9) -0.0030(7) C24 0.0572(13) 0.0252(9) 0.0268(9) -0.0064(7) 0.0159(9) -0.0117(8) C31 0.0193(8) 0.0134(6) 0.0169(7) -0.0039(5) 0.0094(6) -0.0039(5) C32 0.0257(9) 0.0236(8) 0.0275(9) -0.0088(6) 0.0148(7) -0.0032(7) C33 0.0301(9) 0.0145(7) 0.0232(8) -0.0036(6) 0.0104(7) -0.0042(6) C34 0.0246(8) 0.0214(7) 0.0195(7) -0.0037(6) 0.0077(6) -0.0062(7) C41 0.0305(9) 0.0177(7) 0.0267(8) 0.0047(6) 0.0131(7) -0.0022(6) C42 0.0251(9) 0.0297(9) 0.0295(9) -0.0020(7) 0.0188(7) -0.0032(7) C43 0.0315(10) 0.0285(8) 0.0186(8) -0.0009(6) 0.0118(7) -0.0015(7) C51 0.0295(9) 0.0233(8) 0.0297(9) -0.0012(7) 0.0122(8) 0.0073(7) C52 0.0211(8) 0.0207(8) 0.0232(8) 0.0054(6) 0.0041(7) 0.0073(6) C53 0.0207(8) 0.0274(9) 0.0273(9) 0.0028(7) 0.0067(7) 0.0009(7) C61 0.0141(7) 0.0194(7) 0.0259(8) 0.0049(6) 0.0022(6) 0.0056(6) C62 0.0259(10) 0.0219(9) 0.0505(12) 0.0111(8) 0.0001(9) 0.0065(7) C63 0.0167(8) 0.0331(9) 0.0291(9) 0.0032(7) 0.0071(7) 0.0058(7) C64 0.0211(8) 0.0352(9) 0.0225(8) 0.0047(7) 0.0007(7) 0.0036(7) _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 N1 1.6476(14) . ? Mo1 O2 1.8859(11) . ? Mo1 O1 1.8907(12) . ? Mo1 N2 2.1946(12) . ? Mo1 S1 2.5792(9) . ? S1 P1 2.0089(7) . ? P1 O3 1.5866(10) . ? P1 N2 1.5998(13) . ? P1 N3 1.6647(13) . ? Si1 N3 1.7937(12) . ? Si1 C41 1.8635(16) . ? Si1 C43 1.8642(17) . ? Si1 C42 1.8712(18) . ? Si2 N3 1.7884(13) . ? Si2 C52 1.8532(16) . ? Si2 C51 1.8654(16) . ? Si2 C53 1.8663(17) . ? O1 C11 1.4496(17) . ? O2 C21 1.4467(17) . ? O3 C61 1.4987(18) . ? N2 C31 1.5187(18) . ? C11 C12 1.510(2) . ? C11 C13 1.517(2) . ? C11 C14 1.526(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C21 C22 1.503(2) . ? C21 C23 1.520(2) . ? C21 C24 1.525(2) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C31 C34 1.518(2) . ? C31 C32 1.529(2) . ? C31 C33 1.541(2) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C61 C63 1.512(2) . ? C61 C64 1.518(2) . ? C61 C62 1.523(2) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 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 N1 Mo1 O2 104.29(5) . . ? N1 Mo1 O1 106.34(6) . . ? O2 Mo1 O1 98.42(4) . . ? N1 Mo1 N2 104.61(5) . . ? O2 Mo1 N2 144.45(4) . . ? O1 Mo1 N2 92.88(4) . . ? N1 Mo1 S1 102.66(5) . . ? O2 Mo1 S1 83.04(3) . . ? O1 Mo1 S1 149.56(4) . . ? N2 Mo1 S1 70.78(3) . . ? P1 S1 Mo1 82.56(2) . . ? O3 P1 N2 116.43(6) . . ? O3 P1 N3 98.89(6) . . ? N2 P1 N3 115.70(7) . . ? O3 P1 S1 112.92(5) . . ? N2 P1 S1 100.28(5) . . ? N3 P1 S1 113.39(5) . . ? N3 Si1 C41 113.74(7) . . ? N3 Si1 C43 109.71(7) . . ? C41 Si1 C43 111.64(8) . . ? N3 Si1 C42 111.17(7) . . ? C41 Si1 C42 103.56(7) . . ? C43 Si1 C42 106.67(8) . . ? N3 Si2 C52 115.93(7) . . ? N3 Si2 C51 108.60(7) . . ? C52 Si2 C51 103.97(8) . . ? N3 Si2 C53 109.45(7) . . ? C52 Si2 C53 105.88(8) . . ? C51 Si2 C53 113.04(8) . . ? C11 O1 Mo1 138.27(10) . . ? C21 O2 Mo1 141.66(9) . . ? C61 O3 P1 130.11(9) . . ? C31 N2 P1 126.82(9) . . ? C31 N2 Mo1 126.88(9) . . ? P1 N2 Mo1 106.29(6) . . ? P1 N3 Si2 118.10(7) . . ? P1 N3 Si1 120.06(7) . . ? Si2 N3 Si1 117.54(7) . . ? O1 C11 C12 106.61(12) . . ? O1 C11 C13 106.64(13) . . ? C12 C11 C13 110.71(15) . . ? O1 C11 C14 110.90(13) . . ? C12 C11 C14 110.45(15) . . ? C13 C11 C14 111.36(15) . . ? 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 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O2 C21 C22 111.19(12) . . ? O2 C21 C23 106.27(12) . . ? C22 C21 C23 111.26(14) . . ? O2 C21 C24 107.02(12) . . ? C22 C21 C24 110.73(15) . . ? C23 C21 C24 110.20(13) . . ? 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 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C34 C31 N2 109.91(12) . . ? C34 C31 C32 110.39(13) . . ? N2 C31 C32 108.49(12) . . ? C34 C31 C33 108.60(12) . . ? N2 C31 C33 111.44(11) . . ? C32 C31 C33 108.00(12) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si1 C41 H41A 109.5 . . ? Si1 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? Si1 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? Si1 C42 H42A 109.5 . . ? Si1 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? Si1 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? Si1 C43 H43A 109.5 . . ? Si1 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? Si1 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? Si2 C51 H51A 109.5 . . ? Si2 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? Si2 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? Si2 C52 H52A 109.5 . . ? Si2 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? Si2 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? Si2 C53 H53A 109.5 . . ? Si2 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? Si2 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? O3 C61 C63 111.54(12) . . ? O3 C61 C64 107.47(12) . . ? C63 C61 C64 112.13(14) . . ? O3 C61 C62 103.89(12) . . ? C63 C61 C62 110.74(14) . . ? C64 C61 C62 110.73(14) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 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 N1 Mo1 S1 P1 103.02(5) . . . . ? O2 Mo1 S1 P1 -153.83(3) . . . . ? O1 Mo1 S1 P1 -59.04(6) . . . . ? N2 Mo1 S1 P1 1.75(4) . . . . ? Mo1 S1 P1 O3 -126.90(5) . . . . ? Mo1 S1 P1 N2 -2.30(5) . . . . ? Mo1 S1 P1 N3 121.65(5) . . . . ? N1 Mo1 O1 C11 35.05(15) . . . . ? O2 Mo1 O1 C11 -72.61(14) . . . . ? N2 Mo1 O1 C11 141.19(14) . . . . ? S1 Mo1 O1 C11 -163.20(11) . . . . ? N1 Mo1 O2 C21 10.97(15) . . . . ? O1 Mo1 O2 C21 120.31(14) . . . . ? N2 Mo1 O2 C21 -132.56(13) . . . . ? S1 Mo1 O2 C21 -90.39(14) . . . . ? N2 P1 O3 C61 -69.51(13) . . . . ? N3 P1 O3 C61 165.90(11) . . . . ? S1 P1 O3 C61 45.74(12) . . . . ? O3 P1 N2 C31 -56.08(14) . . . . ? N3 P1 N2 C31 59.43(13) . . . . ? S1 P1 N2 C31 -178.22(11) . . . . ? O3 P1 N2 Mo1 124.94(6) . . . . ? N3 P1 N2 Mo1 -119.55(6) . . . . ? S1 P1 N2 Mo1 2.80(6) . . . . ? N1 Mo1 N2 C31 80.18(12) . . . . ? O2 Mo1 N2 C31 -136.36(10) . . . . ? O1 Mo1 N2 C31 -27.53(11) . . . . ? S1 Mo1 N2 C31 178.75(11) . . . . ? N1 Mo1 N2 P1 -100.84(8) . . . . ? O2 Mo1 N2 P1 42.62(11) . . . . ? O1 Mo1 N2 P1 151.45(6) . . . . ? S1 Mo1 N2 P1 -2.27(5) . . . . ? O3 P1 N3 Si2 -174.44(7) . . . . ? N2 P1 N3 Si2 60.45(9) . . . . ? S1 P1 N3 Si2 -54.63(8) . . . . ? O3 P1 N3 Si1 -18.28(8) . . . . ? N2 P1 N3 Si1 -143.39(7) . . . . ? S1 P1 N3 Si1 101.53(7) . . . . ? C52 Si2 N3 P1 -13.18(10) . . . . ? C51 Si2 N3 P1 103.36(9) . . . . ? C53 Si2 N3 P1 -132.81(8) . . . . ? C52 Si2 N3 Si1 -169.94(7) . . . . ? C51 Si2 N3 Si1 -53.39(10) . . . . ? C53 Si2 N3 Si1 70.44(9) . . . . ? C41 Si1 N3 P1 64.09(10) . . . . ? C43 Si1 N3 P1 -61.75(10) . . . . ? C42 Si1 N3 P1 -179.49(8) . . . . ? C41 Si1 N3 Si2 -139.63(8) . . . . ? C43 Si1 N3 Si2 94.54(9) . . . . ? C42 Si1 N3 Si2 -23.21(9) . . . . ? Mo1 O1 C11 C12 74.22(18) . . . . ? Mo1 O1 C11 C13 -167.46(12) . . . . ? Mo1 O1 C11 C14 -46.1(2) . . . . ? Mo1 O2 C21 C22 -25.1(2) . . . . ? Mo1 O2 C21 C23 -146.36(12) . . . . ? Mo1 O2 C21 C24 95.90(16) . . . . ? P1 N2 C31 C34 -105.31(13) . . . . ? Mo1 N2 C31 C34 73.47(14) . . . . ? P1 N2 C31 C32 133.91(12) . . . . ? Mo1 N2 C31 C32 -47.31(15) . . . . ? P1 N2 C31 C33 15.14(18) . . . . ? Mo1 N2 C31 C33 -166.09(10) . . . . ? P1 O3 C61 C63 34.20(17) . . . . ? P1 O3 C61 C64 -89.09(14) . . . . ? P1 O3 C61 C62 153.53(11) . . . . ? 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 C12 H12B S1 0.98 2.99 3.9604(19) 170.5 4_566 C24 H24A S1 0.98 2.90 3.5094(19) 121.0 . C63 H63A S1 0.98 2.93 3.6591(18) 132.0 . C64 H64C S1 0.98 2.87 3.6191(19) 134.2 . C52 H52C S1 0.98 2.89 3.548(2) 125.5 . C14 H14C N1 0.98 2.59 3.278(2) 127.7 . C22 H22C N1 0.98 2.64 3.151(2) 113.0 . C34 H34A O1 0.98 2.42 3.2306(19) 140.1 . _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.95 _refine_diff_density_min -0.47 _refine_diff_density_rms 0.075 #===================================================================== data_8 _database_code_depnum_ccdc_archive 'CCDC 781905' #TrackingRef '- ANAT.cif' #===================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H63 Mo N4 O3 P Si4' _chemical_formula_sum 'C24 H63 Mo N4 O3 P Si4' _chemical_formula_weight 695.05 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 orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' 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' '-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 19.393(6) _cell_length_b 17.061(5) _cell_length_c 22.629(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7487(4) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 24827 _cell_measurement_theta_min 4 _cell_measurement_theta_max 33 _exptl_crystal_description parallelepiped _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.233 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2976 _exptl_absorpt_coefficient_mu 0.549 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.887 _exptl_absorpt_correction_T_max 0.940 _exptl_absorpt_process_details 'CrysAlis RED; Oxford-Diffraction Poland, 2003' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'Xcalibur PX kappa-geometry diffractometer with Onyx CCD camera' _diffrn_measurement_method 'omega and phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 76981 _diffrn_reflns_av_R_equivalents 0.1057 _diffrn_reflns_av_sigmaI/netI 0.1007 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 4.15 _diffrn_reflns_theta_max 32.60 _reflns_number_total 13606 _reflns_number_gt 7164 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD; Oxford-Diffraction Poland, 2003' _computing_cell_refinement 'CrysAlis RED; Oxford-Diffraction Poland, 2003' _computing_data_reduction 'CrysAlis RED; Oxford-Diffraction Poland, 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^)+(0.0350P)^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 13606 _refine_ls_number_parameters 360 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1211 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1006 _refine_ls_wR_factor_gt 0.0864 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.572381(11) 0.257613(11) 0.643968(10) 0.01835(6) Uani 0.9758(10) 1 d P . . Mo1B Mo 0.5700(4) 0.2530(5) 0.6089(4) 0.017(3) Uiso 0.0242(10) 1 d P . . P1 P 0.42467(3) 0.28461(3) 0.63077(2) 0.01887(13) Uani 1 1 d . . . Si1 Si 0.47309(4) 0.28139(4) 0.76324(3) 0.02621(16) Uani 1 1 d . . . Si2 Si 0.35252(4) 0.13135(4) 0.64507(3) 0.03028(17) Uani 1 1 d . . . Si3 Si 0.26997(4) 0.28446(5) 0.63691(3) 0.03014(17) Uani 1 1 d . . . Si4 Si 0.47224(4) 0.24386(4) 0.50242(3) 0.02655(16) Uani 1 1 d . . . O1 O 0.60784(9) 0.34367(9) 0.60260(7) 0.0233(4) Uani 1 1 d . . . O2 O 0.59432(9) 0.16138(10) 0.60829(7) 0.0281(4) Uani 1 1 d . . . O3 O 0.39145(9) 0.36994(9) 0.62954(7) 0.0266(4) Uani 1 1 d . . . N1 N 0.62106(11) 0.25462(12) 0.70441(8) 0.0278(5) Uani 1 1 d . . . N2 N 0.48036(10) 0.27682(11) 0.68569(8) 0.0196(4) Uani 1 1 d . . . N3 N 0.35155(10) 0.23586(12) 0.64241(8) 0.0238(4) Uani 1 1 d . . . N4 N 0.47009(10) 0.26126(11) 0.57668(8) 0.0204(4) Uani 1 1 d . . . C11 C 0.66777(14) 0.39489(15) 0.60739(11) 0.0287(6) Uani 1 1 d . . . C12 C 0.73168(16) 0.34516(19) 0.60544(18) 0.0599(10) Uani 1 1 d . . . H12A H 0.7306 0.3073 0.6380 0.090 Uiso 1 1 calc R . . H12B H 0.7725 0.3787 0.6094 0.090 Uiso 1 1 calc R . . H12C H 0.7336 0.3171 0.5677 0.090 Uiso 1 1 calc R . . C13 C 0.66358(18) 0.44147(19) 0.66443(13) 0.0521(9) Uani 1 1 d . . . H13A H 0.6240 0.4772 0.6627 0.078 Uiso 1 1 calc R . . H13B H 0.7060 0.4719 0.6696 0.078 Uiso 1 1 calc R . . H13C H 0.6580 0.4055 0.6978 0.078 Uiso 1 1 calc R . . C14 C 0.66425(16) 0.44853(17) 0.55423(12) 0.0430(8) Uani 1 1 d . . . H14A H 0.6632 0.4170 0.5180 0.064 Uiso 1 1 calc R . . H14B H 0.7048 0.4827 0.5537 0.064 Uiso 1 1 calc R . . H14C H 0.6224 0.4806 0.5565 0.064 Uiso 1 1 calc R . . C21 C 0.64387(15) 0.09943(15) 0.62056(13) 0.0345(7) Uani 1 1 d . . . C22 C 0.71583(15) 0.13332(18) 0.61840(14) 0.0435(8) Uani 1 1 d . . . H22A H 0.7228 0.1600 0.5805 0.065 Uiso 1 1 calc R . . H22B H 0.7497 0.0910 0.6225 0.065 Uiso 1 1 calc R . . H22C H 0.7217 0.1709 0.6508 0.065 Uiso 1 1 calc R . . C23 C 0.62851(16) 0.06369(17) 0.68138(14) 0.0479(8) Uani 1 1 d . . . H23A H 0.6317 0.1045 0.7117 0.072 Uiso 1 1 calc R . . H23B H 0.6621 0.0223 0.6899 0.072 Uiso 1 1 calc R . . H23C H 0.5819 0.0414 0.6814 0.072 Uiso 1 1 calc R . . C24 C 0.63320(18) 0.03968(18) 0.57148(16) 0.0567(9) Uani 1 1 d . . . H24A H 0.5862 0.0189 0.5736 0.085 Uiso 1 1 calc R . . H24B H 0.6663 -0.0033 0.5761 0.085 Uiso 1 1 calc R . . H24C H 0.6403 0.0650 0.5331 0.085 Uiso 1 1 calc R . . C31 C 0.38481(15) 0.30799(18) 0.78635(11) 0.0412(7) Uani 1 1 d . . . H31A H 0.3740 0.3609 0.7723 0.062 Uiso 1 1 calc R . . H31B H 0.3817 0.3065 0.8296 0.062 Uiso 1 1 calc R . . H31C H 0.3519 0.2706 0.7694 0.062 Uiso 1 1 calc R . . C32 C 0.49386(15) 0.18336(16) 0.79521(11) 0.0360(7) Uani 1 1 d . . . H32A H 0.4599 0.1449 0.7816 0.054 Uiso 1 1 calc R . . H32B H 0.4926 0.1864 0.8384 0.054 Uiso 1 1 calc R . . H32C H 0.5400 0.1673 0.7824 0.054 Uiso 1 1 calc R . . C33 C 0.53272(16) 0.35549(17) 0.79586(11) 0.0409(7) Uani 1 1 d . . . H33A H 0.5799 0.3452 0.7823 0.061 Uiso 1 1 calc R . . H33B H 0.5310 0.3521 0.8391 0.061 Uiso 1 1 calc R . . H33C H 0.5186 0.4081 0.7834 0.061 Uiso 1 1 calc R . . C41 C 0.44068(15) 0.08975(15) 0.64734(13) 0.0379(7) Uani 1 1 d . . . H41A H 0.4643 0.1078 0.6831 0.057 Uiso 1 1 calc R . . H41B H 0.4665 0.1070 0.6124 0.057 Uiso 1 1 calc R . . H41C H 0.4380 0.0324 0.6477 0.057 Uiso 1 1 calc R . . C42 C 0.30963(16) 0.09595(18) 0.71398(13) 0.0466(8) Uani 1 1 d . . . H42A H 0.3303 0.1219 0.7483 0.070 Uiso 1 1 calc R . . H42B H 0.3158 0.0391 0.7175 0.070 Uiso 1 1 calc R . . H42C H 0.2603 0.1082 0.7123 0.070 Uiso 1 1 calc R . . C43 C 0.31100(15) 0.09078(17) 0.57725(13) 0.0433(8) Uani 1 1 d . . . H43A H 0.2622 0.1055 0.5766 0.065 Uiso 1 1 calc R . . H43B H 0.3151 0.0335 0.5773 0.065 Uiso 1 1 calc R . . H43C H 0.3340 0.1120 0.5422 0.065 Uiso 1 1 calc R . . C51 C 0.19676(15) 0.2155(2) 0.64992(14) 0.0503(8) Uani 1 1 d . . . H51A H 0.2026 0.1689 0.6251 0.075 Uiso 1 1 calc R . . H51B H 0.1532 0.2415 0.6398 0.075 Uiso 1 1 calc R . . H51C H 0.1960 0.2000 0.6916 0.075 Uiso 1 1 calc R . . C52 C 0.25288(15) 0.36156(17) 0.69353(12) 0.0382(7) Uani 1 1 d . . . H52A H 0.2451 0.3368 0.7320 0.057 Uiso 1 1 calc R . . H52B H 0.2119 0.3916 0.6822 0.057 Uiso 1 1 calc R . . H52C H 0.2927 0.3968 0.6961 0.057 Uiso 1 1 calc R . . C53 C 0.25532(17) 0.3239(2) 0.56107(12) 0.0507(9) Uani 1 1 d . . . H53A H 0.2936 0.3586 0.5502 0.076 Uiso 1 1 calc R . . H53B H 0.2120 0.3535 0.5603 0.076 Uiso 1 1 calc R . . H53C H 0.2527 0.2804 0.5329 0.076 Uiso 1 1 calc R . . C61 C 0.42311(15) 0.44821(14) 0.62022(11) 0.0306(6) Uani 1 1 d . . . C62 C 0.46626(19) 0.46957(17) 0.67313(13) 0.0521(9) Uani 1 1 d . . . H62A H 0.4382 0.4653 0.7090 0.078 Uiso 1 1 calc R . . H62B H 0.4830 0.5235 0.6689 0.078 Uiso 1 1 calc R . . H62C H 0.5057 0.4338 0.6759 0.078 Uiso 1 1 calc R . . C63 C 0.46451(15) 0.45008(16) 0.56373(12) 0.0369(7) Uani 1 1 d . . . H63A H 0.5039 0.4144 0.5672 0.055 Uiso 1 1 calc R . . H63B H 0.4812 0.5035 0.5566 0.055 Uiso 1 1 calc R . . H63C H 0.4353 0.4335 0.5307 0.055 Uiso 1 1 calc R . . C64 C 0.36135(17) 0.50316(18) 0.61523(16) 0.0563(10) Uani 1 1 d . . . H64A H 0.3316 0.4859 0.5827 0.085 Uiso 1 1 calc R . . H64B H 0.3775 0.5566 0.6075 0.085 Uiso 1 1 calc R . . H64C H 0.3352 0.5022 0.6523 0.085 Uiso 1 1 calc R . . C71 C 0.39540(17) 0.2806(2) 0.46144(12) 0.0546(9) Uani 1 1 d . . . H71A H 0.3545 0.2508 0.4735 0.082 Uiso 1 1 calc R . . H71B H 0.4028 0.2740 0.4189 0.082 Uiso 1 1 calc R . . H71C H 0.3884 0.3362 0.4704 0.082 Uiso 1 1 calc R . . C72 C 0.55095(15) 0.28962(19) 0.47062(11) 0.0400(7) Uani 1 1 d . . . H72A H 0.5474 0.3468 0.4736 0.060 Uiso 1 1 calc R . . H72B H 0.5554 0.2745 0.4290 0.060 Uiso 1 1 calc R . . H72C H 0.5916 0.2717 0.4925 0.060 Uiso 1 1 calc R . . C73 C 0.47908(19) 0.13684(18) 0.48622(12) 0.0524(9) Uani 1 1 d . . . H73A H 0.5197 0.1153 0.5062 0.079 Uiso 1 1 calc R . . H73B H 0.4836 0.1290 0.4435 0.079 Uiso 1 1 calc R . . H73C H 0.4376 0.1100 0.5004 0.079 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 0.02066(10) 0.01805(10) 0.01636(11) -0.00013(8) -0.00049(9) 0.00114(9) P1 0.0210(3) 0.0204(3) 0.0152(3) 0.0013(2) 0.0009(3) 0.0006(3) Si1 0.0344(4) 0.0299(4) 0.0143(3) 0.0007(3) 0.0008(3) 0.0041(3) Si2 0.0326(4) 0.0272(4) 0.0310(4) 0.0020(3) 0.0030(4) -0.0079(3) Si3 0.0214(4) 0.0433(4) 0.0258(4) 0.0008(3) 0.0014(3) -0.0009(3) Si4 0.0271(4) 0.0382(4) 0.0143(3) -0.0044(3) 0.0021(3) -0.0046(3) O1 0.0233(10) 0.0223(9) 0.0241(8) 0.0028(7) -0.0024(8) -0.0020(7) O2 0.0319(11) 0.0195(9) 0.0328(9) -0.0035(7) 0.0001(8) 0.0052(7) O3 0.0303(10) 0.0234(9) 0.0259(8) 0.0068(7) 0.0044(8) 0.0031(7) N1 0.0278(12) 0.0312(12) 0.0244(10) 0.0022(9) -0.0046(9) 0.0033(10) N2 0.0235(11) 0.0211(10) 0.0142(8) -0.0010(7) -0.0004(8) 0.0022(8) N3 0.0196(10) 0.0294(11) 0.0224(9) 0.0003(9) 0.0003(8) -0.0008(8) N4 0.0209(10) 0.0235(10) 0.0168(8) 0.0007(8) 0.0018(8) 0.0003(8) C11 0.0267(15) 0.0269(14) 0.0324(13) 0.0062(11) -0.0033(12) -0.0089(11) C12 0.0296(19) 0.047(2) 0.103(3) 0.0140(19) -0.0040(19) -0.0097(15) C13 0.071(2) 0.052(2) 0.0335(15) -0.0005(14) -0.0061(16) -0.0287(18) C14 0.0476(19) 0.0444(19) 0.0370(15) 0.0148(13) -0.0058(14) -0.0199(14) C21 0.0348(17) 0.0201(14) 0.0486(16) 0.0006(12) 0.0052(14) 0.0122(12) C22 0.0317(18) 0.0401(18) 0.059(2) 0.0060(15) 0.0024(15) 0.0127(13) C23 0.047(2) 0.0329(17) 0.064(2) 0.0174(15) 0.0084(17) 0.0142(14) C24 0.063(2) 0.0311(18) 0.076(2) -0.0166(16) -0.003(2) 0.0149(15) C31 0.0482(19) 0.0527(19) 0.0228(13) 0.0050(13) 0.0075(13) 0.0127(15) C32 0.0472(19) 0.0376(17) 0.0232(12) 0.0080(11) -0.0006(13) 0.0023(13) C33 0.060(2) 0.0399(17) 0.0229(12) -0.0054(12) -0.0035(14) 0.0011(15) C41 0.0463(19) 0.0239(13) 0.0434(16) 0.0043(12) 0.0013(15) -0.0035(12) C42 0.048(2) 0.0454(19) 0.0461(17) 0.0143(14) 0.0082(16) -0.0089(15) C43 0.0399(19) 0.0415(18) 0.0484(17) -0.0104(14) 0.0035(15) -0.0161(14) C51 0.0281(16) 0.063(2) 0.059(2) -0.0083(17) 0.0053(16) -0.0085(15) C52 0.0317(16) 0.0479(18) 0.0349(14) 0.0006(13) 0.0087(13) 0.0056(13) C53 0.0395(19) 0.081(2) 0.0321(15) 0.0056(16) -0.0025(14) 0.0155(17) C61 0.0385(17) 0.0190(13) 0.0344(13) 0.0047(10) 0.0080(13) 0.0051(12) C62 0.086(3) 0.0257(16) 0.0447(17) -0.0044(13) -0.0074(18) -0.0059(16) C63 0.0407(17) 0.0315(16) 0.0386(15) 0.0116(12) 0.0077(14) 0.0006(13) C64 0.057(2) 0.0321(18) 0.080(2) 0.0207(16) 0.0262(19) 0.0187(15) C71 0.045(2) 0.096(3) 0.0227(13) -0.0064(16) -0.0064(14) 0.0045(18) C72 0.0419(18) 0.0563(19) 0.0218(12) -0.0037(13) 0.0049(12) -0.0088(14) C73 0.078(3) 0.047(2) 0.0320(15) -0.0148(14) 0.0094(17) -0.0128(17) _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 N1 1.663(2) . ? Mo1 O1 1.8722(16) . ? Mo1 O2 1.8785(17) . ? Mo1 N2 2.0453(19) . ? Mo1 N4 2.5016(19) . ? Mo1 P1 2.9167(11) . ? P1 N4 1.5598(19) . ? P1 O3 1.5923(17) . ? P1 N2 1.6518(19) . ? P1 N3 1.665(2) . ? Si1 N2 1.7624(19) . ? Si1 C31 1.847(3) . ? Si1 C33 1.866(3) . ? Si1 C32 1.866(3) . ? Si2 N3 1.784(2) . ? Si2 C41 1.852(3) . ? Si2 C43 1.866(3) . ? Si2 C42 1.868(3) . ? Si3 N3 1.791(2) . ? Si3 C53 1.865(3) . ? Si3 C52 1.866(3) . ? Si3 C51 1.867(3) . ? Si4 N4 1.7069(19) . ? Si4 C72 1.860(3) . ? Si4 C71 1.864(3) . ? Si4 C73 1.867(3) . ? O1 C11 1.458(3) . ? O2 C21 1.455(3) . ? O3 C61 1.485(3) . ? C11 C12 1.503(4) . ? C11 C14 1.513(3) . ? C11 C13 1.518(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C21 C22 1.511(4) . ? C21 C24 1.522(4) . ? C21 C23 1.535(4) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C61 C62 1.506(4) . ? C61 C63 1.510(4) . ? C61 C64 1.525(4) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 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 N1 Mo1 O1 103.11(9) . . ? N1 Mo1 O2 101.43(9) . . ? O1 Mo1 O2 112.79(8) . . ? N1 Mo1 N2 96.93(9) . . ? O1 Mo1 N2 115.19(7) . . ? O2 Mo1 N2 122.42(8) . . ? N1 Mo1 N4 162.13(8) . . ? O1 Mo1 N4 88.13(7) . . ? O2 Mo1 N4 86.54(7) . . ? N2 Mo1 N4 65.49(7) . . ? N4 P1 O3 116.63(10) . . ? N4 P1 N2 101.58(10) . . ? O3 P1 N2 110.57(9) . . ? N4 P1 N3 118.52(10) . . ? O3 P1 N3 96.60(10) . . ? N2 P1 N3 113.43(10) . . ? N2 Si1 C31 111.53(11) . . ? N2 Si1 C33 111.99(11) . . ? C31 Si1 C33 107.23(14) . . ? N2 Si1 C32 109.22(11) . . ? C31 Si1 C32 108.09(13) . . ? C33 Si1 C32 108.67(13) . . ? N3 Si2 C41 113.18(11) . . ? N3 Si2 C43 109.78(12) . . ? C41 Si2 C43 106.21(14) . . ? N3 Si2 C42 110.28(12) . . ? C41 Si2 C42 105.31(14) . . ? C43 Si2 C42 111.99(14) . . ? N3 Si3 C53 111.45(12) . . ? N3 Si3 C52 115.82(11) . . ? C53 Si3 C52 110.49(14) . . ? N3 Si3 C51 111.67(13) . . ? C53 Si3 C51 104.88(15) . . ? C52 Si3 C51 101.59(14) . . ? N4 Si4 C72 109.14(11) . . ? N4 Si4 C71 114.33(12) . . ? C72 Si4 C71 108.82(15) . . ? N4 Si4 C73 111.42(12) . . ? C72 Si4 C73 106.04(15) . . ? C71 Si4 C73 106.73(16) . . ? C11 O1 Mo1 136.52(14) . . ? C21 O2 Mo1 134.62(16) . . ? C61 O3 P1 131.10(16) . . ? P1 N2 Si1 133.90(12) . . ? P1 N2 Mo1 103.66(9) . . ? Si1 N2 Mo1 122.45(10) . . ? P1 N3 Si2 119.71(11) . . ? P1 N3 Si3 120.68(12) . . ? Si2 N3 Si3 118.32(11) . . ? P1 N4 Si4 146.18(13) . . ? P1 N4 Mo1 88.65(8) . . ? Si4 N4 Mo1 125.14(10) . . ? O1 C11 C12 108.5(2) . . ? O1 C11 C14 105.5(2) . . ? C12 C11 C14 110.8(3) . . ? O1 C11 C13 109.5(2) . . ? C12 C11 C13 111.4(3) . . ? C14 C11 C13 110.9(2) . . ? 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 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O2 C21 C22 109.0(2) . . ? O2 C21 C24 104.9(2) . . ? C22 C21 C24 111.0(3) . . ? O2 C21 C23 109.4(2) . . ? C22 C21 C23 111.1(3) . . ? C24 C21 C23 111.2(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 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si1 C31 H31A 109.5 . . ? Si1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si1 C32 H32A 109.5 . . ? Si1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si1 C33 H33A 109.5 . . ? Si1 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si1 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si2 C41 H41A 109.5 . . ? Si2 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? Si2 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? Si2 C42 H42A 109.5 . . ? Si2 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? Si2 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? Si2 C43 H43A 109.5 . . ? Si2 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? Si2 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? Si3 C51 H51A 109.5 . . ? Si3 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? Si3 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? Si3 C52 H52A 109.5 . . ? Si3 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? Si3 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? Si3 C53 H53A 109.5 . . ? Si3 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? Si3 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? O3 C61 C62 109.5(2) . . ? O3 C61 C63 111.0(2) . . ? C62 C61 C63 111.9(3) . . ? O3 C61 C64 103.8(2) . . ? C62 C61 C64 110.3(3) . . ? C63 C61 C64 110.0(2) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? Si4 C71 H71A 109.5 . . ? Si4 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? Si4 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? Si4 C72 H72A 109.5 . . ? Si4 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? Si4 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? Si4 C73 H73A 109.5 . . ? Si4 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? Si4 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 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 N1 Mo1 O1 C11 10.0(2) . . . . ? O2 Mo1 O1 C11 -98.5(2) . . . . ? N2 Mo1 O1 C11 114.3(2) . . . . ? N4 Mo1 O1 C11 176.0(2) . . . . ? P1 Mo1 O1 C11 146.1(2) . . . . ? N1 Mo1 O2 C21 -6.4(2) . . . . ? O1 Mo1 O2 C21 103.3(2) . . . . ? N2 Mo1 O2 C21 -112.3(2) . . . . ? N4 Mo1 O2 C21 -170.2(2) . . . . ? P1 Mo1 O2 C21 -146.1(2) . . . . ? N4 P1 O3 C61 -52.5(2) . . . . ? N2 P1 O3 C61 62.8(2) . . . . ? N3 P1 O3 C61 -179.1(2) . . . . ? Mo1 P1 O3 C61 16.3(2) . . . . ? N4 P1 N2 Si1 -171.86(15) . . . . ? O3 P1 N2 Si1 63.70(18) . . . . ? N3 P1 N2 Si1 -43.54(19) . . . . ? N4 P1 N2 Mo1 7.76(11) . . . . ? O3 P1 N2 Mo1 -116.68(9) . . . . ? N3 P1 N2 Mo1 136.08(10) . . . . ? C31 Si1 N2 P1 -5.4(2) . . . . ? C33 Si1 N2 P1 -125.59(17) . . . . ? C32 Si1 N2 P1 113.99(17) . . . . ? C31 Si1 N2 Mo1 175.02(13) . . . . ? C33 Si1 N2 Mo1 54.85(17) . . . . ? C32 Si1 N2 Mo1 -65.57(15) . . . . ? N1 Mo1 N2 P1 178.12(10) . . . . ? O1 Mo1 N2 P1 70.08(11) . . . . ? O2 Mo1 N2 P1 -73.60(11) . . . . ? N4 Mo1 N2 P1 -5.20(8) . . . . ? N1 Mo1 N2 Si1 -2.21(14) . . . . ? O1 Mo1 N2 Si1 -110.25(12) . . . . ? O2 Mo1 N2 Si1 106.07(12) . . . . ? N4 Mo1 N2 Si1 174.47(14) . . . . ? P1 Mo1 N2 Si1 179.67(19) . . . . ? N4 P1 N3 Si2 51.85(16) . . . . ? O3 P1 N3 Si2 177.05(12) . . . . ? N2 P1 N3 Si2 -67.13(14) . . . . ? Mo1 P1 N3 Si2 -22.35(18) . . . . ? N4 P1 N3 Si3 -114.97(13) . . . . ? O3 P1 N3 Si3 10.23(14) . . . . ? N2 P1 N3 Si3 126.05(12) . . . . ? Mo1 P1 N3 Si3 170.83(5) . . . . ? C41 Si2 N3 P1 10.29(17) . . . . ? C43 Si2 N3 P1 -108.18(15) . . . . ? C42 Si2 N3 P1 127.96(15) . . . . ? C41 Si2 N3 Si3 177.42(13) . . . . ? C43 Si2 N3 Si3 58.95(16) . . . . ? C42 Si2 N3 Si3 -64.91(16) . . . . ? C53 Si3 N3 P1 61.42(18) . . . . ? C52 Si3 N3 P1 -66.02(17) . . . . ? C51 Si3 N3 P1 178.36(14) . . . . ? C53 Si3 N3 Si2 -105.58(16) . . . . ? C52 Si3 N3 Si2 126.98(14) . . . . ? C51 Si3 N3 Si2 11.36(17) . . . . ? O3 P1 N4 Si4 -63.7(3) . . . . ? N2 P1 N4 Si4 176.1(2) . . . . ? N3 P1 N4 Si4 51.1(3) . . . . ? Mo1 P1 N4 Si4 -177.8(3) . . . . ? O3 P1 N4 Mo1 114.10(9) . . . . ? N2 P1 N4 Mo1 -6.16(9) . . . . ? N3 P1 N4 Mo1 -131.14(9) . . . . ? C72 Si4 N4 P1 137.5(2) . . . . ? C71 Si4 N4 P1 15.4(3) . . . . ? C73 Si4 N4 P1 -105.7(2) . . . . ? C72 Si4 N4 Mo1 -39.77(16) . . . . ? C71 Si4 N4 Mo1 -161.90(14) . . . . ? C73 Si4 N4 Mo1 76.99(16) . . . . ? N1 Mo1 N4 P1 16.2(3) . . . . ? O1 Mo1 N4 P1 -113.52(9) . . . . ? O2 Mo1 N4 P1 133.51(9) . . . . ? N2 Mo1 N4 P1 5.35(8) . . . . ? N1 Mo1 N4 Si4 -165.4(2) . . . . ? O1 Mo1 N4 Si4 64.95(12) . . . . ? O2 Mo1 N4 Si4 -48.02(12) . . . . ? N2 Mo1 N4 Si4 -176.17(14) . . . . ? P1 Mo1 N4 Si4 178.48(18) . . . . ? Mo1 O1 C11 C12 57.0(3) . . . . ? Mo1 O1 C11 C14 175.82(18) . . . . ? Mo1 O1 C11 C13 -64.7(3) . . . . ? Mo1 O2 C21 C22 -59.6(3) . . . . ? Mo1 O2 C21 C24 -178.6(2) . . . . ? Mo1 O2 C21 C23 62.0(3) . . . . ? P1 O3 C61 C62 -70.5(3) . . . . ? P1 O3 C61 C63 53.6(3) . . . . ? P1 O3 C61 C64 171.76(19) . . . . ? 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 C23 H23A N1 0.98 2.57 3.302(4) 131.1 . C33 H33A N1 0.98 2.48 3.190(4) 129.4 . C52 H52C O3 0.98 2.48 3.056(3) 117.3 . C63 H63A O1 0.98 2.48 3.434(3) 164.0 . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.55 _refine_diff_density_min -0.57 _refine_diff_density_rms 0.102 #===================================================================== data_12 _database_code_depnum_ccdc_archive 'CCDC 781906' #TrackingRef '- ANAT.cif' #===================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H57 Mo N4 O3 P Si4' _chemical_formula_weight 652.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 orthorhombic _symmetry_space_group_name_H-M Pbca 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' '-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 19.010(6) _cell_length_b 16.687(5) _cell_length_c 22.677(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7194(4) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 28053 _cell_measurement_theta_min 3 _cell_measurement_theta_max 35 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.206 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2784 _exptl_absorpt_coefficient_mu 0.568 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.912 _exptl_absorpt_correction_T_max 0.915 _exptl_absorpt_process_details 'CrysAlis RED; Oxford-Diffraction Poland, 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 'Xcalibur PX kappa-geometry diffractometer with Onyx CCD camera' _diffrn_measurement_method 'omega and phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 115343 _diffrn_reflns_av_R_equivalents 0.0662 _diffrn_reflns_av_sigmaI/netI 0.0677 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 35.00 _reflns_number_total 15779 _reflns_number_gt 8917 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD; Oxford-Diffraction Poland, 2003' _computing_cell_refinement 'CrysAlis RED; Oxford-Diffraction Poland, 2003' _computing_data_reduction 'CrysAlis RED; Oxford-Diffraction Poland, 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^)+(0.028P)^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 15779 _refine_ls_number_parameters 396 _refine_ls_number_restraints 332 _refine_ls_R_factor_all 0.0938 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.0760 _refine_ls_wR_factor_gt 0.0708 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.443242(7) 0.742507(8) 0.848690(6) 0.02093(4) Uani 0.9798(9) 1 d P A . Mo11 Mo 0.4452(7) 0.7464(8) 0.8925(7) 0.071(5) Uiso 0.0202(9) 1 d P A . P1 P 0.592870(19) 0.75967(2) 0.870948(17) 0.01819(8) Uani 1 1 d . . . N1 N 0.39779(7) 0.74241(9) 0.78604(6) 0.0330(3) Uani 1 1 d . A . O1 O 0.40872(6) 0.83405(7) 0.88680(5) 0.0314(3) Uani 1 1 d D A 1 C11A C 0.3457(4) 0.8788(5) 0.8706(5) 0.0346(13) Uani 0.258(3) 1 d PD A 1 H11A H 0.3170 0.8501 0.8403 0.041 Uiso 0.258(3) 1 calc PR A 1 C21A C 0.3038(3) 0.8946(4) 0.9278(3) 0.0239(6) Uiso 0.258(3) 1 d PD A 1 H21A H 0.3082 0.8483 0.9541 0.036 Uiso 0.258(3) 1 calc PR A 1 H21B H 0.2542 0.9033 0.9181 0.036 Uiso 0.258(3) 1 calc PR A 1 H21C H 0.3226 0.9424 0.9474 0.036 Uiso 0.258(3) 1 calc PR A 1 C31A C 0.3751(4) 0.9605(5) 0.8470(4) 0.0239(6) Uiso 0.258(3) 1 d PD A 1 H31A H 0.4258 0.9558 0.8404 0.036 Uiso 0.258(3) 1 calc PR A 1 H31B H 0.3660 1.0027 0.8761 0.036 Uiso 0.258(3) 1 calc PR A 1 H31C H 0.3517 0.9741 0.8098 0.036 Uiso 0.258(3) 1 calc PR A 1 C11B C 0.3541(4) 0.8867(5) 0.8629(5) 0.0346(13) Uani 0.266(4) 1 d PD A 2 H11B H 0.3406 0.8714 0.8218 0.041 Uiso 0.266(4) 1 calc PR A 2 C21B C 0.2917(3) 0.8793(5) 0.9061(4) 0.0239(6) Uiso 0.266(4) 1 d PD A 2 H21D H 0.2902 0.8248 0.9223 0.036 Uiso 0.266(4) 1 calc PR A 2 H21E H 0.2477 0.8904 0.8852 0.036 Uiso 0.266(4) 1 calc PR A 2 H21F H 0.2975 0.9178 0.9384 0.036 Uiso 0.266(4) 1 calc PR A 2 C31B C 0.3872(4) 0.9742(4) 0.8656(4) 0.0239(6) Uiso 0.266(4) 1 d PD A 2 H31D H 0.4384 0.9701 0.8696 0.036 Uiso 0.266(4) 1 calc PR A 2 H31E H 0.3678 1.0030 0.8996 0.036 Uiso 0.266(4) 1 calc PR A 2 H31F H 0.3757 1.0032 0.8293 0.036 Uiso 0.266(4) 1 calc PR A 2 C11C C 0.3591(6) 0.8994(7) 0.8774(7) 0.0346(13) Uani 0.130(4) 1 d PD A 3 H11C H 0.3717 0.9367 0.8446 0.041 Uiso 0.130(4) 1 calc PR A 3 C21C C 0.2881(5) 0.8576(8) 0.8703(6) 0.0239(6) Uiso 0.130(4) 1 d PD A 3 H21G H 0.2898 0.8216 0.8362 0.036 Uiso 0.130(4) 1 calc PR A 3 H21H H 0.2513 0.8979 0.8642 0.036 Uiso 0.130(4) 1 calc PR A 3 H21I H 0.2776 0.8266 0.9059 0.036 Uiso 0.130(4) 1 calc PR A 3 C31C C 0.3566(7) 0.9396(7) 0.9411(5) 0.0239(6) Uiso 0.130(4) 1 d PD A 3 H31G H 0.3915 0.9826 0.9432 0.036 Uiso 0.130(4) 1 calc PR A 3 H31H H 0.3670 0.8991 0.9711 0.036 Uiso 0.130(4) 1 calc PR A 3 H31I H 0.3096 0.9618 0.9481 0.036 Uiso 0.130(4) 1 calc PR A 3 C11D C 0.3595(8) 0.8988(7) 0.8749(7) 0.0346(13) Uani 0.111(4) 1 d PD A 4 H11D H 0.3105 0.8792 0.8681 0.041 Uiso 0.111(4) 1 calc PR A 4 C21D C 0.3880(9) 0.9468(9) 0.8236(6) 0.0239(6) Uiso 0.111(4) 1 d PD A 4 H21J H 0.3838 0.9153 0.7873 0.036 Uiso 0.111(4) 1 calc PR A 4 H21K H 0.4376 0.9596 0.8307 0.036 Uiso 0.111(4) 1 calc PR A 4 H21L H 0.3611 0.9965 0.8195 0.036 Uiso 0.111(4) 1 calc PR A 4 C31D C 0.3658(9) 0.9544(8) 0.9312(6) 0.0239(6) Uiso 0.111(4) 1 d PD A 4 H31J H 0.3524 0.9240 0.9664 0.036 Uiso 0.111(4) 1 calc PR A 4 H31K H 0.3345 1.0007 0.9268 0.036 Uiso 0.111(4) 1 calc PR A 4 H31L H 0.4144 0.9731 0.9353 0.036 Uiso 0.111(4) 1 calc PR A 4 C11E C 0.3556(6) 0.8960(8) 0.8854(7) 0.0346(13) Uani 0.155(4) 1 d PD A 5 H11E H 0.3613 0.9348 0.9186 0.041 Uiso 0.155(4) 1 calc PR A 5 C21E C 0.3651(6) 0.9358(7) 0.8265(5) 0.0239(6) Uiso 0.155(4) 1 d PD A 5 H21M H 0.4105 0.9637 0.8256 0.036 Uiso 0.155(4) 1 calc PR A 5 H21N H 0.3271 0.9744 0.8201 0.036 Uiso 0.155(4) 1 calc PR A 5 H21O H 0.3641 0.8951 0.7953 0.036 Uiso 0.155(4) 1 calc PR A 5 C31E C 0.2842(5) 0.8493(8) 0.8895(6) 0.0239(6) Uiso 0.155(4) 1 d PD A 5 H31M H 0.2804 0.8238 0.9283 0.036 Uiso 0.155(4) 1 calc PR A 5 H31N H 0.2826 0.8081 0.8587 0.036 Uiso 0.155(4) 1 calc PR A 5 H31O H 0.2451 0.8867 0.8841 0.036 Uiso 0.155(4) 1 calc PR A 5 C11F C 0.3587(8) 0.8997(7) 0.8838(9) 0.0346(13) Uani 0.080(3) 1 d PD A 6 H11F H 0.3218 0.8923 0.9147 0.041 Uiso 0.080(3) 1 calc PR A 6 C21F C 0.3248(9) 0.9000(10) 0.8236(7) 0.0239(6) Uiso 0.080(3) 1 d PD A 6 H21P H 0.3091 0.8457 0.8137 0.036 Uiso 0.080(3) 1 calc PR A 6 H21Q H 0.3590 0.9182 0.7941 0.036 Uiso 0.080(3) 1 calc PR A 6 H21R H 0.2843 0.9363 0.8238 0.036 Uiso 0.080(3) 1 calc PR A 6 C31F C 0.3987(10) 0.9810(7) 0.8950(9) 0.0239(6) Uiso 0.080(3) 1 d PD A 6 H31P H 0.4296 0.9753 0.9293 0.036 Uiso 0.080(3) 1 calc PR A 6 H31Q H 0.3645 1.0237 0.9023 0.036 Uiso 0.080(3) 1 calc PR A 6 H31R H 0.4270 0.9945 0.8602 0.036 Uiso 0.080(3) 1 calc PR A 6 O2 O 0.41073(6) 0.64623(7) 0.88232(6) 0.0341(3) Uani 1 1 d D A 7 C12A C 0.3608(5) 0.5927(5) 0.8523(5) 0.0353(10) Uani 0.218(3) 1 d PD A 7 H12A H 0.3635 0.5971 0.8084 0.042 Uiso 0.218(3) 1 calc PR A 7 C22A C 0.2894(4) 0.6148(6) 0.8759(6) 0.0252(6) Uiso 0.218(3) 1 d PD A 7 H22A H 0.2789 0.6707 0.8659 0.038 Uiso 0.218(3) 1 calc PR A 7 H22B H 0.2890 0.6083 0.9189 0.038 Uiso 0.218(3) 1 calc PR A 7 H22C H 0.2537 0.5798 0.8583 0.038 Uiso 0.218(3) 1 calc PR A 7 C32A C 0.3769(4) 0.5054(4) 0.8750(4) 0.0252(6) Uiso 0.218(3) 1 d PD A 7 H32A H 0.4051 0.4768 0.8455 0.038 Uiso 0.218(3) 1 calc PR A 7 H32B H 0.3325 0.4767 0.8814 0.038 Uiso 0.218(3) 1 calc PR A 7 H32C H 0.4030 0.5083 0.9122 0.038 Uiso 0.218(3) 1 calc PR A 7 C12B C 0.3512(5) 0.5924(7) 0.8782(6) 0.0353(10) Uani 0.196(5) 1 d PD A 8 H12B H 0.3543 0.5552 0.9127 0.042 Uiso 0.196(5) 1 calc PR A 8 C22B C 0.2821(4) 0.6340(8) 0.8828(6) 0.0252(6) Uiso 0.196(5) 1 d PD A 8 H22D H 0.2812 0.6668 0.9187 0.038 Uiso 0.196(5) 1 calc PR A 8 H22E H 0.2443 0.5942 0.8845 0.038 Uiso 0.196(5) 1 calc PR A 8 H22F H 0.2753 0.6685 0.8483 0.038 Uiso 0.196(5) 1 calc PR A 8 C32B C 0.3671(5) 0.5418(6) 0.8226(4) 0.0252(6) Uiso 0.196(5) 1 d PD A 8 H32D H 0.4180 0.5408 0.8156 0.038 Uiso 0.196(5) 1 calc PR A 8 H32E H 0.3434 0.5656 0.7884 0.038 Uiso 0.196(5) 1 calc PR A 8 H32F H 0.3500 0.4870 0.8284 0.038 Uiso 0.196(5) 1 calc PR A 8 C12C C 0.3533(6) 0.5900(7) 0.8705(6) 0.0353(10) Uani 0.179(4) 1 d PD A 9 H12C H 0.3613 0.5567 0.8345 0.042 Uiso 0.179(4) 1 calc PR A 9 C22C C 0.2854(5) 0.6381(8) 0.8679(6) 0.0252(6) Uiso 0.179(4) 1 d PD A 9 H22G H 0.2856 0.6719 0.8325 0.038 Uiso 0.179(4) 1 calc PR A 9 H22H H 0.2817 0.6721 0.9030 0.038 Uiso 0.179(4) 1 calc PR A 9 H22I H 0.2452 0.6015 0.8664 0.038 Uiso 0.179(4) 1 calc PR A 9 C32C C 0.3494(5) 0.5380(5) 0.9300(4) 0.0252(6) Uiso 0.179(4) 1 d PD A 9 H32G H 0.3936 0.5087 0.9353 0.038 Uiso 0.179(4) 1 calc PR A 9 H32H H 0.3104 0.4998 0.9272 0.038 Uiso 0.179(4) 1 calc PR A 9 H32I H 0.3418 0.5737 0.9637 0.038 Uiso 0.179(4) 1 calc PR A 9 C12D C 0.3575(7) 0.5852(7) 0.8700(5) 0.0353(10) Uani 0.168(3) 1 d PD A 10 H12D H 0.3084 0.6067 0.8721 0.042 Uiso 0.168(3) 1 calc PR A 10 C22D C 0.3704(6) 0.5155(6) 0.9134(5) 0.0252(6) Uiso 0.168(3) 1 d PD A 10 H22J H 0.3984 0.5347 0.9468 0.038 Uiso 0.168(3) 1 calc PR A 10 H22K H 0.3959 0.4724 0.8932 0.038 Uiso 0.168(3) 1 calc PR A 10 H22L H 0.3252 0.4951 0.9277 0.038 Uiso 0.168(3) 1 calc PR A 10 C32D C 0.3763(6) 0.5510(6) 0.8075(4) 0.0252(6) Uiso 0.168(3) 1 d PD A 10 H32J H 0.3625 0.5897 0.7771 0.038 Uiso 0.168(3) 1 calc PR A 10 H32K H 0.3511 0.5005 0.8012 0.038 Uiso 0.168(3) 1 calc PR A 10 H32L H 0.4271 0.5414 0.8052 0.038 Uiso 0.168(3) 1 calc PR A 10 C12E C 0.3509(5) 0.6042(6) 0.8550(4) 0.0353(10) Uani 0.239(3) 1 d PD A 11 H12E H 0.3359 0.6297 0.8171 0.042 Uiso 0.239(3) 1 calc PR A 11 C22E C 0.3750(4) 0.5176(4) 0.8464(4) 0.0252(6) Uiso 0.239(3) 1 d PD A 11 H22M H 0.4000 0.5128 0.8088 0.038 Uiso 0.239(3) 1 calc PR A 11 H22N H 0.3339 0.4821 0.8463 0.038 Uiso 0.239(3) 1 calc PR A 11 H22O H 0.4065 0.5024 0.8788 0.038 Uiso 0.239(3) 1 calc PR A 11 C32E C 0.2914(3) 0.6067(5) 0.9030(4) 0.0252(6) Uiso 0.239(3) 1 d PD A 11 H32M H 0.2830 0.6624 0.9149 0.038 Uiso 0.239(3) 1 calc PR A 11 H32N H 0.3061 0.5755 0.9375 0.038 Uiso 0.239(3) 1 calc PR A 11 H32O H 0.2481 0.5839 0.8868 0.038 Uiso 0.239(3) 1 calc PR A 11 N2 N 0.54081(6) 0.75655(8) 0.81253(6) 0.0202(3) Uani 1 1 d . A . Si1 Si 0.55500(3) 0.76433(3) 0.735988(19) 0.02731(10) Uani 1 1 d . . . C15 C 0.49857(10) 0.84447(12) 0.70330(8) 0.0395(5) Uani 1 1 d . A . H15A H 0.5051 0.8944 0.7253 0.059 Uiso 1 1 calc R . . H15B H 0.4491 0.8282 0.7054 0.059 Uiso 1 1 calc R . . H15C H 0.5118 0.8528 0.6620 0.059 Uiso 1 1 calc R . . C25 C 0.53276(12) 0.66723(12) 0.70016(8) 0.0432(5) Uani 1 1 d . A . H25A H 0.4843 0.6524 0.7100 0.065 Uiso 1 1 calc R . . H25B H 0.5649 0.6256 0.7143 0.065 Uiso 1 1 calc R . . H25C H 0.5374 0.6726 0.6573 0.065 Uiso 1 1 calc R . . C35 C 0.64856(10) 0.78967(13) 0.71984(8) 0.0396(5) Uani 1 1 d . A . H35A H 0.6792 0.7473 0.7352 0.059 Uiso 1 1 calc R . . H35B H 0.6606 0.8407 0.7387 0.059 Uiso 1 1 calc R . . H35C H 0.6551 0.7944 0.6771 0.059 Uiso 1 1 calc R . . N3 N 0.66724(7) 0.70907(8) 0.86238(6) 0.0210(3) Uani 1 1 d . A . Si2 Si 0.66201(3) 0.60213(3) 0.85697(2) 0.02875(11) Uani 1 1 d . . . C16 C 0.69782(11) 0.55590(12) 0.92557(9) 0.0445(5) Uani 1 1 d . A . H16A H 0.6649 0.5649 0.9582 0.067 Uiso 1 1 calc R . . H16B H 0.7433 0.5803 0.9351 0.067 Uiso 1 1 calc R . . H16C H 0.7040 0.4982 0.9195 0.067 Uiso 1 1 calc R . . C26 C 0.70901(11) 0.56767(12) 0.78910(9) 0.0425(5) Uani 1 1 d . A . H26A H 0.7599 0.5714 0.7954 0.064 Uiso 1 1 calc R . . H26B H 0.6955 0.6016 0.7557 0.064 Uiso 1 1 calc R . . H26C H 0.6962 0.5120 0.7807 0.064 Uiso 1 1 calc R . . C36 C 0.57035(10) 0.56425(10) 0.85013(9) 0.0376(4) Uani 1 1 d . A . H36A H 0.5490 0.5857 0.8141 0.056 Uiso 1 1 calc R . . H36B H 0.5429 0.5815 0.8844 0.056 Uiso 1 1 calc R . . H36C H 0.5709 0.5056 0.8483 0.056 Uiso 1 1 calc R . . Si3 Si 0.75140(2) 0.75599(3) 0.87326(2) 0.02575(10) Uani 1 1 d . . . C17 C 0.82399(9) 0.68400(12) 0.85682(9) 0.0397(5) Uani 1 1 d . A . H17A H 0.8247 0.6724 0.8145 0.060 Uiso 1 1 calc R . . H17B H 0.8163 0.6342 0.8788 0.060 Uiso 1 1 calc R . . H17C H 0.8691 0.7076 0.8685 0.060 Uiso 1 1 calc R . . C27 C 0.76249(10) 0.78848(14) 0.95125(8) 0.0424(5) Uani 1 1 d . A . H27A H 0.7598 0.7417 0.9772 0.064 Uiso 1 1 calc R . . H27B H 0.7251 0.8265 0.9616 0.064 Uiso 1 1 calc R . . H27C H 0.8084 0.8144 0.9560 0.064 Uiso 1 1 calc R . . C37 C 0.77222(9) 0.84219(11) 0.82430(9) 0.0381(4) Uani 1 1 d . A . H37A H 0.7332 0.8806 0.8251 0.057 Uiso 1 1 calc R . . H37B H 0.7791 0.8229 0.7839 0.057 Uiso 1 1 calc R . . H37C H 0.8153 0.8685 0.8381 0.057 Uiso 1 1 calc R . . N4 N 0.54106(6) 0.73621(8) 0.92141(6) 0.0229(3) Uani 1 1 d . A . Si4 Si 0.53120(3) 0.72364(4) 0.99548(2) 0.04218(15) Uani 1 1 d . . . C18 C 0.61473(11) 0.72846(18) 1.03809(9) 0.0636(7) Uani 1 1 d . A . H18A H 0.6347 0.7825 1.0351 0.095 Uiso 1 1 calc R . . H18B H 0.6482 0.6895 1.0221 0.095 Uiso 1 1 calc R . . H18C H 0.6053 0.7160 1.0796 0.095 Uiso 1 1 calc R . . C28 C 0.47068(13) 0.8021(2) 1.02470(11) 0.0809(10) Uani 1 1 d . A . H28A H 0.4248 0.7973 1.0053 0.121 Uiso 1 1 calc R . . H28B H 0.4905 0.8552 1.0168 0.121 Uiso 1 1 calc R . . H28C H 0.4650 0.7949 1.0673 0.121 Uiso 1 1 calc R . . C38 C 0.49077(17) 0.62332(19) 1.01078(12) 0.0906(11) Uani 1 1 d . A . H38A H 0.5232 0.5809 0.9983 0.136 Uiso 1 1 calc R . . H38B H 0.4465 0.6184 0.9889 0.136 Uiso 1 1 calc R . . H38C H 0.4814 0.6182 1.0531 0.136 Uiso 1 1 calc R . . O3 O 0.62569(6) 0.84738(7) 0.87660(5) 0.0285(3) Uani 1 1 d . A . C13 C 0.58076(10) 0.91696(11) 0.88964(11) 0.0450(6) Uani 1 1 d . . . H13 H 0.5309 0.8990 0.8945 0.054 Uiso 1 1 calc R A . C23 C 0.58599(14) 0.97296(13) 0.83817(13) 0.0683(8) Uani 1 1 d . A . H23A H 0.5710 0.9452 0.8022 0.102 Uiso 1 1 calc R . . H23B H 0.6348 0.9908 0.8337 0.102 Uiso 1 1 calc R . . H23C H 0.5556 1.0195 0.8449 0.102 Uiso 1 1 calc R . . C33 C 0.60690(14) 0.95285(14) 0.94659(13) 0.0734(8) Uani 1 1 d . A . H33A H 0.6560 0.9696 0.9419 0.110 Uiso 1 1 calc R . . H33B H 0.6037 0.9128 0.9781 0.110 Uiso 1 1 calc R . . H33C H 0.5780 0.9995 0.9568 0.110 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 0.01695(6) 0.02394(7) 0.02191(7) 0.00164(6) -0.00261(5) -0.00139(5) P1 0.01681(16) 0.01872(19) 0.01905(18) -0.00106(15) -0.00119(14) 0.00076(15) N1 0.0250(7) 0.0445(9) 0.0293(8) 0.0022(7) -0.0036(6) -0.0034(7) O1 0.0216(6) 0.0332(7) 0.0393(7) 0.0001(5) 0.0007(5) 0.0063(5) C11A 0.0233(15) 0.031(2) 0.050(4) 0.0015(19) 0.0042(16) 0.0087(14) O1B 0.0216(6) 0.0332(7) 0.0393(7) 0.0001(5) 0.0007(5) 0.0063(5) C11B 0.0233(15) 0.031(2) 0.050(4) 0.0015(19) 0.0042(16) 0.0087(14) O1C 0.0216(6) 0.0332(7) 0.0393(7) 0.0001(5) 0.0007(5) 0.0063(5) C11C 0.0233(15) 0.031(2) 0.050(4) 0.0015(19) 0.0042(16) 0.0087(14) O1D 0.0216(6) 0.0332(7) 0.0393(7) 0.0001(5) 0.0007(5) 0.0063(5) C11D 0.0233(15) 0.031(2) 0.050(4) 0.0015(19) 0.0042(16) 0.0087(14) O1E 0.0216(6) 0.0332(7) 0.0393(7) 0.0001(5) 0.0007(5) 0.0063(5) C11E 0.0233(15) 0.031(2) 0.050(4) 0.0015(19) 0.0042(16) 0.0087(14) O1F 0.0216(6) 0.0332(7) 0.0393(7) 0.0001(5) 0.0007(5) 0.0063(5) C11F 0.0233(15) 0.031(2) 0.050(4) 0.0015(19) 0.0042(16) 0.0087(14) O2 0.0288(7) 0.0313(7) 0.0422(8) 0.0052(5) -0.0018(6) -0.0118(5) C12A 0.0385(15) 0.0416(19) 0.026(3) 0.0089(18) 0.0073(18) -0.0271(13) O2B 0.0288(7) 0.0313(7) 0.0422(8) 0.0052(5) -0.0018(6) -0.0118(5) C12B 0.0385(15) 0.0416(19) 0.026(3) 0.0089(18) 0.0073(18) -0.0271(13) O2C 0.0288(7) 0.0313(7) 0.0422(8) 0.0052(5) -0.0018(6) -0.0118(5) C12C 0.0385(15) 0.0416(19) 0.026(3) 0.0089(18) 0.0073(18) -0.0271(13) O2D 0.0288(7) 0.0313(7) 0.0422(8) 0.0052(5) -0.0018(6) -0.0118(5) C12D 0.0385(15) 0.0416(19) 0.026(3) 0.0089(18) 0.0073(18) -0.0271(13) O2E 0.0288(7) 0.0313(7) 0.0422(8) 0.0052(5) -0.0018(6) -0.0118(5) C12E 0.0385(15) 0.0416(19) 0.026(3) 0.0089(18) 0.0073(18) -0.0271(13) N2 0.0185(5) 0.0230(7) 0.0190(6) 0.0027(5) -0.0017(5) 0.0006(5) Si1 0.0274(2) 0.0350(3) 0.0196(2) 0.00486(18) -0.00190(18) 0.0039(2) C15 0.0374(10) 0.0487(12) 0.0324(10) 0.0158(8) -0.0034(9) 0.0047(9) C25 0.0538(13) 0.0501(13) 0.0255(10) -0.0069(8) -0.0074(9) 0.0065(10) C35 0.0347(10) 0.0605(13) 0.0236(9) 0.0109(9) 0.0028(8) 0.0036(9) N3 0.0187(6) 0.0219(6) 0.0223(7) -0.0008(5) -0.0006(5) 0.0042(5) Si2 0.0325(2) 0.0207(2) 0.0331(3) 0.00128(19) -0.0037(2) 0.00805(18) C16 0.0504(12) 0.0361(11) 0.0471(13) 0.0119(9) -0.0055(10) 0.0140(9) C26 0.0486(12) 0.0340(11) 0.0450(12) -0.0108(9) -0.0038(10) 0.0147(9) C36 0.0427(11) 0.0179(8) 0.0522(12) -0.0005(8) -0.0054(10) -0.0017(7) Si3 0.01743(18) 0.0334(3) 0.0264(2) -0.00229(19) -0.00045(16) 0.00351(19) C17 0.0249(9) 0.0519(12) 0.0423(11) 0.0004(9) 0.0000(8) 0.0137(8) C27 0.0244(9) 0.0656(14) 0.0373(11) -0.0135(10) -0.0039(8) -0.0011(9) C37 0.0220(9) 0.0389(11) 0.0533(12) 0.0033(9) 0.0037(8) -0.0013(7) N4 0.0195(6) 0.0307(7) 0.0186(6) 0.0003(5) -0.0013(5) 0.0004(5) Si4 0.0267(2) 0.0802(4) 0.0197(2) 0.0046(3) 0.0013(2) -0.0030(3) C18 0.0352(11) 0.132(2) 0.0241(10) 0.0056(12) -0.0047(9) 0.0035(13) C28 0.0408(13) 0.165(3) 0.0365(13) -0.0269(16) 0.0071(11) 0.0252(17) C38 0.101(2) 0.126(3) 0.0458(16) 0.0419(16) -0.0060(15) -0.047(2) O3 0.0180(5) 0.0200(6) 0.0474(7) -0.0071(5) 0.0028(5) 0.0008(4) C13 0.0232(9) 0.0198(9) 0.0920(18) -0.0139(10) 0.0082(10) 0.0025(7) C23 0.0564(15) 0.0280(11) 0.121(2) 0.0071(13) -0.0052(15) 0.0085(10) C33 0.0633(16) 0.0471(14) 0.110(2) -0.0449(14) 0.0165(16) 0.0013(12) _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 Mo11 0.996(15) . ? Mo1 N1 1.6628(15) . ? Mo1 O1 1.8738(12) . ? Mo1 O2 1.8828(12) . ? Mo11 O1 1.624(13) . ? Mo11 O2 1.810(13) . ? P1 N4 1.5597(14) . ? P1 O3 1.5961(12) . ? P1 N2 1.6544(13) . ? P1 N3 1.6582(13) . ? O1 C11A 1.459(6) . ? C11A C21A 1.544(9) . ? C11A C31A 1.567(9) . ? C11A H11A 1.0000 . ? C21A H21A 0.9800 . ? C21A H21B 0.9800 . ? C21A H21C 0.9800 . ? C31A H31A 0.9800 . ? C31A H31B 0.9800 . ? C31A H31C 0.9800 . ? C11B C21B 1.545(9) . ? C11B C31B 1.590(9) . ? C11B H11B 1.0000 . ? C21B H21D 0.9800 . ? C21B H21E 0.9800 . ? C21B H21F 0.9800 . ? C31B H31D 0.9800 . ? C31B H31E 0.9800 . ? C31B H31F 0.9800 . ? C11C C21C 1.527(10) . ? C11C C31C 1.593(10) . ? C11C H11C 1.0000 . ? C21C H21G 0.9800 . ? C21C H21H 0.9800 . ? C21C H21I 0.9800 . ? C31C H31G 0.9800 . ? C31C H31H 0.9800 . ? C31C H31I 0.9800 . ? C11D C21D 1.514(11) . ? C11D C31D 1.584(10) . ? C11D H11D 1.0000 . ? C21D H21J 0.9800 . ? C21D H21K 0.9800 . ? C21D H21L 0.9800 . ? C31D H31J 0.9800 . ? C31D H31K 0.9800 . ? C31D H31L 0.9800 . ? C11E C21E 1.503(10) . ? C11E C31E 1.568(11) . ? C11E H11E 1.0000 . ? C21E H21M 0.9800 . ? C21E H21N 0.9800 . ? C21E H21O 0.9800 . ? C31E H31M 0.9800 . ? C31E H31N 0.9800 . ? C31E H31O 0.9800 . ? C11F C21F 1.511(11) . ? C11F C31F 1.575(10) . ? C11F H11F 1.0000 . ? C21F H21P 0.9800 . ? C21F H21Q 0.9800 . ? C21F H21R 0.9800 . ? C31F H31P 0.9800 . ? C31F H31Q 0.9800 . ? C31F H31R 0.9800 . ? O2 C12A 1.471(7) . ? C12A C22A 1.505(9) . ? C12A C32A 1.575(9) . ? C12A H12A 1.0000 . ? C22A H22A 0.9800 . ? C22A H22B 0.9800 . ? C22A H22C 0.9800 . ? C32A H32A 0.9800 . ? C32A H32B 0.9800 . ? C32A H32C 0.9800 . ? C12B C22B 1.489(9) . ? C12B C32B 1.548(9) . ? C12B H12B 1.0000 . ? C22B H22D 0.9800 . ? C22B H22E 0.9800 . ? C22B H22F 0.9800 . ? C32B H32D 0.9800 . ? C32B H32E 0.9800 . ? C32B H32F 0.9800 . ? C12C C22C 1.521(10) . ? C12C C32C 1.606(10) . ? C12C H12C 1.0000 . ? C22C H22G 0.9800 . ? C22C H22H 0.9800 . ? C22C H22I 0.9800 . ? C32C H32G 0.9800 . ? C32C H32H 0.9800 . ? C32C H32I 0.9800 . ? C12D C22D 1.545(11) . ? C12D C32D 1.569(10) . ? C12D H12D 1.0000 . ? C22D H22J 0.9800 . ? C22D H22K 0.9800 . ? C22D H22L 0.9800 . ? C32D H32J 0.9800 . ? C32D H32K 0.9800 . ? C32D H32L 0.9800 . ? C12E C22E 1.528(10) . ? C12E C32E 1.571(9) . ? C12E H12E 1.0000 . ? C22E H22M 0.9800 . ? C22E H22N 0.9800 . ? C22E H22O 0.9800 . ? C32E H32M 0.9800 . ? C32E H32N 0.9800 . ? C32E H32O 0.9800 . ? N2 Si1 1.7615(14) . ? Si1 C25 1.861(2) . ? Si1 C35 1.864(2) . ? Si1 C15 1.8678(19) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? N3 Si2 1.7915(14) . ? N3 Si3 1.7982(14) . ? Si2 C36 1.8601(19) . ? Si2 C16 1.865(2) . ? Si2 C26 1.870(2) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? Si3 C37 1.860(2) . ? Si3 C27 1.8617(19) . ? Si3 C17 1.8672(18) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? N4 Si4 1.7031(15) . ? Si4 C18 1.861(2) . ? Si4 C28 1.864(3) . ? Si4 C38 1.874(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? O3 C13 1.472(2) . ? C13 C23 1.499(3) . ? C13 C33 1.508(3) . ? C13 H13 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 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 N1 Mo1 O1 102.29(7) . . ? N1 Mo1 O2 100.06(7) . . ? O1 Mo1 O2 113.20(6) . . ? N4 P1 O3 114.72(7) . . ? N4 P1 N2 101.64(7) . . ? O3 P1 N2 109.09(7) . . ? N4 P1 N3 119.77(7) . . ? O3 P1 N3 98.23(6) . . ? N2 P1 N3 113.59(7) . . ? C11A O1 Mo1 126.1(4) . . ? O1 C11A C21A 107.4(7) . . ? O1 C11A C31A 103.8(6) . . ? C21A C11A C31A 108.7(7) . . ? O1 C11A H11A 112.1 . . ? C21A C11A H11A 112.1 . . ? C31A C11A H11A 112.1 . . ? C11A C21A H21A 109.5 . . ? C11A C21A H21B 109.5 . . ? H21A C21A H21B 109.5 . . ? C11A C21A H21C 109.5 . . ? H21A C21A H21C 109.5 . . ? H21B C21A H21C 109.5 . . ? C11A C31A H31A 109.5 . . ? C11A C31A H31B 109.5 . . ? H31A C31A H31B 109.5 . . ? C11A C31A H31C 109.5 . . ? H31A C31A H31C 109.5 . . ? H31B C31A H31C 109.5 . . ? C21B C11B C31B 110.7(7) . . ? C21B C11B H11B 111.9 . . ? C31B C11B H11B 111.9 . . ? C11B C21B H21D 109.5 . . ? C11B C21B H21E 109.5 . . ? H21D C21B H21E 109.5 . . ? C11B C21B H21F 109.5 . . ? H21D C21B H21F 109.5 . . ? H21E C21B H21F 109.5 . . ? C11B C31B H31D 109.5 . . ? C11B C31B H31E 109.5 . . ? H31D C31B H31E 109.5 . . ? C11B C31B H31F 109.5 . . ? H31D C31B H31F 109.5 . . ? H31E C31B H31F 109.5 . . ? C21C C11C C31C 105.2(9) . . ? C21C C11C H11C 114.7 . . ? C31C C11C H11C 114.7 . . ? C11C C21C H21G 109.5 . . ? C11C C21C H21H 109.5 . . ? H21G C21C H21H 109.5 . . ? C11C C21C H21I 109.5 . . ? H21G C21C H21I 109.5 . . ? H21H C21C H21I 109.5 . . ? C11C C31C H31G 109.5 . . ? C11C C31C H31H 109.5 . . ? H31G C31C H31H 109.5 . . ? C11C C31C H31I 109.5 . . ? H31G C31C H31I 109.5 . . ? H31H C31C H31I 109.5 . . ? C21D C11D C31D 106.4(10) . . ? C21D C11D H11D 112.8 . . ? C31D C11D H11D 112.8 . . ? C11D C21D H21J 109.5 . . ? C11D C21D H21K 109.5 . . ? H21J C21D H21K 109.5 . . ? C11D C21D H21L 109.5 . . ? H21J C21D H21L 109.5 . . ? H21K C21D H21L 109.5 . . ? C11D C31D H31J 109.5 . . ? C11D C31D H31K 109.5 . . ? H31J C31D H31K 109.5 . . ? C11D C31D H31L 109.5 . . ? H31J C31D H31L 109.5 . . ? H31K C31D H31L 109.5 . . ? C21E C11E C31E 112.1(10) . . ? C21E C11E H11E 111.8 . . ? C31E C11E H11E 111.8 . . ? C11E C21E H21M 109.5 . . ? C11E C21E H21N 109.5 . . ? H21M C21E H21N 109.5 . . ? C11E C21E H21O 109.5 . . ? H21M C21E H21O 109.5 . . ? H21N C21E H21O 109.5 . . ? C11E C31E H31M 109.5 . . ? C11E C31E H31N 109.5 . . ? H31M C31E H31N 109.5 . . ? C11E C31E H31O 109.5 . . ? H31M C31E H31O 109.5 . . ? H31N C31E H31O 109.5 . . ? C21F C11F C31F 110.4(11) . . ? C21F C11F H11F 109.5 . . ? C31F C11F H11F 109.5 . . ? C11F C21F H21P 109.5 . . ? C11F C21F H21Q 109.5 . . ? H21P C21F H21Q 109.5 . . ? C11F C21F H21R 109.5 . . ? H21P C21F H21R 109.5 . . ? H21Q C21F H21R 109.5 . . ? C11F C31F H31P 109.5 . . ? C11F C31F H31Q 109.5 . . ? H31P C31F H31Q 109.5 . . ? C11F C31F H31R 109.5 . . ? H31P C31F H31R 109.5 . . ? H31Q C31F H31R 109.5 . . ? C12A O2 Mo1 122.9(4) . . ? O2 C12A C22A 105.6(7) . . ? O2 C12A C32A 106.6(6) . . ? C22A C12A C32A 106.6(8) . . ? O2 C12A H12A 112.5 . . ? C22A C12A H12A 112.5 . . ? C32A C12A H12A 112.5 . . ? C12A C22A H22A 109.5 . . ? C12A C22A H22B 109.5 . . ? H22A C22A H22B 109.5 . . ? C12A C22A H22C 109.5 . . ? H22A C22A H22C 109.5 . . ? H22B C22A H22C 109.5 . . ? C12A C32A H32A 109.5 . . ? C12A C32A H32B 109.5 . . ? H32A C32A H32B 109.5 . . ? C12A C32A H32C 109.5 . . ? H32A C32A H32C 109.5 . . ? H32B C32A H32C 109.5 . . ? C22B C12B C32B 118.9(9) . . ? C22B C12B H12B 106.7 . . ? C32B C12B H12B 106.7 . . ? C12B C22B H22D 109.5 . . ? C12B C22B H22E 109.5 . . ? H22D C22B H22E 109.5 . . ? C12B C22B H22F 109.5 . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 109.5 . . ? C12B C32B H32D 109.5 . . ? C12B C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? C12B C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? C22C C12C C32C 106.3(8) . . ? C22C C12C H12C 113.1 . . ? C32C C12C H12C 113.1 . . ? C12C C22C H22G 109.5 . . ? C12C C22C H22H 109.5 . . ? H22G C22C H22H 109.5 . . ? C12C C22C H22I 109.5 . . ? H22G C22C H22I 109.5 . . ? H22H C22C H22I 109.5 . . ? C12C C32C H32G 109.5 . . ? C12C C32C H32H 109.5 . . ? H32G C32C H32H 109.5 . . ? C12C C32C H32I 109.5 . . ? H32G C32C H32I 109.5 . . ? H32H C32C H32I 109.5 . . ? C22D C12D C32D 105.4(9) . . ? C22D C12D H12D 112.8 . . ? C32D C12D H12D 112.8 . . ? C12D C22D H22J 109.5 . . ? C12D C22D H22K 109.5 . . ? H22J C22D H22K 109.5 . . ? C12D C22D H22L 109.5 . . ? H22J C22D H22L 109.5 . . ? H22K C22D H22L 109.5 . . ? C12D C32D H32J 109.5 . . ? C12D C32D H32K 109.5 . . ? H32J C32D H32K 109.5 . . ? C12D C32D H32L 109.5 . . ? H32J C32D H32L 109.5 . . ? H32K C32D H32L 109.5 . . ? C22E C12E C32E 109.2(7) . . ? C22E C12E H12E 112.3 . . ? C32E C12E H12E 112.3 . . ? C12E C22E H22M 109.5 . . ? C12E C22E H22N 109.5 . . ? H22M C22E H22N 109.5 . . ? C12E C22E H22O 109.5 . . ? H22M C22E H22O 109.5 . . ? H22N C22E H22O 109.5 . . ? C12E C32E H32M 109.5 . . ? C12E C32E H32N 109.5 . . ? H32M C32E H32N 109.5 . . ? C12E C32E H32O 109.5 . . ? H32M C32E H32O 109.5 . . ? H32N C32E H32O 109.5 . . ? P1 N2 Si1 134.03(8) . . ? P1 N2 Mo1 103.04(7) . . ? Si1 N2 Mo1 122.92(7) . . ? N2 Si1 C25 109.34(8) . . ? N2 Si1 C35 110.88(7) . . ? C25 Si1 C35 109.17(10) . . ? N2 Si1 C15 110.85(8) . . ? C25 Si1 C15 108.63(10) . . ? C35 Si1 C15 107.92(9) . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si1 C25 H25A 109.5 . . ? Si1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si1 C35 H35A 109.5 . . ? Si1 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si1 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? P1 N3 Si2 117.91(8) . . ? P1 N3 Si3 121.38(8) . . ? Si2 N3 Si3 119.50(7) . . ? N3 Si2 C36 113.34(7) . . ? N3 Si2 C16 109.55(8) . . ? C36 Si2 C16 105.72(10) . . ? N3 Si2 C26 109.64(8) . . ? C36 Si2 C26 105.93(10) . . ? C16 Si2 C26 112.64(10) . . ? Si2 C16 H16A 109.5 . . ? Si2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si2 C26 H26A 109.5 . . ? Si2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si2 C36 H36A 109.5 . . ? Si2 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? Si2 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N3 Si3 C37 116.37(8) . . ? N3 Si3 C27 110.97(8) . . ? C37 Si3 C27 108.53(10) . . ? N3 Si3 C17 110.49(8) . . ? C37 Si3 C17 102.78(9) . . ? C27 Si3 C17 107.05(9) . . ? Si3 C17 H17A 109.5 . . ? Si3 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si3 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si3 C27 H27A 109.5 . . ? Si3 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si3 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si3 C37 H37A 109.5 . . ? Si3 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? Si3 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? P1 N4 Si4 145.49(9) . . ? P1 N4 Mo1 88.57(6) . . ? Si4 N4 Mo1 125.22(7) . . ? N4 Si4 C18 114.39(9) . . ? N4 Si4 C28 109.39(10) . . ? C18 Si4 C28 108.16(12) . . ? N4 Si4 C38 109.74(10) . . ? C18 Si4 C38 107.01(13) . . ? C28 Si4 C38 107.95(16) . . ? Si4 C18 H18A 109.5 . . ? Si4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si4 C28 H28A 109.5 . . ? Si4 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si4 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si4 C38 H38A 109.5 . . ? Si4 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Si4 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C13 O3 P1 120.85(11) . . ? O3 C13 C23 107.27(17) . . ? O3 C13 C33 107.12(17) . . ? C23 C13 C33 113.4(2) . . ? O3 C13 H13 109.6 . . ? C23 C13 H13 109.6 . . ? C33 C13 H13 109.6 . . ? C13 C23 H23A 109.5 . . ? C13 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C13 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C13 C33 H33A 109.5 . . ? C13 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C13 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 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 N1 Mo1 O1 C11A 13.8(5) . . . . ? O2 Mo1 O1 C11A -92.9(5) . . . . ? Mo1 O1 C11A C21A 133.5(5) . . . . ? Mo1 O1 C11A C31A -111.4(7) . . . . ? N1 Mo1 O2 C12A 2.2(6) . . . . ? O1 Mo1 O2 C12A 110.4(5) . . . . ? Mo1 O2 C12A C22A -96.1(8) . . . . ? Mo1 O2 C12A C32A 150.9(5) . . . . ? N4 P1 N2 Si1 -172.40(11) . . . . ? O3 P1 N2 Si1 66.06(12) . . . . ? N3 P1 N2 Si1 -42.38(13) . . . . ? N4 P1 N2 Mo1 8.89(8) . . . . ? O3 P1 N2 Mo1 -112.64(6) . . . . ? N3 P1 N2 Mo1 138.92(6) . . . . ? N1 Mo1 N2 P1 178.86(7) . . . . ? O1 Mo1 N2 P1 71.78(7) . . . . ? O2 Mo1 N2 P1 -73.67(8) . . . . ? N1 Mo1 N2 Si1 -0.03(10) . . . . ? O1 Mo1 N2 Si1 -107.11(8) . . . . ? O2 Mo1 N2 Si1 107.44(8) . . . . ? P1 N2 Si1 C25 114.63(12) . . . . ? Mo1 N2 Si1 C25 -66.88(11) . . . . ? P1 N2 Si1 C35 -5.80(14) . . . . ? Mo1 N2 Si1 C35 172.69(9) . . . . ? P1 N2 Si1 C15 -125.64(12) . . . . ? Mo1 N2 Si1 C15 52.85(11) . . . . ? N4 P1 N3 Si2 52.48(11) . . . . ? O3 P1 N3 Si2 177.19(8) . . . . ? N2 P1 N3 Si2 -67.75(10) . . . . ? Mo1 P1 N3 Si2 -23.43(12) . . . . ? N4 P1 N3 Si3 -114.89(9) . . . . ? O3 P1 N3 Si3 9.82(10) . . . . ? N2 P1 N3 Si3 124.89(8) . . . . ? Mo1 P1 N3 Si3 169.21(4) . . . . ? P1 N3 Si2 C36 9.06(12) . . . . ? Si3 N3 Si2 C36 176.67(9) . . . . ? P1 N3 Si2 C16 -108.73(10) . . . . ? Si3 N3 Si2 C16 58.88(11) . . . . ? P1 N3 Si2 C26 127.19(10) . . . . ? Si3 N3 Si2 C26 -65.21(11) . . . . ? P1 N3 Si3 C37 -60.75(12) . . . . ? Si2 N3 Si3 C37 132.09(10) . . . . ? P1 N3 Si3 C27 64.00(12) . . . . ? Si2 N3 Si3 C27 -103.17(10) . . . . ? P1 N3 Si3 C17 -177.41(9) . . . . ? Si2 N3 Si3 C17 15.42(11) . . . . ? O3 P1 N4 Si4 -58.67(17) . . . . ? N2 P1 N4 Si4 -176.20(15) . . . . ? N3 P1 N4 Si4 57.74(18) . . . . ? Mo1 P1 N4 Si4 -169.10(18) . . . . ? O3 P1 N4 Mo1 110.44(6) . . . . ? N2 P1 N4 Mo1 -7.10(6) . . . . ? N3 P1 N4 Mo1 -133.15(6) . . . . ? N1 Mo1 N4 P1 22.5(2) . . . . ? O1 Mo1 N4 P1 -110.78(6) . . . . ? O2 Mo1 N4 P1 135.94(6) . . . . ? N1 Mo1 N4 Si4 -165.05(18) . . . . ? O1 Mo1 N4 Si4 61.69(9) . . . . ? O2 Mo1 N4 Si4 -51.59(9) . . . . ? P1 N4 Si4 C18 -9.4(2) . . . . ? Mo1 N4 Si4 C18 -176.06(11) . . . . ? P1 N4 Si4 C28 112.05(18) . . . . ? Mo1 N4 Si4 C28 -54.57(13) . . . . ? P1 N4 Si4 C38 -129.69(18) . . . . ? Mo1 N4 Si4 C38 63.68(14) . . . . ? Mo1 Mo11 Si4 N4 20.0(14) . . . . ? N4 P1 O3 C13 -47.15(16) . . . . ? N2 P1 O3 C13 66.07(15) . . . . ? N3 P1 O3 C13 -175.38(14) . . . . ? P1 O3 C13 C23 -117.85(16) . . . . ? P1 O3 C13 C33 120.05(16) . . . . ? 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 C37 H37A O3 0.98 2.42 3.029(2) 119.9 . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.84 _refine_diff_density_min -0.34 _refine_diff_density_rms 0.079 # start Validation Reply Form _vrf_PLAT242_5c ; PROBLEM: Check Low Ueq as Compared to Neighbors for C13A RESPONSE: The thermal parameter is affected by the disorder of the whole t-Bu group ; # end Validation Reply Form