data_compound3b _audit_creation_date 2009-07-27T11:45:44-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C33 H39 Mo2 O4 P1' _chemical_formula_sum 'C33 H39 Mo2 O4 P' _chemical_formula_weight 722.49 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.403(2) _cell_length_b 15.504(3) _cell_length_c 15.517(3) _cell_angle_alpha 84.337(3) _cell_angle_beta 72.189(3) _cell_angle_gamma 83.307(3) _cell_volume 3042.2(9) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 1290 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 26.155 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.577 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.913 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'BRUKER Sadabs' _exptl_absorpt_correction_T_min 0.808 _exptl_absorpt_correction_T_max 0.938 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_monochromador graphite _diffrn_measurement_device_type 'Smart-CCD-1000 BRUKER' _diffrn_measurement_method 'omega scans' _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0579 _diffrn_reflns_av_unetI/netI 0.0835 _diffrn_reflns_number 32980 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 26.43 _diffrn_reflns_theta_full 26.43 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.985 _reflns_number_total 12335 _reflns_number_gt 7844 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Brucker Smart' _computing_cell_refinement 'Brucker Smart' _computing_data_reduction 'Brucker Smart' _computing_structure_solution 'DIRDIF (1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0568P)^2^+0.0975P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 12335 _refine_ls_number_parameters 728 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0898 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1392 _refine_ls_wR_factor_gt 0.1109 _refine_ls_goodness_of_fit_ref 1.166 _refine_ls_restrained_S_all 1.166 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.274 _refine_diff_density_min -1.714 _refine_diff_density_rms 0.186 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.04927(4) 0.35374(4) -0.28693(4) 0.02150(14) Uani 1 1 d . . . Mo2 Mo 0.28523(4) 0.26076(3) -0.33268(4) 0.02062(14) Uani 1 1 d . . . P1 P 0.21576(12) 0.41117(10) -0.29848(11) 0.0207(4) Uani 1 1 d . . . O1 O -0.0132(4) 0.4976(3) -0.1474(3) 0.0438(13) Uani 1 1 d . . . O2 O 0.0021(4) 0.2341(3) -0.1091(3) 0.0425(13) Uani 1 1 d . . . O3 O 0.2716(4) 0.2468(3) -0.5267(3) 0.0312(11) Uani 1 1 d . . . O4 O 0.4648(4) 0.3728(3) -0.4475(4) 0.0447(13) Uani 1 1 d . . . C1 C 0.0113(5) 0.4449(4) -0.1998(5) 0.0308(16) Uani 1 1 d . . . C2 C 0.0222(5) 0.2793(5) -0.1745(4) 0.0294(16) Uani 1 1 d . . . C3 C 0.2755(5) 0.2546(4) -0.4542(4) 0.0259(15) Uani 1 1 d . . . C4 C 0.3990(5) 0.3322(4) -0.4027(5) 0.0309(16) Uani 1 1 d . . . C5 C -0.0922(5) 0.3018(4) -0.3211(4) 0.0270(15) Uani 1 1 d . . . H5 H -0.1336 0.2616 -0.2819 0.032 Uiso 1 1 calc R . . C6 C -0.0009(5) 0.2821(4) -0.3945(4) 0.0246(15) Uani 1 1 d . . . H6 H 0.028 0.2265 -0.4114 0.029 Uiso 1 1 calc R . . C7 C 0.0390(5) 0.3617(4) -0.4378(4) 0.0265(15) Uani 1 1 d . . . H7 H 0.0981 0.3678 -0.4878 0.032 Uiso 1 1 calc R . . C8 C -0.0290(5) 0.4303(4) -0.3896(5) 0.0300(16) Uani 1 1 d . . . H8 H -0.0221 0.4895 -0.4029 0.036 Uiso 1 1 calc R . . C9 C -0.1089(5) 0.3929(4) -0.3181(5) 0.0357(18) Uani 1 1 d . . . H9 H -0.1632 0.4234 -0.2763 0.043 Uiso 1 1 calc R . . C10 C 0.4107(5) 0.1534(4) -0.3088(5) 0.0313(16) Uani 1 1 d . . . H10 H 0.4794 0.1544 -0.3467 0.038 Uiso 1 1 calc R . . C11 C 0.3678(5) 0.1956(4) -0.2262(5) 0.0311(16) Uani 1 1 d . . . H11 H 0.4042 0.2279 -0.2003 0.037 Uiso 1 1 calc R . . C12 C 0.2608(5) 0.1801(4) -0.1902(4) 0.0273(15) Uani 1 1 d . . . H12 H 0.214 0.2007 -0.137 0.033 Uiso 1 1 calc R . . C13 C 0.2374(6) 0.1271(4) -0.2504(4) 0.0290(16) Uani 1 1 d . . . H13 H 0.1722 0.1074 -0.2431 0.035 Uiso 1 1 calc R . . C14 C 0.3298(6) 0.1093(4) -0.3233(4) 0.0295(16) Uani 1 1 d . . . C15 C 0.3406(6) 0.0529(4) -0.3988(5) 0.0341(17) Uani 1 1 d . . . H15A H 0.387 0.0781 -0.4541 0.041 Uiso 1 1 calc R . . H15B H 0.2722 0.0525 -0.4079 0.041 Uiso 1 1 calc R . . C16 C 0.3830(5) -0.0395(4) -0.3830(5) 0.0295(16) Uani 1 1 d . . . C17 C 0.3923(6) -0.0994(5) -0.4470(5) 0.0380(18) Uani 1 1 d . . . H17 H 0.3713 -0.0812 -0.4982 0.046 Uiso 1 1 calc R . . C18 C 0.4311(6) -0.1839(5) -0.4368(5) 0.044(2) Uani 1 1 d . . . H18 H 0.4381 -0.222 -0.4814 0.053 Uiso 1 1 calc R . . C19 C 0.4600(6) -0.2125(5) -0.3598(6) 0.044(2) Uani 1 1 d . . . H19 H 0.4852 -0.2703 -0.3516 0.053 Uiso 1 1 calc R . . C20 C 0.4513(5) -0.1549(5) -0.2959(5) 0.0406(19) Uani 1 1 d . . . H20 H 0.4709 -0.1739 -0.2442 0.049 Uiso 1 1 calc R . . C21 C 0.4140(6) -0.0695(5) -0.3070(5) 0.0397(18) Uani 1 1 d . . . H21 H 0.4094 -0.0313 -0.263 0.048 Uiso 1 1 calc R . . C22 C 0.2430(5) 0.4518(4) -0.1989(4) 0.0181(13) Uani 1 1 d . . . H22 H 0.1986 0.5065 -0.1851 0.022 Uiso 1 1 calc R . . C23 C 0.2149(5) 0.3920(4) -0.1130(4) 0.0244(15) Uani 1 1 d . . . H23A H 0.2569 0.3366 -0.1239 0.029 Uiso 1 1 calc R . . H23B H 0.1414 0.3813 -0.0974 0.029 Uiso 1 1 calc R . . C24 C 0.2344(5) 0.4319(5) -0.0334(4) 0.0310(16) Uani 1 1 d . . . H24A H 0.1889 0.4853 -0.0196 0.037 Uiso 1 1 calc R . . H24B H 0.2175 0.3918 0.02 0.037 Uiso 1 1 calc R . . C25 C 0.3490(6) 0.4512(5) -0.0570(4) 0.0347(17) Uani 1 1 d . . . H25A H 0.3941 0.3972 -0.0662 0.042 Uiso 1 1 calc R . . H25B H 0.3595 0.4782 -0.0071 0.042 Uiso 1 1 calc R . . C26 C 0.3786(5) 0.5115(4) -0.1425(4) 0.0311(16) Uani 1 1 d . . . H26A H 0.4525 0.5206 -0.1581 0.037 Uiso 1 1 calc R . . H26B H 0.3381 0.5675 -0.1312 0.037 Uiso 1 1 calc R . . C27 C 0.3576(5) 0.4737(4) -0.2223(4) 0.0279(15) Uani 1 1 d . . . H27A H 0.4044 0.4213 -0.2385 0.033 Uiso 1 1 calc R . . H27B H 0.3726 0.5154 -0.2744 0.033 Uiso 1 1 calc R . . C28 C 0.2556(5) 0.5023(4) -0.3859(4) 0.0218(14) Uani 1 1 d . . . H28 H 0.3306 0.5067 -0.3951 0.026 Uiso 1 1 calc R . . C29 C 0.2443(5) 0.4878(4) -0.4785(4) 0.0264(15) Uani 1 1 d . . . H29A H 0.2791 0.4315 -0.4977 0.032 Uiso 1 1 calc R . . H29B H 0.1704 0.4881 -0.4737 0.032 Uiso 1 1 calc R . . C30 C 0.2928(6) 0.5591(4) -0.5490(4) 0.0316(16) Uani 1 1 d . . . H30A H 0.2835 0.5498 -0.6069 0.038 Uiso 1 1 calc R . . H30B H 0.3677 0.5563 -0.5568 0.038 Uiso 1 1 calc R . . C31 C 0.2412(6) 0.6487(4) -0.5193(4) 0.0332(17) Uani 1 1 d . . . H31A H 0.2776 0.6931 -0.562 0.04 Uiso 1 1 calc R . . H31B H 0.1687 0.6542 -0.5203 0.04 Uiso 1 1 calc R . . C32 C 0.2435(6) 0.6636(4) -0.4260(4) 0.0318(17) Uani 1 1 d . . . H32A H 0.2037 0.7186 -0.4077 0.038 Uiso 1 1 calc R . . H32B H 0.3156 0.6677 -0.4274 0.038 Uiso 1 1 calc R . . C33 C 0.1981(6) 0.5916(4) -0.3568(4) 0.0312(16) Uani 1 1 d . . . H33A H 0.1238 0.5913 -0.3504 0.037 Uiso 1 1 calc R . . H33B H 0.2048 0.6022 -0.2983 0.037 Uiso 1 1 calc R . . Mo3 Mo 0.15360(4) 0.02379(3) 0.31254(3) 0.01904(14) Uani 1 1 d . . . Mo4 Mo 0.23909(4) 0.02759(3) 0.09323(3) 0.01850(13) Uani 1 1 d . . . P2 P 0.15015(12) 0.14204(10) 0.19534(10) 0.0180(3) Uani 1 1 d . . . O51 O -0.0296(4) -0.0807(3) 0.3134(3) 0.0435(13) Uani 1 1 d . . . O52 O -0.0345(4) 0.1566(3) 0.4025(3) 0.0418(13) Uani 1 1 d . . . O53 O 0.4647(4) -0.0023(3) 0.1135(3) 0.0337(11) Uani 1 1 d . . . O54 O 0.3340(4) 0.1970(3) -0.0090(3) 0.0318(11) Uani 1 1 d . . . C51 C 0.0385(5) -0.0398(4) 0.3104(5) 0.0310(16) Uani 1 1 d . . . C52 C 0.0360(6) 0.1087(4) 0.3677(5) 0.0327(17) Uani 1 1 d . . . C53 C 0.3799(6) 0.0105(4) 0.1066(4) 0.0244(15) Uani 1 1 d . . . C54 C 0.2972(5) 0.1340(5) 0.0307(4) 0.0252(15) Uani 1 1 d . . . C55 C 0.3236(5) 0.0128(4) 0.3306(4) 0.0307(16) Uani 1 1 d . . . H55 H 0.3795 0.0366 0.2867 0.037 Uiso 1 1 calc R . . C56 C 0.2520(6) 0.0549(4) 0.4047(4) 0.0326(17) Uani 1 1 d . . . H56 H 0.2528 0.1117 0.4189 0.039 Uiso 1 1 calc R . . C57 C 0.1792(5) -0.0043(5) 0.4533(4) 0.0309(16) Uani 1 1 d . . . H57 H 0.1223 0.0074 0.5041 0.037 Uiso 1 1 calc R . . C58 C 0.2068(6) -0.0839(4) 0.4123(4) 0.0316(16) Uani 1 1 d . . . H58 H 0.1736 -0.1348 0.4319 0.038 Uiso 1 1 calc R . . C59 C 0.2936(5) -0.0719(4) 0.3364(5) 0.0307(16) Uani 1 1 d . . . H59 H 0.3269 -0.1139 0.2956 0.037 Uiso 1 1 calc R . . C60 C 0.2547(5) -0.0230(4) -0.0456(4) 0.0284(16) Uani 1 1 d . . . H60 H 0.3039 0.0002 -0.0964 0.034 Uiso 1 1 calc R . . C61 C 0.1480(6) 0.0123(4) -0.0090(4) 0.0338(18) Uani 1 1 d . . . H61 H 0.115 0.0611 -0.0321 0.041 Uiso 1 1 calc R . . C62 C 0.1033(5) -0.0405(4) 0.0678(4) 0.0255(15) Uani 1 1 d . . . H62 H 0.0345 -0.033 0.1055 0.031 Uiso 1 1 calc R . . C63 C 0.1806(5) -0.1077(4) 0.0786(4) 0.0259(15) Uani 1 1 d . . . H63 H 0.1711 -0.151 0.1256 0.031 Uiso 1 1 calc R . . C64 C 0.2729(5) -0.0987(4) 0.0080(4) 0.0253(15) Uani 1 1 d . . . C65 C 0.3732(5) -0.1611(4) -0.0129(4) 0.0329(17) Uani 1 1 d . . . H65A H 0.3827 -0.1861 -0.0701 0.04 Uiso 1 1 calc R . . H65B H 0.4329 -0.1283 -0.0202 0.04 Uiso 1 1 calc R . . C66 C 0.3728(6) -0.2339(4) 0.0590(4) 0.0300(16) Uani 1 1 d . . . C67 C 0.4062(5) -0.2226(4) 0.1329(4) 0.0314(16) Uani 1 1 d . . . H67 H 0.4315 -0.1701 0.1365 0.038 Uiso 1 1 calc R . . C68 C 0.4030(6) -0.2869(4) 0.2011(5) 0.0374(18) Uani 1 1 d . . . H68 H 0.4224 -0.2767 0.2516 0.045 Uiso 1 1 calc R . . C69 C 0.3711(6) -0.3661(5) 0.1942(5) 0.0408(19) Uani 1 1 d . . . H69 H 0.3727 -0.4111 0.2382 0.049 Uiso 1 1 calc R . . C70 C 0.3368(6) -0.3784(5) 0.1221(5) 0.045(2) Uani 1 1 d . . . H70 H 0.3114 -0.431 0.1191 0.054 Uiso 1 1 calc R . . C71 C 0.3394(6) -0.3132(5) 0.0536(5) 0.0392(19) Uani 1 1 d . . . H71 H 0.3185 -0.3232 0.0038 0.047 Uiso 1 1 calc R . . C72 C 0.2177(5) 0.2396(4) 0.1980(4) 0.0250(15) Uani 1 1 d . . . H72 H 0.2194 0.2751 0.1418 0.03 Uiso 1 1 calc R . . C73 C 0.3324(4) 0.2210(4) 0.1988(4) 0.0180(13) Uani 1 1 d . . . H73A H 0.3707 0.1829 0.1512 0.022 Uiso 1 1 calc R . . H73B H 0.3348 0.192 0.2566 0.022 Uiso 1 1 calc R . . C74 C 0.3837(5) 0.3070(4) 0.1837(4) 0.0256(15) Uani 1 1 d . . . H74A H 0.4567 0.2952 0.1829 0.031 Uiso 1 1 calc R . . H74B H 0.3824 0.3353 0.1254 0.031 Uiso 1 1 calc R . . C75 C 0.3258(5) 0.3673(4) 0.2585(4) 0.0318(17) Uani 1 1 d . . . H75A H 0.3349 0.3421 0.3157 0.038 Uiso 1 1 calc R . . H75B H 0.356 0.4228 0.2452 0.038 Uiso 1 1 calc R . . C76 C 0.2104(5) 0.3818(4) 0.2672(5) 0.0318(16) Uani 1 1 d . . . H76A H 0.2013 0.4169 0.2143 0.038 Uiso 1 1 calc R . . H76B H 0.175 0.4143 0.3201 0.038 Uiso 1 1 calc R . . C77 C 0.1581(5) 0.2972(4) 0.2759(4) 0.0301(16) Uani 1 1 d . . . H77A H 0.0859 0.3109 0.2751 0.036 Uiso 1 1 calc R . . H77B H 0.157 0.2658 0.3334 0.036 Uiso 1 1 calc R . . C78 C 0.0221(5) 0.1955(4) 0.1847(4) 0.0236(14) Uani 1 1 d . . . H78 H -0.0082 0.2309 0.2371 0.028 Uiso 1 1 calc R . . C79 C 0.0324(5) 0.2579(4) 0.0999(4) 0.0231(14) Uani 1 1 d . . . H79A H 0.0821 0.2995 0.0976 0.028 Uiso 1 1 calc R . . H79B H 0.0598 0.2251 0.0462 0.028 Uiso 1 1 calc R . . C80 C -0.0729(5) 0.3066(4) 0.0999(5) 0.0322(17) Uani 1 1 d . . . H80A H -0.0956 0.3452 0.1493 0.039 Uiso 1 1 calc R . . H80B H -0.0641 0.3423 0.0435 0.039 Uiso 1 1 calc R . . C81 C -0.1572(5) 0.2459(4) 0.1103(5) 0.0323(17) Uani 1 1 d . . . H81A H -0.1405 0.2144 0.0559 0.039 Uiso 1 1 calc R . . H81B H -0.2243 0.2799 0.1168 0.039 Uiso 1 1 calc R . . C82 C -0.1666(5) 0.1812(4) 0.1921(5) 0.0328(17) Uani 1 1 d . . . H82A H -0.2162 0.14 0.1932 0.039 Uiso 1 1 calc R . . H82B H -0.1931 0.2119 0.2473 0.039 Uiso 1 1 calc R . . C83 C -0.0593(5) 0.1322(4) 0.1881(5) 0.0287(16) Uani 1 1 d . . . H83A H -0.0349 0.0988 0.1348 0.034 Uiso 1 1 calc R . . H83B H -0.0666 0.0919 0.2412 0.034 Uiso 1 1 calc R . . H1 H 0.132(5) 0.263(4) -0.293(4) 0.034 Uiso 1 1 d . . . H2 H 0.208(6) -0.025(5) 0.194(5) 0.06(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0179(3) 0.0249(3) 0.0227(3) -0.0023(2) -0.0065(2) -0.0037(2) Mo2 0.0211(3) 0.0198(3) 0.0233(3) -0.0035(2) -0.0095(2) -0.0014(2) P1 0.0168(8) 0.0221(9) 0.0243(9) -0.0041(7) -0.0066(7) -0.0032(7) O1 0.028(3) 0.052(3) 0.053(3) -0.029(3) -0.007(2) -0.003(2) O2 0.050(3) 0.063(4) 0.019(3) 0.020(3) -0.014(2) -0.030(3) O3 0.042(3) 0.028(3) 0.030(3) -0.006(2) -0.018(2) -0.003(2) O4 0.031(3) 0.036(3) 0.060(4) -0.011(3) 0.003(3) -0.012(2) C1 0.024(4) 0.032(4) 0.041(4) -0.008(3) -0.011(3) -0.016(3) C2 0.027(4) 0.047(5) 0.018(4) -0.005(3) -0.009(3) -0.016(3) C3 0.028(4) 0.021(4) 0.031(4) 0.002(3) -0.011(3) -0.006(3) C4 0.029(4) 0.023(4) 0.045(4) -0.014(3) -0.014(3) 0.000(3) C5 0.021(4) 0.042(4) 0.021(3) 0.005(3) -0.011(3) -0.008(3) C6 0.039(4) 0.028(4) 0.013(3) 0.005(3) -0.018(3) -0.007(3) C7 0.023(4) 0.030(4) 0.032(4) -0.004(3) -0.016(3) -0.005(3) C8 0.025(4) 0.025(4) 0.047(4) -0.007(3) -0.020(3) 0.000(3) C9 0.017(4) 0.034(4) 0.062(5) -0.009(4) -0.019(4) 0.000(3) C10 0.031(4) 0.031(4) 0.035(4) -0.007(3) -0.016(3) 0.007(3) C11 0.031(4) 0.030(4) 0.037(4) -0.004(3) -0.019(3) 0.005(3) C12 0.028(4) 0.030(4) 0.026(4) -0.003(3) -0.013(3) 0.002(3) C13 0.043(4) 0.028(4) 0.018(3) 0.007(3) -0.013(3) -0.004(3) C14 0.048(5) 0.021(4) 0.027(4) 0.002(3) -0.026(3) 0.005(3) C15 0.044(4) 0.030(4) 0.033(4) -0.005(3) -0.020(3) 0.001(3) C16 0.025(4) 0.025(4) 0.035(4) 0.001(3) -0.005(3) -0.003(3) C17 0.038(4) 0.036(4) 0.038(4) -0.008(3) -0.009(4) 0.002(3) C18 0.054(5) 0.026(4) 0.047(5) -0.010(4) -0.007(4) -0.001(4) C19 0.027(4) 0.022(4) 0.069(6) 0.008(4) 0.003(4) -0.002(3) C20 0.032(4) 0.029(4) 0.063(5) 0.004(4) -0.021(4) 0.001(3) C21 0.040(5) 0.038(4) 0.044(5) 0.000(4) -0.017(4) 0.000(4) C22 0.024(3) 0.017(3) 0.017(3) -0.004(2) -0.009(3) -0.004(3) C23 0.027(4) 0.032(4) 0.015(3) -0.002(3) -0.007(3) -0.002(3) C24 0.035(4) 0.042(4) 0.018(3) -0.004(3) -0.007(3) -0.007(3) C25 0.052(5) 0.040(4) 0.017(3) -0.003(3) -0.015(3) -0.007(4) C26 0.028(4) 0.032(4) 0.040(4) -0.013(3) -0.016(3) -0.004(3) C27 0.030(4) 0.029(4) 0.029(4) -0.006(3) -0.013(3) -0.004(3) C28 0.034(4) 0.013(3) 0.019(3) 0.000(3) -0.007(3) -0.006(3) C29 0.041(4) 0.025(4) 0.016(3) 0.002(3) -0.011(3) -0.011(3) C30 0.042(4) 0.034(4) 0.021(4) 0.004(3) -0.010(3) -0.014(3) C31 0.042(4) 0.031(4) 0.030(4) 0.010(3) -0.016(3) -0.011(3) C32 0.045(5) 0.021(4) 0.032(4) 0.006(3) -0.019(3) -0.001(3) C33 0.048(5) 0.022(4) 0.025(4) -0.005(3) -0.013(3) 0.004(3) Mo3 0.0199(3) 0.0183(3) 0.0190(3) -0.0006(2) -0.0056(2) -0.0036(2) Mo4 0.0179(3) 0.0200(3) 0.0187(3) -0.0035(2) -0.0057(2) -0.0034(2) P2 0.0152(8) 0.0178(8) 0.0211(8) -0.0021(7) -0.0049(7) -0.0028(6) O51 0.045(3) 0.038(3) 0.059(4) 0.011(3) -0.030(3) -0.019(3) O52 0.041(3) 0.033(3) 0.035(3) 0.004(2) 0.007(2) 0.007(2) O53 0.026(3) 0.037(3) 0.043(3) -0.001(2) -0.019(2) 0.002(2) O54 0.042(3) 0.040(3) 0.011(2) 0.008(2) -0.005(2) -0.014(2) C51 0.026(4) 0.022(4) 0.045(4) 0.000(3) -0.011(3) 0.000(3) C52 0.042(5) 0.025(4) 0.026(4) 0.006(3) -0.004(3) -0.008(3) C53 0.048(5) 0.022(3) 0.004(3) 0.005(2) -0.009(3) -0.010(3) C54 0.011(3) 0.047(4) 0.016(3) -0.009(3) -0.002(3) 0.003(3) C55 0.033(4) 0.041(4) 0.026(4) 0.009(3) -0.020(3) -0.014(3) C56 0.061(5) 0.019(4) 0.032(4) 0.003(3) -0.033(4) -0.012(3) C57 0.030(4) 0.045(5) 0.019(3) 0.002(3) -0.010(3) 0.000(3) C58 0.047(5) 0.023(4) 0.027(4) 0.012(3) -0.015(3) -0.012(3) C59 0.033(4) 0.026(4) 0.038(4) 0.000(3) -0.019(3) 0.001(3) C60 0.033(4) 0.038(4) 0.015(3) -0.012(3) -0.002(3) -0.013(3) C61 0.057(5) 0.029(4) 0.027(4) -0.002(3) -0.029(4) -0.004(4) C62 0.013(3) 0.032(4) 0.033(4) -0.010(3) -0.009(3) -0.002(3) C63 0.034(4) 0.020(3) 0.028(4) -0.010(3) -0.010(3) -0.010(3) C64 0.035(4) 0.024(4) 0.022(3) -0.005(3) -0.013(3) -0.004(3) C65 0.040(4) 0.037(4) 0.019(4) -0.005(3) -0.006(3) 0.001(3) C66 0.042(4) 0.024(4) 0.021(4) -0.002(3) -0.006(3) -0.002(3) C67 0.031(4) 0.028(4) 0.036(4) 0.005(3) -0.011(3) -0.007(3) C68 0.038(4) 0.028(4) 0.049(5) -0.004(4) -0.016(4) -0.003(3) C69 0.036(4) 0.037(5) 0.038(4) 0.003(4) 0.002(4) 0.004(4) C70 0.062(6) 0.045(5) 0.027(4) -0.001(4) -0.007(4) -0.019(4) C71 0.066(5) 0.030(4) 0.027(4) -0.005(3) -0.021(4) -0.003(4) C72 0.021(3) 0.026(4) 0.027(4) 0.000(3) -0.008(3) 0.004(3) C73 0.019(3) 0.017(3) 0.020(3) -0.002(2) -0.008(3) -0.001(3) C74 0.027(4) 0.026(4) 0.026(4) 0.003(3) -0.009(3) -0.008(3) C75 0.045(4) 0.028(4) 0.029(4) 0.002(3) -0.016(3) -0.018(3) C76 0.033(4) 0.020(4) 0.043(4) -0.012(3) -0.007(3) -0.006(3) C77 0.032(4) 0.031(4) 0.024(4) -0.003(3) -0.003(3) -0.005(3) C78 0.022(3) 0.029(4) 0.019(3) -0.004(3) -0.006(3) -0.001(3) C79 0.018(3) 0.032(4) 0.020(3) -0.002(3) -0.007(3) -0.001(3) C80 0.038(4) 0.025(4) 0.037(4) -0.005(3) -0.020(3) 0.008(3) C81 0.022(4) 0.036(4) 0.048(5) -0.012(3) -0.023(3) 0.006(3) C82 0.014(3) 0.035(4) 0.049(5) -0.007(3) -0.007(3) -0.001(3) C83 0.031(4) 0.017(3) 0.041(4) 0.002(3) -0.017(3) -0.002(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C2 1.954(7) . ? Mo1 C1 1.968(7) . ? Mo1 C9 2.317(6) . ? Mo1 C8 2.325(6) . ? Mo1 C5 2.362(6) . ? Mo1 C7 2.376(6) . ? Mo1 C6 2.387(6) . ? Mo1 P1 2.4476(17) . ? Mo1 Mo2 3.2171(9) . ? Mo1 H1 1.68(6) . ? Mo2 C3 1.942(7) . ? Mo2 C4 1.968(7) . ? Mo2 C10 2.312(6) . ? Mo2 C11 2.347(6) . ? Mo2 C14 2.356(6) . ? Mo2 C13 2.371(6) . ? Mo2 C12 2.381(6) . ? Mo2 P1 2.4541(17) . ? Mo2 H1 1.95(6) . ? P1 C28 1.865(6) . ? P1 C22 1.873(6) . ? O1 C1 1.158(7) . ? O2 C2 1.154(7) . ? O3 C3 1.159(7) . ? O4 C4 1.152(8) . ? C5 C9 1.407(9) . ? C5 C6 1.421(9) . ? C5 H5 0.93 . ? C6 C7 1.426(8) . ? C6 H6 0.93 . ? C7 C8 1.426(9) . ? C7 H7 0.93 . ? C8 C9 1.415(9) . ? C8 H8 0.93 . ? C9 H9 0.93 . ? C10 C11 1.424(9) . ? C10 C14 1.431(9) . ? C10 H10 0.93 . ? C11 C12 1.411(9) . ? C11 H11 0.93 . ? C12 C13 1.428(9) . ? C12 H12 0.93 . ? C13 C14 1.419(9) . ? C13 H13 0.93 . ? C14 C15 1.493(9) . ? C15 C16 1.503(9) . ? C15 H15A 0.97 . ? C15 H15B 0.97 . ? C16 C21 1.388(9) . ? C16 C17 1.394(9) . ? C17 C18 1.365(9) . ? C17 H17 0.93 . ? C18 C19 1.382(10) . ? C18 H18 0.93 . ? C19 C20 1.369(10) . ? C19 H19 0.93 . ? C20 C21 1.374(9) . ? C20 H20 0.93 . ? C21 H21 0.93 . ? C22 C23 1.519(8) . ? C22 C27 1.537(8) . ? C22 H22 0.98 . ? C23 C24 1.538(8) . ? C23 H23A 0.97 . ? C23 H23B 0.97 . ? C24 C25 1.524(9) . ? C24 H24A 0.97 . ? C24 H24B 0.97 . ? C25 C26 1.521(9) . ? C25 H25A 0.97 . ? C25 H25B 0.97 . ? C26 C27 1.533(8) . ? C26 H26A 0.97 . ? C26 H26B 0.97 . ? C27 H27A 0.97 . ? C27 H27B 0.97 . ? C28 C29 1.531(8) . ? C28 C33 1.541(8) . ? C28 H28 0.98 . ? C29 C30 1.527(8) . ? C29 H29A 0.97 . ? C29 H29B 0.97 . ? C30 C31 1.527(9) . ? C30 H30A 0.97 . ? C30 H30B 0.97 . ? C31 C32 1.497(9) . ? C31 H31A 0.97 . ? C31 H31B 0.97 . ? C32 C33 1.515(9) . ? C32 H32A 0.97 . ? C32 H32B 0.97 . ? C33 H33A 0.97 . ? C33 H33B 0.97 . ? Mo3 C51 1.936(7) . ? Mo3 C52 1.966(7) . ? Mo3 C57 2.305(6) . ? Mo3 C56 2.336(6) . ? Mo3 C59 2.351(6) . ? Mo3 C55 2.364(6) . ? Mo3 C58 2.362(6) . ? Mo3 P2 2.4586(17) . ? Mo3 Mo4 3.2385(10) . ? Mo3 H2 1.95(7) . ? Mo4 C53 1.946(7) . ? Mo4 C54 1.947(7) . ? Mo4 C60 2.307(6) . ? Mo4 C61 2.321(6) . ? Mo4 C62 2.356(6) . ? Mo4 C63 2.377(6) . ? Mo4 C64 2.394(6) . ? Mo4 P2 2.4468(17) . ? Mo4 H2 1.65(7) . ? P2 C72 1.861(6) . ? P2 C78 1.864(6) . ? O51 C51 1.157(8) . ? O52 C52 1.157(8) . ? O53 C53 1.166(7) . ? O54 C54 1.176(7) . ? C55 C59 1.405(9) . ? C55 C56 1.412(9) . ? C55 H55 0.93 . ? C56 C57 1.409(9) . ? C56 H56 0.93 . ? C57 C58 1.403(9) . ? C57 H57 0.93 . ? C58 C59 1.394(9) . ? C58 H58 0.93 . ? C59 H59 0.93 . ? C60 C64 1.413(9) . ? C60 C61 1.431(9) . ? C60 H60 0.93 . ? C61 C62 1.390(9) . ? C61 H61 0.93 . ? C62 C63 1.417(8) . ? C62 H62 0.93 . ? C63 C64 1.390(9) . ? C63 H63 0.93 . ? C64 C65 1.530(9) . ? C65 C66 1.506(9) . ? C65 H65A 0.97 . ? C65 H65B 0.97 . ? C66 C71 1.375(9) . ? C66 C67 1.385(9) . ? C67 C68 1.374(9) . ? C67 H67 0.93 . ? C68 C69 1.370(10) . ? C68 H68 0.93 . ? C69 C70 1.371(10) . ? C69 H69 0.93 . ? C70 C71 1.388(10) . ? C70 H70 0.93 . ? C71 H71 0.93 . ? C72 C77 1.533(8) . ? C72 C73 1.534(8) . ? C72 H72 0.98 . ? C73 C74 1.536(8) . ? C73 H73A 0.97 . ? C73 H73B 0.97 . ? C74 C75 1.522(9) . ? C74 H74A 0.97 . ? C74 H74B 0.97 . ? C75 C76 1.504(9) . ? C75 H75A 0.97 . ? C75 H75B 0.97 . ? C76 C77 1.534(8) . ? C76 H76A 0.97 . ? C76 H76B 0.97 . ? C77 H77A 0.97 . ? C77 H77B 0.97 . ? C78 C83 1.537(8) . ? C78 C79 1.535(8) . ? C78 H78 0.98 . ? C79 C80 1.521(8) . ? C79 H79A 0.97 . ? C79 H79B 0.97 . ? C80 C81 1.515(9) . ? C80 H80A 0.97 . ? C80 H80B 0.97 . ? C81 C82 1.520(9) . ? C81 H81A 0.97 . ? C81 H81B 0.97 . ? C82 C83 1.533(8) . ? C82 H82A 0.97 . ? C82 H82B 0.97 . ? C83 H83A 0.97 . ? C83 H83B 0.97 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Mo1 C1 81.2(3) . . ? C2 Mo1 C9 108.5(3) . . ? C1 Mo1 C9 88.6(3) . . ? C2 Mo1 C8 143.9(3) . . ? C1 Mo1 C8 95.5(3) . . ? C9 Mo1 C8 35.5(2) . . ? C2 Mo1 C5 90.6(2) . . ? C1 Mo1 C5 116.0(2) . . ? C9 Mo1 C5 35.0(2) . . ? C8 Mo1 C5 58.4(2) . . ? C2 Mo1 C7 142.6(2) . . ? C1 Mo1 C7 129.2(3) . . ? C9 Mo1 C7 58.8(2) . . ? C8 Mo1 C7 35.3(2) . . ? C5 Mo1 C7 58.4(2) . . ? C2 Mo1 C6 107.7(2) . . ? C1 Mo1 C6 146.8(2) . . ? C9 Mo1 C6 58.1(2) . . ? C8 Mo1 C6 58.1(2) . . ? C5 Mo1 C6 34.8(2) . . ? C7 Mo1 C6 34.8(2) . . ? C2 Mo1 P1 103.33(18) . . ? C1 Mo1 P1 75.07(19) . . ? C9 Mo1 P1 141.42(18) . . ? C8 Mo1 P1 110.48(17) . . ? C5 Mo1 P1 163.71(16) . . ? C7 Mo1 P1 105.51(16) . . ? C6 Mo1 P1 130.28(16) . . ? C2 Mo1 Mo2 85.3(2) . . ? C1 Mo1 Mo2 116.97(19) . . ? C9 Mo1 Mo2 152.96(19) . . ? C8 Mo1 Mo2 126.55(17) . . ? C5 Mo1 Mo2 125.45(16) . . ? C7 Mo1 Mo2 95.95(16) . . ? C6 Mo1 Mo2 95.89(16) . . ? P1 Mo1 Mo2 49.07(4) . . ? C2 Mo1 H1 66(2) . . ? C1 Mo1 H1 131(2) . . ? C9 Mo1 H1 135(2) . . ? C8 Mo1 H1 133(2) . . ? C5 Mo1 H1 101(2) . . ? C7 Mo1 H1 97(2) . . ? C6 Mo1 H1 81(2) . . ? P1 Mo1 H1 78(2) . . ? Mo2 Mo1 H1 30(2) . . ? C3 Mo2 C4 79.8(3) . . ? C3 Mo2 C10 108.6(2) . . ? C4 Mo2 C10 89.1(3) . . ? C3 Mo2 C11 144.2(3) . . ? C4 Mo2 C11 97.1(3) . . ? C10 Mo2 C11 35.6(2) . . ? C3 Mo2 C14 90.2(2) . . ? C4 Mo2 C14 116.2(3) . . ? C10 Mo2 C14 35.7(2) . . ? C11 Mo2 C14 58.9(2) . . ? C3 Mo2 C13 107.6(2) . . ? C4 Mo2 C13 147.6(3) . . ? C10 Mo2 C13 58.5(2) . . ? C11 Mo2 C13 58.0(2) . . ? C14 Mo2 C13 34.9(2) . . ? C3 Mo2 C12 142.6(2) . . ? C4 Mo2 C12 130.4(2) . . ? C10 Mo2 C12 58.7(2) . . ? C11 Mo2 C12 34.7(2) . . ? C14 Mo2 C12 58.6(2) . . ? C13 Mo2 C12 35.0(2) . . ? C3 Mo2 P1 102.72(19) . . ? C4 Mo2 P1 75.07(19) . . ? C10 Mo2 P1 141.61(17) . . ? C11 Mo2 P1 110.99(17) . . ? C14 Mo2 P1 164.50(17) . . ? C13 Mo2 P1 130.64(17) . . ? C12 Mo2 P1 106.19(16) . . ? C3 Mo2 Mo1 85.67(19) . . ? C4 Mo2 Mo1 116.70(19) . . ? C10 Mo2 Mo1 152.83(18) . . ? C11 Mo2 Mo1 125.83(17) . . ? C14 Mo2 Mo1 125.11(18) . . ? C13 Mo2 Mo1 95.54(17) . . ? C12 Mo2 Mo1 95.79(16) . . ? P1 Mo2 Mo1 48.89(4) . . ? C3 Mo2 H1 85.7(17) . . ? C4 Mo2 H1 140.9(17) . . ? C10 Mo2 H1 130.0(18) . . ? C11 Mo2 H1 115.1(17) . . ? C14 Mo2 H1 99.8(18) . . ? C13 Mo2 H1 71.5(17) . . ? C12 Mo2 H1 80.7(17) . . ? P1 Mo2 H1 73.1(18) . . ? Mo1 Mo2 H1 25.3(18) . . ? C28 P1 C22 101.2(3) . . ? C28 P1 Mo1 116.2(2) . . ? C22 P1 Mo1 122.45(19) . . ? C28 P1 Mo2 120.2(2) . . ? C22 P1 Mo2 115.61(19) . . ? Mo1 P1 Mo2 82.04(5) . . ? O1 C1 Mo1 178.4(6) . . ? O2 C2 Mo1 176.7(5) . . ? O3 C3 Mo2 176.7(6) . . ? O4 C4 Mo2 176.7(6) . . ? C9 C5 C6 107.9(6) . . ? C9 C5 Mo1 70.8(4) . . ? C6 C5 Mo1 73.6(3) . . ? C9 C5 H5 126 . . ? C6 C5 H5 126 . . ? Mo1 C5 H5 121.4 . . ? C5 C6 C7 108.5(6) . . ? C5 C6 Mo1 71.6(3) . . ? C7 C6 Mo1 72.2(3) . . ? C5 C6 H6 125.8 . . ? C7 C6 H6 125.8 . . ? Mo1 C6 H6 122.1 . . ? C8 C7 C6 106.8(6) . . ? C8 C7 Mo1 70.4(4) . . ? C6 C7 Mo1 73.0(3) . . ? C8 C7 H7 126.6 . . ? C6 C7 H7 126.6 . . ? Mo1 C7 H7 121.8 . . ? C9 C8 C7 108.5(6) . . ? C9 C8 Mo1 71.9(4) . . ? C7 C8 Mo1 74.3(4) . . ? C9 C8 H8 125.8 . . ? C7 C8 H8 125.8 . . ? Mo1 C8 H8 119.8 . . ? C5 C9 C8 108.3(6) . . ? C5 C9 Mo1 74.2(4) . . ? C8 C9 Mo1 72.5(4) . . ? C5 C9 H9 125.8 . . ? C8 C9 H9 125.8 . . ? Mo1 C9 H9 119.2 . . ? C11 C10 C14 108.2(6) . . ? C11 C10 Mo2 73.5(4) . . ? C14 C10 Mo2 73.8(4) . . ? C11 C10 H10 125.9 . . ? C14 C10 H10 125.9 . . ? Mo2 C10 H10 118.6 . . ? C12 C11 C10 108.5(6) . . ? C12 C11 Mo2 74.0(4) . . ? C10 C11 Mo2 70.9(4) . . ? C12 C11 H11 125.8 . . ? C10 C11 H11 125.8 . . ? Mo2 C11 H11 121.1 . . ? C11 C12 C13 107.4(6) . . ? C11 C12 Mo2 71.3(4) . . ? C13 C12 Mo2 72.1(3) . . ? C11 C12 H12 126.3 . . ? C13 C12 H12 126.3 . . ? Mo2 C12 H12 122 . . ? C14 C13 C12 109.0(6) . . ? C14 C13 Mo2 71.9(4) . . ? C12 C13 Mo2 72.9(4) . . ? C14 C13 H13 125.5 . . ? C12 C13 H13 125.5 . . ? Mo2 C13 H13 121.4 . . ? C13 C14 C10 106.9(6) . . ? C13 C14 C15 126.2(6) . . ? C10 C14 C15 126.9(6) . . ? C13 C14 Mo2 73.1(4) . . ? C10 C14 Mo2 70.5(4) . . ? C15 C14 Mo2 123.1(4) . . ? C14 C15 C16 114.2(5) . . ? C14 C15 H15A 108.7 . . ? C16 C15 H15A 108.7 . . ? C14 C15 H15B 108.7 . . ? C16 C15 H15B 108.7 . . ? H15A C15 H15B 107.6 . . ? C21 C16 C17 117.1(6) . . ? C21 C16 C15 123.4(6) . . ? C17 C16 C15 119.4(6) . . ? C18 C17 C16 122.1(7) . . ? C18 C17 H17 118.9 . . ? C16 C17 H17 118.9 . . ? C17 C18 C19 119.7(7) . . ? C17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? C20 C19 C18 119.2(7) . . ? C20 C19 H19 120.4 . . ? C18 C19 H19 120.4 . . ? C19 C20 C21 121.1(7) . . ? C19 C20 H20 119.5 . . ? C21 C20 H20 119.5 . . ? C20 C21 C16 120.8(7) . . ? C20 C21 H21 119.6 . . ? C16 C21 H21 119.6 . . ? C23 C22 C27 110.4(5) . . ? C23 C22 P1 114.6(4) . . ? C27 C22 P1 111.5(4) . . ? C23 C22 H22 106.6 . . ? C27 C22 H22 106.6 . . ? P1 C22 H22 106.6 . . ? C22 C23 C24 111.4(5) . . ? C22 C23 H23A 109.3 . . ? C24 C23 H23A 109.3 . . ? C22 C23 H23B 109.3 . . ? C24 C23 H23B 109.3 . . ? H23A C23 H23B 108 . . ? C25 C24 C23 110.4(5) . . ? C25 C24 H24A 109.6 . . ? C23 C24 H24A 109.6 . . ? C25 C24 H24B 109.6 . . ? C23 C24 H24B 109.6 . . ? H24A C24 H24B 108.1 . . ? C24 C25 C26 110.6(5) . . ? C24 C25 H25A 109.5 . . ? C26 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? C26 C25 H25B 109.5 . . ? H25A C25 H25B 108.1 . . ? C25 C26 C27 111.4(5) . . ? C25 C26 H26A 109.3 . . ? C27 C26 H26A 109.3 . . ? C25 C26 H26B 109.3 . . ? C27 C26 H26B 109.3 . . ? H26A C26 H26B 108 . . ? C26 C27 C22 111.6(5) . . ? C26 C27 H27A 109.3 . . ? C22 C27 H27A 109.3 . . ? C26 C27 H27B 109.3 . . ? C22 C27 H27B 109.3 . . ? H27A C27 H27B 108 . . ? C29 C28 C33 108.2(5) . . ? C29 C28 P1 114.2(4) . . ? C33 C28 P1 113.8(4) . . ? C29 C28 H28 106.7 . . ? C33 C28 H28 106.7 . . ? P1 C28 H28 106.7 . . ? C30 C29 C28 110.6(5) . . ? C30 C29 H29A 109.5 . . ? C28 C29 H29A 109.5 . . ? C30 C29 H29B 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 108.1 . . ? C29 C30 C31 110.6(5) . . ? C29 C30 H30A 109.5 . . ? C31 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? C31 C30 H30B 109.5 . . ? H30A C30 H30B 108.1 . . ? C32 C31 C30 112.1(5) . . ? C32 C31 H31A 109.2 . . ? C30 C31 H31A 109.2 . . ? C32 C31 H31B 109.2 . . ? C30 C31 H31B 109.2 . . ? H31A C31 H31B 107.9 . . ? C31 C32 C33 112.4(5) . . ? C31 C32 H32A 109.1 . . ? C33 C32 H32A 109.1 . . ? C31 C32 H32B 109.1 . . ? C33 C32 H32B 109.1 . . ? H32A C32 H32B 107.9 . . ? C32 C33 C28 110.8(5) . . ? C32 C33 H33A 109.5 . . ? C28 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? C28 C33 H33B 109.5 . . ? H33A C33 H33B 108.1 . . ? C51 Mo3 C52 81.3(3) . . ? C51 Mo3 C57 108.0(3) . . ? C52 Mo3 C57 87.9(3) . . ? C51 Mo3 C56 143.3(3) . . ? C52 Mo3 C56 92.8(3) . . ? C57 Mo3 C56 35.3(2) . . ? C51 Mo3 C59 110.8(2) . . ? C52 Mo3 C59 145.3(3) . . ? C57 Mo3 C59 57.6(2) . . ? C56 Mo3 C59 57.6(2) . . ? C51 Mo3 C55 145.5(3) . . ? C52 Mo3 C55 125.7(3) . . ? C57 Mo3 C55 58.5(2) . . ? C56 Mo3 C55 34.9(2) . . ? C59 Mo3 C55 34.7(2) . . ? C51 Mo3 C58 92.1(3) . . ? C52 Mo3 C58 116.7(3) . . ? C57 Mo3 C58 35.0(2) . . ? C56 Mo3 C58 58.2(2) . . ? C59 Mo3 C58 34.4(2) . . ? C55 Mo3 C58 58.1(2) . . ? C51 Mo3 P2 101.8(2) . . ? C52 Mo3 P2 73.52(19) . . ? C57 Mo3 P2 141.89(18) . . ? C56 Mo3 P2 111.23(16) . . ? C59 Mo3 P2 130.94(17) . . ? C55 Mo3 P2 106.28(16) . . ? C58 Mo3 P2 164.14(18) . . ? C51 Mo3 Mo4 89.4(2) . . ? C52 Mo3 Mo4 117.82(19) . . ? C57 Mo3 Mo4 151.38(17) . . ? C56 Mo3 Mo4 124.44(18) . . ? C59 Mo3 Mo4 95.33(17) . . ? C55 Mo3 Mo4 94.32(16) . . ? C58 Mo3 Mo4 125.07(17) . . ? P2 Mo3 Mo4 48.53(4) . . ? C51 Mo3 H2 78(2) . . ? C52 Mo3 H2 135(2) . . ? C57 Mo3 H2 137(2) . . ? C56 Mo3 H2 126(2) . . ? C59 Mo3 H2 80(2) . . ? C55 Mo3 H2 92(2) . . ? C58 Mo3 H2 104(2) . . ? P2 Mo3 H2 72(2) . . ? Mo4 Mo3 H2 24(2) . . ? C53 Mo4 C54 79.1(2) . . ? C53 Mo4 C60 105.7(2) . . ? C54 Mo4 C60 89.0(2) . . ? C53 Mo4 C61 141.6(2) . . ? C54 Mo4 C61 93.9(2) . . ? C60 Mo4 C61 36.0(2) . . ? C53 Mo4 C62 145.3(2) . . ? C54 Mo4 C62 126.6(2) . . ? C60 Mo4 C62 58.2(2) . . ? C61 Mo4 C62 34.6(2) . . ? C53 Mo4 C63 110.6(2) . . ? C54 Mo4 C63 146.3(2) . . ? C60 Mo4 C63 57.4(2) . . ? C61 Mo4 C63 57.9(2) . . ? C62 Mo4 C63 34.8(2) . . ? C53 Mo4 C64 91.0(2) . . ? C54 Mo4 C64 117.6(2) . . ? C60 Mo4 C64 34.9(2) . . ? C61 Mo4 C64 58.7(2) . . ? C62 Mo4 C64 57.6(2) . . ? C63 Mo4 C64 33.9(2) . . ? C53 Mo4 P2 103.73(18) . . ? C54 Mo4 P2 75.24(18) . . ? C60 Mo4 P2 143.13(18) . . ? C61 Mo4 P2 110.92(18) . . ? C62 Mo4 P2 105.40(16) . . ? C63 Mo4 P2 129.28(16) . . ? C64 Mo4 P2 162.39(16) . . ? C53 Mo4 Mo3 86.52(16) . . ? C54 Mo4 Mo3 116.43(18) . . ? C60 Mo4 Mo3 153.77(16) . . ? C61 Mo4 Mo3 129.00(18) . . ? C62 Mo4 Mo3 98.67(16) . . ? C63 Mo4 Mo3 96.74(16) . . ? C64 Mo4 Mo3 124.25(15) . . ? P2 Mo4 Mo3 48.84(4) . . ? C53 Mo4 H2 82(2) . . ? C54 Mo4 H2 141(2) . . ? C60 Mo4 H2 129(2) . . ? C61 Mo4 H2 121(2) . . ? C62 Mo4 H2 86(2) . . ? C63 Mo4 H2 72(2) . . ? C64 Mo4 H2 96(2) . . ? P2 Mo4 H2 76(2) . . ? Mo3 Mo4 H2 28(2) . . ? C72 P2 C78 100.1(3) . . ? C72 P2 Mo4 120.6(2) . . ? C78 P2 Mo4 117.6(2) . . ? C72 P2 Mo3 116.9(2) . . ? C78 P2 Mo3 120.2(2) . . ? Mo4 P2 Mo3 82.63(5) . . ? O51 C51 Mo3 176.1(6) . . ? O52 C52 Mo3 177.6(6) . . ? O53 C53 Mo4 177.9(6) . . ? O54 C54 Mo4 178.1(6) . . ? C59 C55 C56 106.5(6) . . ? C59 C55 Mo3 72.2(4) . . ? C56 C55 Mo3 71.4(4) . . ? C59 C55 H55 126.8 . . ? C56 C55 H55 126.8 . . ? Mo3 C55 H55 121.5 . . ? C55 C56 C57 107.9(6) . . ? C55 C56 Mo3 73.6(3) . . ? C57 C56 Mo3 71.2(4) . . ? C55 C56 H56 126 . . ? C57 C56 H56 126 . . ? Mo3 C56 H56 120.9 . . ? C58 C57 C56 108.7(6) . . ? C58 C57 Mo3 74.7(4) . . ? C56 C57 Mo3 73.5(3) . . ? C58 C57 H57 125.7 . . ? C56 C57 H57 125.7 . . ? Mo3 C57 H57 118 . . ? C59 C58 C57 106.7(6) . . ? C59 C58 Mo3 72.4(4) . . ? C57 C58 Mo3 70.3(4) . . ? C59 C58 H58 126.6 . . ? C57 C58 H58 126.6 . . ? Mo3 C58 H58 122.4 . . ? C58 C59 C55 110.1(6) . . ? C58 C59 Mo3 73.2(4) . . ? C55 C59 Mo3 73.2(4) . . ? C58 C59 H59 124.9 . . ? C55 C59 H59 124.9 . . ? Mo3 C59 H59 120.3 . . ? C64 C60 C61 108.7(6) . . ? C64 C60 Mo4 75.9(4) . . ? C61 C60 Mo4 72.5(3) . . ? C64 C60 H60 125.6 . . ? C61 C60 H60 125.6 . . ? Mo4 C60 H60 117.8 . . ? C62 C61 C60 106.9(6) . . ? C62 C61 Mo4 74.1(3) . . ? C60 C61 Mo4 71.4(3) . . ? C62 C61 H61 126.5 . . ? C60 C61 H61 126.5 . . ? Mo4 C61 H61 119.8 . . ? C61 C62 C63 108.2(6) . . ? C61 C62 Mo4 71.3(4) . . ? C63 C62 Mo4 73.4(3) . . ? C61 C62 H62 125.9 . . ? C63 C62 H62 125.9 . . ? Mo4 C62 H62 121.1 . . ? C64 C63 C62 109.3(6) . . ? C64 C63 Mo4 73.7(4) . . ? C62 C63 Mo4 71.8(3) . . ? C64 C63 H63 125.4 . . ? C62 C63 H63 125.4 . . ? Mo4 C63 H63 120.9 . . ? C63 C64 C60 106.8(6) . . ? C63 C64 C65 127.4(6) . . ? C60 C64 C65 125.7(6) . . ? C63 C64 Mo4 72.4(4) . . ? C60 C64 Mo4 69.2(3) . . ? C65 C64 Mo4 126.4(4) . . ? C66 C65 C64 114.0(5) . . ? C66 C65 H65A 108.8 . . ? C64 C65 H65A 108.8 . . ? C66 C65 H65B 108.8 . . ? C64 C65 H65B 108.8 . . ? H65A C65 H65B 107.6 . . ? C71 C66 C67 118.0(6) . . ? C71 C66 C65 121.4(6) . . ? C67 C66 C65 120.6(6) . . ? C68 C67 C66 121.8(7) . . ? C68 C67 H67 119.1 . . ? C66 C67 H67 119.1 . . ? C69 C68 C67 119.6(7) . . ? C69 C68 H68 120.2 . . ? C67 C68 H68 120.2 . . ? C68 C69 C70 119.5(7) . . ? C68 C69 H69 120.2 . . ? C70 C69 H69 120.2 . . ? C69 C70 C71 120.7(7) . . ? C69 C70 H70 119.7 . . ? C71 C70 H70 119.7 . . ? C66 C71 C70 120.3(7) . . ? C66 C71 H71 119.9 . . ? C70 C71 H71 119.9 . . ? C77 C72 C73 108.7(5) . . ? C77 C72 P2 113.6(4) . . ? C73 C72 P2 115.3(4) . . ? C77 C72 H72 106.2 . . ? C73 C72 H72 106.2 . . ? P2 C72 H72 106.2 . . ? C72 C73 C74 109.5(5) . . ? C72 C73 H73A 109.8 . . ? C74 C73 H73A 109.8 . . ? C72 C73 H73B 109.8 . . ? C74 C73 H73B 109.8 . . ? H73A C73 H73B 108.2 . . ? C75 C74 C73 110.7(5) . . ? C75 C74 H74A 109.5 . . ? C73 C74 H74A 109.5 . . ? C75 C74 H74B 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 108.1 . . ? C76 C75 C74 111.4(5) . . ? C76 C75 H75A 109.3 . . ? C74 C75 H75A 109.3 . . ? C76 C75 H75B 109.3 . . ? C74 C75 H75B 109.3 . . ? H75A C75 H75B 108 . . ? C75 C76 C77 113.5(5) . . ? C75 C76 H76A 108.9 . . ? C77 C76 H76A 108.9 . . ? C75 C76 H76B 108.9 . . ? C77 C76 H76B 108.9 . . ? H76A C76 H76B 107.7 . . ? C76 C77 C72 110.8(5) . . ? C76 C77 H77A 109.5 . . ? C72 C77 H77A 109.5 . . ? C76 C77 H77B 109.5 . . ? C72 C77 H77B 109.5 . . ? H77A C77 H77B 108.1 . . ? C83 C78 C79 108.2(5) . . ? C83 C78 P2 114.5(4) . . ? C79 C78 P2 113.9(4) . . ? C83 C78 H78 106.5 . . ? C79 C78 H78 106.5 . . ? P2 C78 H78 106.5 . . ? C80 C79 C78 111.6(5) . . ? C80 C79 H79A 109.3 . . ? C78 C79 H79A 109.3 . . ? C80 C79 H79B 109.3 . . ? C78 C79 H79B 109.3 . . ? H79A C79 H79B 108 . . ? C81 C80 C79 112.5(5) . . ? C81 C80 H80A 109.1 . . ? C79 C80 H80A 109.1 . . ? C81 C80 H80B 109.1 . . ? C79 C80 H80B 109.1 . . ? H80A C80 H80B 107.8 . . ? C80 C81 C82 111.9(5) . . ? C80 C81 H81A 109.2 . . ? C82 C81 H81A 109.2 . . ? C80 C81 H81B 109.2 . . ? C82 C81 H81B 109.2 . . ? H81A C81 H81B 107.9 . . ? C81 C82 C83 110.5(5) . . ? C81 C82 H82A 109.5 . . ? C83 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? C83 C82 H82B 109.5 . . ? H82A C82 H82B 108.1 . . ? C82 C83 C78 111.1(5) . . ? C82 C83 H83A 109.4 . . ? C78 C83 H83A 109.4 . . ? C82 C83 H83B 109.4 . . ? C78 C83 H83B 109.4 . . ? H83A C83 H83B 108 . . ? #===END data_compound4 _audit_creation_date 2008-07-23T11:52:01-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C24 H27 Mo2 O7 P1' _chemical_formula_sum 'C24 H27 Mo2 O7 P' _chemical_formula_weight 650.31 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 15.2107(3) _cell_length_b 11.5579(2) _cell_length_c 17.7653(4) _cell_angle_alpha 90 _cell_angle_beta 125.1440(10) _cell_angle_gamma 90 _cell_volume 2553.87(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4783 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 25.350 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.691 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.085 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.8075 _exptl_absorpt_correction_T_max 0.8780 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _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 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_device '90 mm CCD camera on \k-goniostat' _diffrn_measurement_method 'CCD' _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_unetI/netI 0.0279 _diffrn_reflns_number 23604 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 25.35 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _reflns_number_total 4670 _reflns_number_gt 4283 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor, 1997) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0387P)^2^+0.9114P] 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_number_reflns 4670 _refine_ls_number_parameters 301 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0255 _refine_ls_R_factor_gt 0.0194 _refine_ls_wR_factor_ref 0.0756 _refine_ls_wR_factor_gt 0.0649 _refine_ls_goodness_of_fit_ref 1.284 _refine_ls_restrained_S_all 1.284 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.641 _refine_diff_density_min -0.834 _refine_diff_density_rms 0.226 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.857096(16) 0.815143(18) 0.334868(14) 0.01201(8) Uani 1 1 d . A . Mo2 Mo 0.745089(16) 0.841678(17) 0.117671(13) 0.01249(8) Uani 1 1 d . A . P1 P 0.71361(5) 0.70277(5) 0.21162(4) 0.01103(14) Uani 1 1 d . . . O1 O 0.71208(16) 0.81501(16) 0.40514(13) 0.0245(4) Uani 1 1 d . A . O2 O 0.78968(15) 1.07345(15) 0.31919(13) 0.0244(4) Uani 1 1 d . A . O3 O 0.90065(17) 0.65883(17) 0.11624(14) 0.0285(5) Uani 1 1 d . A . O4 O 0.53425(15) 0.71665(17) -0.05020(12) 0.0243(4) Uani 1 1 d . A . O5 O 0.94885(16) 1.00602(17) 0.23282(13) 0.0284(5) Uani 1 1 d . A . O6 O 0.59874(16) 1.05321(17) 0.10068(14) 0.0359(5) Uani 1 1 d . A . O7 O 0.7533(2) 0.9618(2) -0.03767(16) 0.0518(7) Uani 1 1 d . A . C1 C 0.7638(2) 0.8135(2) 0.37645(17) 0.0167(6) Uani 1 1 d . . . C2 C 0.8133(2) 0.9780(2) 0.32228(16) 0.0169(5) Uani 1 1 d . . . C3 C 0.8441(2) 0.7198(2) 0.11954(17) 0.0179(5) Uani 1 1 d . . . C4 C 0.6093(2) 0.7586(2) 0.01130(17) 0.0176(5) Uani 1 1 d . . . C5 C 0.8777(2) 0.9429(2) 0.20078(17) 0.0198(6) Uani 1 1 d . . . C6 C 0.6499(2) 0.9756(2) 0.10975(18) 0.0232(6) Uani 1 1 d . . . C7 C 0.7484(3) 0.9191(2) 0.01776(19) 0.0283(7) Uani 1 1 d . . . C8 C 0.9908(2) 0.6678(2) 0.39177(18) 0.0220(6) Uani 1 1 d . . . H8 H 0.9759 0.5946 0.3655 0.026 Uiso 1 1 calc R A . C9 C 1.0295(2) 0.7627(2) 0.36914(18) 0.0215(6) Uani 1 1 d . A . H9 H 1.0446 0.7629 0.3253 0.026 Uiso 1 1 calc R . . C10 C 1.0417(2) 0.8579(2) 0.42466(18) 0.0238(6) Uani 1 1 d . . . H10 H 1.0655 0.9315 0.4234 0.029 Uiso 1 1 calc R A . C11 C 1.0109(2) 0.8209(2) 0.48238(18) 0.0248(6) Uani 1 1 d . A . H11 H 1.0116 0.8657 0.5263 0.03 Uiso 1 1 calc R . . C12 C 0.9786(2) 0.7032(2) 0.46120(18) 0.0252(6) Uani 1 1 d . A . H12 H 0.9538 0.6575 0.4884 0.03 Uiso 1 1 calc R . . C13 C 0.75312(19) 0.5518(2) 0.20679(16) 0.0136(5) Uani 1 1 d . A . H13 H 0.8246 0.5595 0.2193 0.016 Uiso 1 1 calc R . . C14 C 0.7707(2) 0.4738(2) 0.28406(17) 0.0180(5) Uani 1 1 d . . . H14A H 0.8144 0.5142 0.3424 0.022 Uiso 1 1 calc R A . H14B H 0.702 0.4561 0.2732 0.022 Uiso 1 1 calc R . . C15 C 0.8264(2) 0.3620(2) 0.28846(19) 0.0236(6) Uani 1 1 d . A . H15A H 0.8979 0.3796 0.305 0.028 Uiso 1 1 calc R . . H15B H 0.834 0.3124 0.3359 0.028 Uiso 1 1 calc R . . C16 C 0.7637(2) 0.2984(2) 0.1972(2) 0.0238(6) Uani 1 1 d . . . H16A H 0.6956 0.2723 0.1841 0.029 Uiso 1 1 calc R A . H16B H 0.8039 0.2309 0.2008 0.029 Uiso 1 1 calc R . . C17 C 0.7432(3) 0.3770(3) 0.1199(2) 0.0352(8) Uani 1 1 d . A . H17A H 0.6996 0.336 0.0618 0.042 Uiso 1 1 calc R . . H17B H 0.8113 0.3958 0.1297 0.042 Uiso 1 1 calc R . . C18 C 0.6862(2) 0.4891(2) 0.11407(18) 0.0237(6) Uani 1 1 d . . . H18A H 0.6154 0.4717 0.099 0.028 Uiso 1 1 calc R A . H18B H 0.6776 0.5382 0.066 0.028 Uiso 1 1 calc R . . C21 C 0.5850(3) 0.6962(3) 0.2026(3) 0.0129(8) Uiso 0.7 1 d P A 1 H21 H 0.6041 0.6723 0.2633 0.015 Uiso 0.7 1 calc PR A 1 C22 C 0.5357(4) 0.8174(4) 0.1850(4) 0.0161(12) Uiso 0.7 1 d P A 1 H22A H 0.5901 0.8713 0.2292 0.019 Uiso 0.7 1 calc PR A 1 H22B H 0.5115 0.8429 0.1239 0.019 Uiso 0.7 1 calc PR A 1 C23 C 0.4409(3) 0.8183(3) 0.1930(3) 0.0200(8) Uiso 0.7 1 d P A 1 H23A H 0.4657 0.7973 0.2552 0.024 Uiso 0.7 1 calc PR A 1 H23B H 0.4108 0.8956 0.1808 0.024 Uiso 0.7 1 calc PR A 1 C24 C 0.3543(3) 0.7334(3) 0.1250(3) 0.0207(8) Uiso 0.7 1 d P A 1 H24A H 0.3233 0.7598 0.0626 0.025 Uiso 0.7 1 calc PR A 1 H24B H 0.2975 0.7307 0.1344 0.025 Uiso 0.7 1 calc PR A 1 C25 C 0.4016(3) 0.6118(3) 0.1376(3) 0.0204(8) Uiso 0.7 1 d P A 1 H25A H 0.4231 0.5815 0.1969 0.024 Uiso 0.7 1 calc PR A 1 H25B H 0.3464 0.5612 0.0903 0.024 Uiso 0.7 1 calc PR A 1 C26 C 0.4987(3) 0.6106(3) 0.1325(2) 0.0165(7) Uiso 0.7 1 d P A 1 H26A H 0.4759 0.6318 0.0709 0.02 Uiso 0.7 1 calc PR A 1 H26B H 0.5288 0.5333 0.1453 0.02 Uiso 0.7 1 calc PR A 1 C31 C 0.5661(7) 0.6958(7) 0.1655(8) 0.0129(19) Uiso 0.3 1 d P A 2 H31 H 0.5268 0.6623 0.1035 0.016 Uiso 0.3 1 calc PR A 2 C32 C 0.5489(7) 0.6182(8) 0.2245(6) 0.0214(19) Uiso 0.3 1 d P A 2 H32A H 0.5941 0.6441 0.2879 0.026 Uiso 0.3 1 calc PR A 2 H32B H 0.5696 0.5397 0.222 0.026 Uiso 0.3 1 calc PR A 2 C33 C 0.4308(8) 0.6197(8) 0.1914(7) 0.027(2) Uiso 0.3 1 d P A 2 H33A H 0.4225 0.5723 0.2319 0.032 Uiso 0.3 1 calc PR A 2 H33B H 0.3862 0.5872 0.1299 0.032 Uiso 0.3 1 calc PR A 2 C34 C 0.3932(8) 0.7453(8) 0.1902(7) 0.028(2) Uiso 0.3 1 d P A 2 H34A H 0.3183 0.7446 0.1683 0.034 Uiso 0.3 1 calc PR A 2 H34B H 0.4351 0.7765 0.2522 0.034 Uiso 0.3 1 calc PR A 2 C35 C 0.4065(8) 0.8189(8) 0.1303(7) 0.023(2) Uiso 0.3 1 d P A 2 H35A H 0.3862 0.8975 0.1331 0.028 Uiso 0.3 1 calc PR A 2 H35B H 0.3584 0.7922 0.0673 0.028 Uiso 0.3 1 calc PR A 2 C36 C 0.5224(8) 0.8188(8) 0.1573(8) 0.009(2) Uiso 0.3 1 d P A 2 H36A H 0.5685 0.8583 0.2157 0.011 Uiso 0.3 1 calc PR A 2 H36B H 0.5246 0.8614 0.1114 0.011 Uiso 0.3 1 calc PR A 2 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 0.01339(13) 0.01195(13) 0.01095(13) -0.00066(7) 0.00716(10) -0.00037(8) Mo2 0.01528(13) 0.01030(13) 0.01015(13) 0.00058(7) 0.00631(10) -0.00017(8) P1 0.0114(3) 0.0094(3) 0.0141(3) -0.0001(2) 0.0084(3) -0.0005(2) O1 0.0289(11) 0.0303(11) 0.0217(10) -0.0017(8) 0.0189(9) -0.0035(8) O2 0.0318(11) 0.0134(10) 0.0278(10) -0.0032(8) 0.0171(9) -0.0005(8) O3 0.0319(12) 0.0330(12) 0.0276(11) 0.0092(9) 0.0211(10) 0.0142(9) O4 0.0195(10) 0.0254(10) 0.0192(10) -0.0045(8) 0.0060(9) -0.0024(8) O5 0.0305(11) 0.0308(11) 0.0278(10) -0.0050(9) 0.0189(9) -0.0160(9) O6 0.0310(11) 0.0172(10) 0.0379(12) -0.0040(9) 0.0072(10) 0.0091(9) O7 0.098(2) 0.0370(13) 0.0364(13) 0.0070(11) 0.0479(14) -0.0094(13) C1 0.0217(14) 0.0135(13) 0.0126(12) 0.0002(9) 0.0087(11) -0.0012(10) C2 0.0168(12) 0.0216(15) 0.0119(12) -0.0021(10) 0.0081(10) -0.0052(10) C3 0.0194(13) 0.0215(13) 0.0119(12) 0.0048(10) 0.0084(10) -0.0012(11) C4 0.0225(14) 0.0144(13) 0.0173(13) 0.0031(10) 0.0123(12) 0.0058(11) C5 0.0248(14) 0.0208(13) 0.0174(13) 0.0005(11) 0.0142(11) -0.0011(12) C6 0.0238(14) 0.0180(14) 0.0159(13) -0.0021(10) 0.0045(11) -0.0017(11) C7 0.0426(17) 0.0179(14) 0.0215(14) -0.0003(11) 0.0168(13) -0.0029(12) C8 0.0145(13) 0.0205(14) 0.0206(14) 0.0009(10) 0.0041(11) 0.0056(10) C9 0.0133(12) 0.0287(15) 0.0212(13) -0.0025(11) 0.0091(11) 0.0007(11) C10 0.0133(13) 0.0242(14) 0.0233(14) -0.0048(11) 0.0044(11) -0.0041(11) C11 0.0183(14) 0.0320(16) 0.0133(13) -0.0025(11) 0.0028(11) 0.0041(11) C12 0.0201(14) 0.0305(15) 0.0176(13) 0.0096(12) 0.0065(11) 0.0063(12) C13 0.0164(12) 0.0101(11) 0.0190(12) 0.0012(10) 0.0129(10) 0.0017(9) C14 0.0206(13) 0.0154(13) 0.0167(12) 0.0015(10) 0.0099(11) -0.0021(10) C15 0.0173(13) 0.0144(13) 0.0310(15) 0.0067(11) 0.0093(12) 0.0011(10) C16 0.0283(15) 0.0113(12) 0.0369(16) 0.0025(11) 0.0217(14) 0.0052(11) C17 0.067(2) 0.0169(15) 0.0385(18) -0.0003(12) 0.0399(18) 0.0090(14) C18 0.0414(16) 0.0139(13) 0.0171(13) 0.0002(10) 0.0176(12) 0.0041(12) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C1 1.941(3) . ? Mo1 C2 1.967(3) . ? Mo1 C11 2.299(3) . ? Mo1 C12 2.313(3) . ? Mo1 C10 2.348(3) . ? Mo1 C8 2.385(3) . ? Mo1 P1 2.3964(6) . ? Mo1 C9 2.404(3) . ? Mo1 Mo2 3.2120(3) . ? Mo2 C7 2.014(3) . ? Mo2 C5 2.047(3) . ? Mo2 C3 2.048(3) . ? Mo2 C4 2.065(3) . ? Mo2 C6 2.068(3) . ? Mo2 P1 2.5520(6) . ? P1 C13 1.863(2) . ? P1 C21 1.871(4) . ? P1 C31 1.896(9) . ? O1 C1 1.158(3) . ? O2 C2 1.151(3) . ? O3 C3 1.139(3) . ? O4 C4 1.139(3) . ? O5 C5 1.148(3) . ? O6 C6 1.137(3) . ? O7 C7 1.141(4) . ? C8 C9 1.409(4) . ? C8 C12 1.409(4) . ? C8 H8 0.93 . ? C9 C10 1.417(4) . ? C9 H9 0.93 . ? C10 C11 1.417(4) . ? C10 H10 0.93 . ? C11 C12 1.422(4) . ? C11 H11 0.93 . ? C12 H12 0.93 . ? C13 C14 1.531(3) . ? C13 C18 1.531(3) . ? C13 H13 0.98 . ? C14 C15 1.523(4) . ? C14 H14A 0.97 . ? C14 H14B 0.97 . ? C15 C16 1.516(4) . ? C15 H15A 0.97 . ? C15 H15B 0.97 . ? C16 C17 1.521(4) . ? C16 H16A 0.97 . ? C16 H16B 0.97 . ? C17 C18 1.529(4) . ? C17 H17A 0.97 . ? C17 H17B 0.97 . ? C18 H18A 0.97 . ? C18 H18B 0.97 . ? C21 C22 1.533(6) . ? C21 C26 1.540(5) . ? C21 H21 0.98 . ? C22 C23 1.528(6) . ? C22 H22A 0.97 . ? C22 H22B 0.97 . ? C23 C24 1.524(5) . ? C23 H23A 0.97 . ? C23 H23B 0.97 . ? C24 C25 1.536(5) . ? C24 H24A 0.97 . ? C24 H24B 0.97 . ? C25 C26 1.531(5) . ? C25 H25A 0.97 . ? C25 H25B 0.97 . ? C26 H26A 0.97 . ? C26 H26B 0.97 . ? C31 C32 1.512(13) . ? C31 C36 1.540(12) . ? C31 H31 0.98 . ? C32 C33 1.534(13) . ? C32 H32A 0.97 . ? C32 H32B 0.97 . ? C33 C34 1.556(14) . ? C33 H33A 0.97 . ? C33 H33B 0.97 . ? C34 C35 1.464(14) . ? C34 H34A 0.97 . ? C34 H34B 0.97 . ? C35 C36 1.538(13) . ? C35 H35A 0.97 . ? C35 H35B 0.97 . ? C36 H36A 0.97 . ? C36 H36B 0.97 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Mo1 C2 77.17(10) . . ? C1 Mo1 C11 93.06(11) . . ? C2 Mo1 C11 99.06(10) . . ? C1 Mo1 C12 88.64(11) . . ? C2 Mo1 C12 132.45(10) . . ? C11 Mo1 C12 35.91(10) . . ? C1 Mo1 C10 126.41(10) . . ? C2 Mo1 C10 94.02(10) . . ? C11 Mo1 C10 35.47(11) . . ? C12 Mo1 C10 58.92(10) . . ? C1 Mo1 C8 117.62(10) . . ? C2 Mo1 C8 151.89(10) . . ? C11 Mo1 C8 58.53(10) . . ? C12 Mo1 C8 34.87(10) . . ? C10 Mo1 C8 57.88(10) . . ? C1 Mo1 P1 82.05(8) . . ? C2 Mo1 P1 110.13(7) . . ? C11 Mo1 P1 148.34(7) . . ? C12 Mo1 P1 112.46(8) . . ? C10 Mo1 P1 147.01(7) . . ? C8 Mo1 P1 96.10(7) . . ? C1 Mo1 C9 146.25(10) . . ? C2 Mo1 C9 121.27(10) . . ? C11 Mo1 C9 58.19(10) . . ? C12 Mo1 C9 57.83(10) . . ? C10 Mo1 C9 34.67(9) . . ? C8 Mo1 C9 34.22(10) . . ? P1 Mo1 C9 112.46(7) . . ? C1 Mo1 Mo2 117.37(7) . . ? C2 Mo1 Mo2 82.03(7) . . ? C11 Mo1 Mo2 148.71(8) . . ? C12 Mo1 Mo2 142.56(8) . . ? C10 Mo1 Mo2 113.32(7) . . ? C8 Mo1 Mo2 108.09(7) . . ? P1 Mo1 Mo2 51.672(16) . . ? C9 Mo1 Mo2 94.31(7) . . ? C7 Mo2 C5 82.39(11) . . ? C7 Mo2 C3 85.90(11) . . ? C5 Mo2 C3 88.34(11) . . ? C7 Mo2 C4 85.36(11) . . ? C5 Mo2 C4 167.70(10) . . ? C3 Mo2 C4 91.92(10) . . ? C7 Mo2 C6 88.82(12) . . ? C5 Mo2 C6 88.98(10) . . ? C3 Mo2 C6 174.35(11) . . ? C4 Mo2 C6 89.64(10) . . ? C7 Mo2 P1 164.82(8) . . ? C5 Mo2 P1 111.46(7) . . ? C3 Mo2 P1 88.26(7) . . ? C4 Mo2 P1 80.84(7) . . ? C6 Mo2 P1 97.35(8) . . ? C7 Mo2 Mo1 146.73(8) . . ? C5 Mo2 Mo1 64.34(7) . . ? C3 Mo2 Mo1 92.19(7) . . ? C4 Mo2 Mo1 127.91(7) . . ? C6 Mo2 Mo1 91.13(7) . . ? P1 Mo2 Mo1 47.447(14) . . ? C13 P1 C21 107.91(14) . . ? C13 P1 C31 105.8(3) . . ? C13 P1 Mo1 113.66(8) . . ? C21 P1 Mo1 117.23(14) . . ? C31 P1 Mo1 130.3(3) . . ? C13 P1 Mo2 111.84(8) . . ? C21 P1 Mo2 123.40(13) . . ? C31 P1 Mo2 111.4(3) . . ? Mo1 P1 Mo2 80.881(19) . . ? O1 C1 Mo1 176.7(2) . . ? O2 C2 Mo1 176.9(2) . . ? O3 C3 Mo2 173.9(2) . . ? O4 C4 Mo2 176.7(2) . . ? O5 C5 Mo2 167.7(2) . . ? O6 C6 Mo2 174.7(3) . . ? O7 C7 Mo2 178.0(3) . . ? C9 C8 C12 108.1(2) . . ? C9 C8 Mo1 73.62(15) . . ? C12 C8 Mo1 69.77(15) . . ? C9 C8 H8 125.9 . . ? C12 C8 H8 125.9 . . ? Mo1 C8 H8 122.3 . . ? C8 C9 C10 108.3(3) . . ? C8 C9 Mo1 72.16(15) . . ? C10 C9 Mo1 70.52(15) . . ? C8 C9 H9 125.8 . . ? C10 C9 H9 125.8 . . ? Mo1 C9 H9 123.1 . . ? C11 C10 C9 107.7(2) . . ? C11 C10 Mo1 70.37(15) . . ? C9 C10 Mo1 74.81(15) . . ? C11 C10 H10 126.1 . . ? C9 C10 H10 126.1 . . ? Mo1 C10 H10 120.5 . . ? C10 C11 C12 107.8(3) . . ? C10 C11 Mo1 74.16(15) . . ? C12 C11 Mo1 72.58(15) . . ? C10 C11 H11 126.1 . . ? C12 C11 H11 126.1 . . ? Mo1 C11 H11 119 . . ? C8 C12 C11 108.1(3) . . ? C8 C12 Mo1 75.36(15) . . ? C11 C12 Mo1 71.51(15) . . ? C8 C12 H12 126 . . ? C11 C12 H12 126 . . ? Mo1 C12 H12 119 . . ? C14 C13 C18 110.5(2) . . ? C14 C13 P1 113.86(17) . . ? C18 C13 P1 117.43(17) . . ? C14 C13 H13 104.5 . . ? C18 C13 H13 104.5 . . ? P1 C13 H13 104.5 . . ? C15 C14 C13 110.5(2) . . ? C15 C14 H14A 109.5 . . ? C13 C14 H14A 109.5 . . ? C15 C14 H14B 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? C16 C15 C14 111.6(2) . . ? C16 C15 H15A 109.3 . . ? C14 C15 H15A 109.3 . . ? C16 C15 H15B 109.3 . . ? C14 C15 H15B 109.3 . . ? H15A C15 H15B 108 . . ? C15 C16 C17 110.6(2) . . ? C15 C16 H16A 109.5 . . ? C17 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? C16 C17 C18 112.4(2) . . ? C16 C17 H17A 109.1 . . ? C18 C17 H17A 109.1 . . ? C16 C17 H17B 109.1 . . ? C18 C17 H17B 109.1 . . ? H17A C17 H17B 107.9 . . ? C17 C18 C13 109.2(2) . . ? C17 C18 H18A 109.8 . . ? C13 C18 H18A 109.8 . . ? C17 C18 H18B 109.8 . . ? C13 C18 H18B 109.8 . . ? H18A C18 H18B 108.3 . . ? C22 C21 C26 109.4(3) . . ? C22 C21 P1 110.2(3) . . ? C26 C21 P1 117.2(3) . . ? C22 C21 H21 106.5 . . ? C26 C21 H21 106.5 . . ? P1 C21 H21 106.5 . . ? C23 C22 C21 111.3(3) . . ? C23 C22 H22A 109.4 . . ? C21 C22 H22A 109.4 . . ? C23 C22 H22B 109.4 . . ? C21 C22 H22B 109.4 . . ? H22A C22 H22B 108 . . ? C24 C23 C22 110.7(3) . . ? C24 C23 H23A 109.5 . . ? C22 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 108.1 . . ? C23 C24 C25 110.8(3) . . ? C23 C24 H24A 109.5 . . ? C25 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C25 C24 H24B 109.5 . . ? H24A C24 H24B 108.1 . . ? C26 C25 C24 112.7(3) . . ? C26 C25 H25A 109.1 . . ? C24 C25 H25A 109.1 . . ? C26 C25 H25B 109.1 . . ? C24 C25 H25B 109.1 . . ? H25A C25 H25B 107.8 . . ? C25 C26 C21 110.4(3) . . ? C25 C26 H26A 109.6 . . ? C21 C26 H26A 109.6 . . ? C25 C26 H26B 109.6 . . ? C21 C26 H26B 109.6 . . ? H26A C26 H26B 108.1 . . ? C32 C31 C36 112.0(8) . . ? C32 C31 P1 111.1(6) . . ? C36 C31 P1 109.9(6) . . ? C32 C31 H31 107.9 . . ? C36 C31 H31 107.9 . . ? P1 C31 H31 107.9 . . ? C31 C32 C33 111.0(7) . . ? C31 C32 H32A 109.4 . . ? C33 C32 H32A 109.4 . . ? C31 C32 H32B 109.4 . . ? C33 C32 H32B 109.4 . . ? H32A C32 H32B 108 . . ? C32 C33 C34 110.9(8) . . ? C32 C33 H33A 109.5 . . ? C34 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? C34 C33 H33B 109.5 . . ? H33A C33 H33B 108.1 . . ? C35 C34 C33 110.4(9) . . ? C35 C34 H34A 109.6 . . ? C33 C34 H34A 109.6 . . ? C35 C34 H34B 109.6 . . ? C33 C34 H34B 109.6 . . ? H34A C34 H34B 108.1 . . ? C34 C35 C36 112.7(8) . . ? C34 C35 H35A 109.1 . . ? C36 C35 H35A 109.1 . . ? C34 C35 H35B 109.1 . . ? C36 C35 H35B 109.1 . . ? H35A C35 H35B 107.8 . . ? C35 C36 C31 112.7(7) . . ? C35 C36 H36A 109.1 . . ? C31 C36 H36A 109.1 . . ? C35 C36 H36B 109.1 . . ? C31 C36 H36B 109.1 . . ? H36A C36 H36B 107.8 . . ? #===END data_compound6a _audit_creation_date 2008-04-11T14:37:08-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C24 H35 Mo2 N2 O3 P1' _chemical_formula_sum 'C24 H35 Mo2 N2 O3 P1' _chemical_formula_weight 622.39 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration unk #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c a 21' _symmetry_space_group_name_Hall 'P 2c -2ac' _symmetry_Int_Tables_number 29 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 9.903(5) _cell_length_b 27.514(5) _cell_length_c 17.963(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 90.000(5) _cell_volume 4894(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 12334 _cell_measurement_theta_min 2.9338 _cell_measurement_theta_max 73.6647 _cell_measurement_wavelength 1.5418 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.689 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2528 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 9.238 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.446 _exptl_absorpt_correction_T_max 0.83 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_type CuK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'ONYX CCD' _diffrn_measurement_method 'CCD' _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_unetI/netI 0.0209 _diffrn_reflns_number 17200 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 73.87 _diffrn_reflns_theta_full 70 _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 0.949 _reflns_number_total 8162 _reflns_number_gt 7604 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_structure_solution 'SIR-92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0516P)^2^+14.2617P] 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_number_reflns 8162 _refine_ls_number_parameters 580 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.0979 _refine_ls_wR_factor_gt 0.0958 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.282(15) _refine_diff_density_max 1.683 _refine_diff_density_min -0.772 _refine_diff_density_rms 0.104 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 1.12784(5) 0.37411(2) -0.18845(3) 0.02228(13) Uani 1 1 d . . . Mo2 Mo 1.39599(5) 0.39702(2) -0.10978(3) 0.02214(13) Uani 1 1 d . . . P1 P 1.19651(15) 0.36219(6) -0.05568(10) 0.0219(3) Uani 1 1 d . . . O1 O 0.9005(5) 0.3035(2) -0.1309(4) 0.0364(14) Uani 1 1 d . . . O2 O 1.2602(6) 0.2887(2) -0.2597(4) 0.0457(15) Uani 1 1 d . . . O3 O 1.3216(5) 0.50193(18) -0.1012(3) 0.0309(11) Uani 1 1 d . . . N2 N 1.2090(6) 0.3214(2) -0.2267(4) 0.0328(14) Uani 1 1 d . . . N3 N 1.3455(5) 0.4580(2) -0.1000(4) 0.0253(12) Uani 1 1 d . . . C1 C 0.9826(7) 0.3306(3) -0.1506(5) 0.0311(16) Uani 1 1 d . . . C2 C 1.4712(7) 0.3984(3) 0.0057(5) 0.0337(17) Uani 1 1 d . . . H2A H 1.5439 0.4214 0.0096 0.051 Uiso 1 1 calc R . . H2B H 1.503 0.3667 0.0193 0.051 Uiso 1 1 calc R . . H2C H 1.3994 0.4078 0.0386 0.051 Uiso 1 1 calc R . . C3 C 1.1374(7) 0.4200(3) -0.3001(4) 0.0268(15) Uani 1 1 d . . . H3 H 1.1895 0.4105 -0.3406 0.032 Uiso 1 1 calc R . . C4 C 1.1805(6) 0.4509(2) -0.2407(4) 0.0228(13) Uani 1 1 d . . . H4 H 1.2666 0.4638 -0.2348 0.027 Uiso 1 1 calc R . . C5 C 1.0693(6) 0.4585(2) -0.1923(5) 0.0280(14) Uani 1 1 d . . . H5 H 1.0686 0.4774 -0.1495 0.034 Uiso 1 1 calc R . . C6 C 0.9592(7) 0.4315(3) -0.2220(5) 0.0329(17) Uani 1 1 d . . . H6 H 0.8726 0.4306 -0.202 0.039 Uiso 1 1 calc R . . C7 C 1.0017(7) 0.4063(3) -0.2867(4) 0.0310(16) Uani 1 1 d . . . H7 H 0.9502 0.3848 -0.3149 0.037 Uiso 1 1 calc R . . C8 C 1.5581(7) 0.4124(3) -0.2049(4) 0.0314(16) Uani 1 1 d . . . H8 H 1.5609 0.4417 -0.2308 0.038 Uiso 1 1 calc R . . C9 C 1.4866(7) 0.3702(3) -0.2263(4) 0.0315(16) Uani 1 1 d . . . H9 H 1.4295 0.3674 -0.2672 0.038 Uiso 1 1 calc R . . C10 C 1.5173(7) 0.3326(3) -0.1741(5) 0.0321(16) Uani 1 1 d . . . H10 H 1.4861 0.3007 -0.1756 0.038 Uiso 1 1 calc R . . C11 C 1.6035(7) 0.3527(4) -0.1202(5) 0.038(2) Uani 1 1 d . . . H11 H 1.6404 0.3359 -0.0801 0.046 Uiso 1 1 calc R . . C12 C 1.6258(7) 0.4021(4) -0.1358(5) 0.0338(19) Uani 1 1 d . . . H12 H 1.6748 0.424 -0.107 0.041 Uiso 1 1 calc R . . C13 C 1.1966(6) 0.2991(3) -0.0176(4) 0.0234(14) Uani 1 1 d . . . H13 H 1.1057 0.292 0.0011 0.028 Uiso 1 1 calc R . . C14 C 1.2969(6) 0.2949(2) 0.0486(3) 0.0234(12) Uani 1 1 d . . . H14A H 1.3873 0.3023 0.0312 0.028 Uiso 1 1 calc R . . H14B H 1.2732 0.3187 0.0862 0.028 Uiso 1 1 calc R . . C15 C 1.2957(7) 0.2444(2) 0.0833(3) 0.0274(13) Uani 1 1 d . . . H15A H 1.363 0.2426 0.1224 0.033 Uiso 1 1 calc R . . H15B H 1.2079 0.238 0.1051 0.033 Uiso 1 1 calc R . . C16 C 1.3261(8) 0.2067(2) 0.0237(4) 0.0342(17) Uani 1 1 d . . . H16A H 1.4171 0.2119 0.0052 0.041 Uiso 1 1 calc R . . H16B H 1.3227 0.1746 0.0458 0.041 Uiso 1 1 calc R . . C17 C 1.2310(8) 0.2087(3) -0.0393(5) 0.0378(18) Uani 1 1 d . . . H17A H 1.1404 0.2016 -0.0219 0.045 Uiso 1 1 calc R . . H17B H 1.2556 0.1845 -0.076 0.045 Uiso 1 1 calc R . . C18 C 1.2344(8) 0.2597(3) -0.0750(5) 0.0377(18) Uani 1 1 d . . . H18A H 1.3241 0.2662 -0.0942 0.045 Uiso 1 1 calc R . . H18B H 1.1714 0.2609 -0.1163 0.045 Uiso 1 1 calc R . . C19 C 1.0957(6) 0.3937(3) 0.0179(4) 0.0210(14) Uani 1 1 d . . . H19 H 1.1218 0.3789 0.0654 0.025 Uiso 1 1 calc R . . C20 C 1.1237(6) 0.4484(3) 0.0254(5) 0.0260(16) Uani 1 1 d . . . H20A H 1.22 0.4537 0.0308 0.031 Uiso 1 1 calc R . . H20B H 1.0941 0.465 -0.0194 0.031 Uiso 1 1 calc R . . C21 C 1.0504(7) 0.4695(3) 0.0924(4) 0.0275(15) Uani 1 1 d . . . H21A H 1.069 0.5041 0.0956 0.033 Uiso 1 1 calc R . . H21B H 1.0839 0.4543 0.1375 0.033 Uiso 1 1 calc R . . C22 C 0.8989(7) 0.4616(3) 0.0865(5) 0.0291(17) Uani 1 1 d . . . H22A H 0.8555 0.4731 0.1316 0.035 Uiso 1 1 calc R . . H22B H 0.8636 0.4803 0.0451 0.035 Uiso 1 1 calc R . . C23 C 0.8657(7) 0.4081(3) 0.0752(5) 0.0321(18) Uani 1 1 d . . . H23A H 0.8883 0.3903 0.1201 0.039 Uiso 1 1 calc R . . H23B H 0.7695 0.4047 0.0667 0.039 Uiso 1 1 calc R . . C24 C 0.9411(6) 0.3866(3) 0.0105(4) 0.0257(14) Uani 1 1 d . . . H24A H 0.9103 0.4018 -0.0352 0.031 Uiso 1 1 calc R . . H24B H 0.9212 0.3522 0.0074 0.031 Uiso 1 1 calc R . . Mo1B Mo 0.89077(5) 0.12535(2) 0.33567(3) 0.02397(14) Uani 1 1 d . . . Mo2B Mo 0.62206(5) 0.10431(2) 0.25798(3) 0.02480(14) Uani 1 1 d . . . P1B P 0.82346(15) 0.13703(6) 0.20306(10) 0.0225(3) Uani 1 1 d . . . O1B O 1.1252(5) 0.1914(2) 0.2777(5) 0.0466(18) Uani 1 1 d . . . O2B O 0.7747(7) 0.2142(2) 0.4057(4) 0.0602(19) Uani 1 1 d . . . O3B O 0.6873(5) -0.00108(19) 0.2472(3) 0.0329(11) Uani 1 1 d . . . N2B N 0.8181(7) 0.1794(2) 0.3728(4) 0.0378(16) Uani 1 1 d . . . N3B N 0.6669(5) 0.0423(2) 0.2478(4) 0.0265(13) Uani 1 1 d . . . C1B C 1.0406(7) 0.1663(3) 0.2952(5) 0.0309(16) Uani 1 1 d . . . C2B C 0.5481(8) 0.1069(3) 0.1400(5) 0.040(2) Uani 1 1 d . . . H2B1 H 0.6042 0.0866 0.1094 0.06 Uiso 1 1 calc R . . H2B2 H 0.552 0.1398 0.1221 0.06 Uiso 1 1 calc R . . H2B3 H 0.4566 0.0955 0.1379 0.06 Uiso 1 1 calc R . . C31 C 0.8292(7) 0.0494(3) 0.3911(5) 0.0312(16) Uani 1 1 d . . . H31 H 0.7439 0.0355 0.3871 0.037 Uiso 1 1 calc R . . C32 C 0.8700(7) 0.0815(3) 0.4441(6) 0.041(2) Uani 1 1 d . . . H32 H 0.8149 0.0946 0.481 0.049 Uiso 1 1 calc R . . C33 C 1.0091(7) 0.0921(3) 0.4347(5) 0.0338(18) Uani 1 1 d . . . H33 H 1.0621 0.1119 0.4648 0.041 Uiso 1 1 calc R . . C34 C 1.0517(7) 0.0663(3) 0.3700(5) 0.0322(17) Uani 1 1 d . . . H34 H 1.1382 0.0665 0.3498 0.039 Uiso 1 1 calc R . . C35 C 0.9416(7) 0.0407(2) 0.3422(5) 0.0280(15) Uani 1 1 d . . . H35 H 0.9408 0.0215 0.2997 0.034 Uiso 1 1 calc R . . C36 C 0.5336(7) 0.1308(3) 0.3756(5) 0.0359(18) Uani 1 1 d . . . H36 H 0.5894 0.1335 0.4171 0.043 Uiso 1 1 calc R . . C37 C 0.4632(7) 0.0887(3) 0.3536(5) 0.0380(19) Uani 1 1 d . . . H37 H 0.4656 0.0586 0.3771 0.046 Uiso 1 1 calc R . . C38 C 0.3907(7) 0.1004(4) 0.2913(7) 0.046(3) Uani 1 1 d . . . H38 H 0.3334 0.0794 0.2659 0.055 Uiso 1 1 calc R . . C39 C 0.4161(8) 0.1501(4) 0.2710(6) 0.051(3) Uani 1 1 d . . . H39 H 0.38 0.1667 0.2305 0.061 Uiso 1 1 calc R . . C40 C 0.5050(7) 0.1685(3) 0.3237(6) 0.042(2) Uani 1 1 d . . . H40 H 0.5398 0.1999 0.3249 0.05 Uiso 1 1 calc R . . C41 C 0.9199(7) 0.1038(2) 0.1301(5) 0.0262(15) Uani 1 1 d . . . H41 H 0.8893 0.1172 0.0824 0.031 Uiso 1 1 calc R . . C42 C 1.0719(7) 0.1133(3) 0.1333(5) 0.0288(15) Uani 1 1 d . . . H42A H 1.109 0.0996 0.1786 0.035 Uiso 1 1 calc R . . H42B H 1.0887 0.1481 0.1337 0.035 Uiso 1 1 calc R . . C43 C 1.1419(7) 0.0900(3) 0.0646(5) 0.0309(16) Uani 1 1 d . . . H43A H 1.113 0.1068 0.0199 0.037 Uiso 1 1 calc R . . H43B H 1.2389 0.094 0.0691 0.037 Uiso 1 1 calc R . . C44 C 1.1100(6) 0.0367(3) 0.0571(6) 0.034(2) Uani 1 1 d . . . H44A H 1.1511 0.0192 0.0981 0.041 Uiso 1 1 calc R . . H44B H 1.149 0.0245 0.0112 0.041 Uiso 1 1 calc R . . C45 C 0.9596(7) 0.0269(3) 0.0568(5) 0.0364(18) Uani 1 1 d . . . H45A H 0.9436 -0.0079 0.0565 0.044 Uiso 1 1 calc R . . H45B H 0.9196 0.0406 0.0122 0.044 Uiso 1 1 calc R . . C46 C 0.8928(7) 0.0497(3) 0.1262(7) 0.040(2) Uani 1 1 d . . . H46A H 0.7961 0.0441 0.1244 0.048 Uiso 1 1 calc R . . H46B H 0.9277 0.0341 0.1706 0.048 Uiso 1 1 calc R . . C47 C 0.8272(7) 0.2016(3) 0.1695(5) 0.0299(16) Uani 1 1 d . . . H47 H 0.9187 0.2123 0.1824 0.036 Uiso 1 1 calc R . . C48 C 0.8242(10) 0.2063(3) 0.0848(5) 0.057(2) Uani 1 1 d . . . H48A H 0.7434 0.1909 0.0654 0.068 Uiso 1 1 calc R . . H48B H 0.902 0.1899 0.0636 0.068 Uiso 1 1 calc R . . C49 C 0.8260(10) 0.2603(3) 0.0622(6) 0.061(2) Uani 1 1 d . . . H49A H 0.8199 0.263 0.0085 0.074 Uiso 1 1 calc R . . H49B H 0.9101 0.2751 0.078 0.074 Uiso 1 1 calc R . . C50 C 0.7036(8) 0.2876(4) 0.0993(6) 0.072(4) Uani 1 1 d . . . H50A H 0.6194 0.2706 0.0907 0.086 Uiso 1 1 calc R . . H50B H 0.6958 0.3206 0.0807 0.086 Uiso 1 1 calc R . . C51 C 0.7433(16) 0.2870(3) 0.1844(6) 0.083(4) Uani 1 1 d . . . H51A H 0.8318 0.3014 0.1913 0.099 Uiso 1 1 calc R . . H51B H 0.6783 0.3056 0.2131 0.099 Uiso 1 1 calc R . . C52 C 0.7442(14) 0.2340(3) 0.2102(6) 0.074(4) Uani 1 1 d . . . H52A H 0.7728 0.2333 0.2618 0.088 Uiso 1 1 calc R . . H52B H 0.6523 0.2219 0.2084 0.088 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 0.0220(2) 0.0230(3) 0.0218(3) 0.0006(3) -0.00317(18) -0.00025(17) Mo2 0.0185(2) 0.0260(3) 0.0220(3) 0.0011(3) 0.00044(19) 0.00027(17) P1 0.0204(7) 0.0205(8) 0.0249(8) -0.0007(7) -0.0007(6) 0.0002(6) O1 0.037(3) 0.038(3) 0.033(3) 0.010(3) -0.007(2) -0.011(2) O2 0.072(4) 0.031(3) 0.034(3) -0.005(3) 0.001(3) 0.013(3) O3 0.034(2) 0.019(2) 0.039(3) -0.004(3) 0.006(2) -0.0036(17) N2 0.041(3) 0.034(3) 0.023(3) 0.002(3) -0.006(2) 0.006(2) N3 0.020(2) 0.031(3) 0.024(3) -0.001(3) 0.003(2) -0.004(2) C1 0.029(3) 0.029(3) 0.035(4) 0.000(3) -0.005(3) -0.005(3) C2 0.031(4) 0.044(4) 0.026(4) -0.003(3) -0.005(3) 0.003(3) C3 0.036(3) 0.034(4) 0.010(3) 0.002(3) 0.005(3) -0.009(3) C4 0.022(3) 0.023(3) 0.024(3) 0.005(3) -0.002(3) 0.001(2) C5 0.027(3) 0.026(3) 0.031(4) -0.004(3) 0.003(3) -0.002(2) C6 0.022(3) 0.037(4) 0.040(5) 0.010(4) 0.003(3) 0.000(3) C7 0.034(4) 0.036(4) 0.023(4) 0.005(3) -0.007(3) 0.001(3) C8 0.027(3) 0.038(4) 0.029(4) 0.000(3) 0.015(3) -0.002(3) C9 0.035(4) 0.033(4) 0.027(4) 0.001(3) 0.002(3) -0.003(3) C10 0.034(3) 0.023(3) 0.039(5) 0.001(3) 0.013(3) 0.008(3) C11 0.035(4) 0.048(5) 0.033(5) -0.002(4) 0.005(3) 0.013(3) C12 0.028(4) 0.048(5) 0.024(4) -0.003(4) 0.001(2) 0.002(3) C13 0.027(3) 0.025(3) 0.018(3) -0.007(3) -0.004(2) 0.002(2) C14 0.033(3) 0.016(2) 0.021(3) 0.003(2) -0.006(2) 0.002(2) C15 0.043(4) 0.016(3) 0.023(3) -0.003(2) -0.007(3) 0.004(2) C16 0.045(4) 0.016(3) 0.042(4) -0.001(3) -0.008(3) -0.001(3) C17 0.047(4) 0.029(4) 0.037(5) 0.008(4) -0.004(3) 0.011(3) C18 0.053(4) 0.028(4) 0.033(4) -0.008(3) -0.004(3) 0.011(3) C19 0.015(3) 0.030(4) 0.018(3) -0.002(3) 0.004(2) 0.003(2) C20 0.028(3) 0.029(4) 0.021(4) -0.004(3) 0.002(2) -0.003(2) C21 0.032(3) 0.027(3) 0.024(4) -0.005(3) 0.005(3) -0.001(3) C22 0.031(4) 0.030(4) 0.026(4) 0.012(3) 0.002(3) 0.007(3) C23 0.016(3) 0.035(4) 0.045(5) 0.001(4) -0.003(3) -0.003(3) C24 0.017(3) 0.028(3) 0.032(4) 0.004(3) -0.002(3) 0.000(2) Mo1B 0.0230(3) 0.0203(3) 0.0286(3) 0.0002(3) 0.00043(19) 0.00112(17) Mo2B 0.0177(2) 0.0265(3) 0.0301(3) 0.0017(3) 0.0051(2) 0.00251(17) P1B 0.0194(7) 0.0212(8) 0.0271(9) -0.0008(7) 0.0056(6) -0.0008(6) O1B 0.033(3) 0.037(3) 0.070(5) -0.007(3) -0.006(3) -0.009(2) O2B 0.096(5) 0.041(3) 0.044(4) -0.018(3) 0.002(3) 0.033(3) O3B 0.033(2) 0.026(2) 0.040(3) 0.006(3) 0.004(2) -0.0035(18) N2B 0.055(4) 0.026(3) 0.033(4) -0.002(3) 0.002(3) 0.007(3) N3B 0.022(3) 0.028(3) 0.029(3) 0.005(3) 0.004(2) -0.003(2) C1B 0.027(3) 0.030(3) 0.036(4) 0.001(3) -0.006(3) 0.000(3) C2B 0.032(4) 0.053(5) 0.034(4) 0.007(4) 0.005(3) 0.011(3) C31 0.026(3) 0.026(4) 0.042(4) 0.012(4) 0.001(3) 0.000(2) C32 0.031(4) 0.030(4) 0.061(6) 0.010(5) -0.003(4) 0.019(3) C33 0.036(4) 0.018(3) 0.047(5) 0.003(3) -0.014(3) 0.000(3) C34 0.025(3) 0.030(4) 0.041(5) 0.003(3) 0.001(3) 0.008(3) C35 0.033(3) 0.016(3) 0.035(4) 0.003(3) -0.002(3) 0.008(2) C36 0.030(4) 0.035(4) 0.042(5) -0.004(4) 0.019(3) 0.003(3) C37 0.027(3) 0.042(4) 0.046(5) 0.002(4) 0.015(3) -0.002(3) C38 0.020(4) 0.062(6) 0.056(6) -0.006(5) 0.013(3) 0.000(3) C39 0.028(4) 0.061(6) 0.063(7) 0.019(5) 0.015(4) 0.023(4) C40 0.034(4) 0.030(4) 0.061(6) 0.009(4) 0.025(4) 0.010(3) C41 0.016(3) 0.023(3) 0.040(4) -0.007(3) 0.003(3) -0.003(2) C42 0.020(3) 0.029(3) 0.037(4) -0.005(3) -0.003(3) 0.002(3) C43 0.021(3) 0.039(4) 0.033(4) -0.002(3) 0.004(3) 0.005(3) C44 0.029(4) 0.035(4) 0.038(5) -0.012(4) 0.007(3) 0.008(3) C45 0.031(3) 0.030(4) 0.048(5) -0.009(4) 0.008(3) -0.007(3) C46 0.033(4) 0.025(4) 0.063(7) -0.008(5) 0.019(3) -0.005(3) C47 0.028(3) 0.023(4) 0.039(4) 0.007(3) 0.000(3) -0.003(2) C48 0.067(6) 0.054(5) 0.049(5) 0.007(4) 0.012(4) 0.002(4) C49 0.067(6) 0.058(5) 0.059(6) 0.014(5) -0.005(5) 0.001(5) C50 0.037(4) 0.083(7) 0.095(8) 0.075(7) -0.037(5) -0.021(4) C51 0.184(13) 0.030(5) 0.034(5) 0.003(4) 0.025(7) 0.050(7) C52 0.136(10) 0.044(5) 0.041(5) 0.024(5) 0.040(6) 0.047(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 N2 1.794(6) . ? Mo1 C1 1.991(7) . ? Mo1 C7 2.336(7) . ? Mo1 C4 2.369(7) . ? Mo1 C3 2.371(7) . ? Mo1 C6 2.376(7) . ? Mo1 C5 2.393(7) . ? Mo1 P1 2.502(2) . ? Mo1 Mo2 3.0735(14) . ? Mo2 N3 1.760(6) . ? Mo2 C2 2.205(8) . ? Mo2 C12 2.327(7) . ? Mo2 C8 2.382(7) . ? Mo2 C9 2.394(8) . ? Mo2 C11 2.397(7) . ? Mo2 P1 2.4011(19) . ? Mo2 C10 2.434(7) . ? P1 C13 1.866(7) . ? P1 C19 1.870(7) . ? O1 C1 1.159(9) . ? O2 N2 1.191(9) . ? O3 N3 1.231(8) . ? C2 H2A 0.96 . ? C2 H2B 0.96 . ? C2 H2C 0.96 . ? C3 C7 1.416(10) . ? C3 C4 1.430(10) . ? C3 H3 0.93 . ? C4 C5 1.417(10) . ? C4 H4 0.93 . ? C5 C6 1.422(10) . ? C5 H5 0.93 . ? C6 C7 1.418(12) . ? C6 H6 0.93 . ? C7 H7 0.93 . ? C8 C9 1.414(11) . ? C8 C12 1.439(12) . ? C8 H8 0.93 . ? C9 C10 1.431(11) . ? C9 H9 0.93 . ? C10 C11 1.406(12) . ? C10 H10 0.93 . ? C11 C12 1.405(14) . ? C11 H11 0.93 . ? C12 H12 0.93 . ? C13 C18 1.541(10) . ? C13 C14 1.552(8) . ? C13 H13 0.98 . ? C14 C15 1.524(8) . ? C14 H14A 0.97 . ? C14 H14B 0.97 . ? C15 C16 1.520(9) . ? C15 H15A 0.97 . ? C15 H15B 0.97 . ? C16 C17 1.472(11) . ? C16 H16A 0.97 . ? C16 H16B 0.97 . ? C17 C18 1.544(11) . ? C17 H17A 0.97 . ? C17 H17B 0.97 . ? C18 H18A 0.97 . ? C18 H18B 0.97 . ? C19 C20 1.535(10) . ? C19 C24 1.549(8) . ? C19 H19 0.98 . ? C20 C21 1.520(10) . ? C20 H20A 0.97 . ? C20 H20B 0.97 . ? C21 C22 1.521(10) . ? C21 H21A 0.97 . ? C21 H21B 0.97 . ? C22 C23 1.520(11) . ? C22 H22A 0.97 . ? C22 H22B 0.97 . ? C23 C24 1.502(11) . ? C23 H23A 0.97 . ? C23 H23B 0.97 . ? C24 H24A 0.97 . ? C24 H24B 0.97 . ? Mo1B N2B 1.781(6) . ? Mo1B C1B 2.000(7) . ? Mo1B C32 2.300(10) . ? Mo1B C33 2.319(8) . ? Mo1B C34 2.358(7) . ? Mo1B C35 2.384(6) . ? Mo1B C31 2.393(7) . ? Mo1B P1B 2.494(2) . ? Mo1B Mo2B 3.0600(14) . ? Mo2B N3B 1.772(6) . ? Mo2B C2B 2.244(9) . ? Mo2B C37 2.368(8) . ? Mo2B C38 2.371(7) . ? Mo2B P1B 2.4003(18) . ? Mo2B C36 2.401(8) . ? Mo2B C39 2.409(7) . ? Mo2B C40 2.419(8) . ? P1B C41 1.861(7) . ? P1B C47 1.876(7) . ? O1B C1B 1.131(9) . ? O2B N2B 1.206(9) . ? O3B N3B 1.211(8) . ? C2B H2B1 0.96 . ? C2B H2B2 0.96 . ? C2B H2B3 0.96 . ? C31 C32 1.361(13) . ? C31 C35 1.438(11) . ? C31 H31 0.93 . ? C32 C33 1.418(11) . ? C32 H32 0.93 . ? C33 C34 1.427(12) . ? C33 H33 0.93 . ? C34 C35 1.390(10) . ? C34 H34 0.93 . ? C35 H35 0.93 . ? C36 C37 1.408(11) . ? C36 C40 1.422(12) . ? C36 H36 0.93 . ? C37 C38 1.368(15) . ? C37 H37 0.93 . ? C38 C39 1.436(15) . ? C38 H38 0.93 . ? C39 C40 1.388(15) . ? C39 H39 0.93 . ? C40 H40 0.93 . ? C41 C46 1.516(10) . ? C41 C42 1.528(8) . ? C41 H41 0.98 . ? C42 C43 1.554(10) . ? C42 H42A 0.97 . ? C42 H42B 0.97 . ? C43 C44 1.506(12) . ? C43 H43A 0.97 . ? C43 H43B 0.97 . ? C44 C45 1.513(9) . ? C44 H44A 0.97 . ? C44 H44B 0.97 . ? C45 C46 1.543(12) . ? C45 H45A 0.97 . ? C45 H45B 0.97 . ? C46 H46A 0.97 . ? C46 H46B 0.97 . ? C47 C52 1.416(12) . ? C47 C48 1.528(12) . ? C47 H47 0.98 . ? C48 C49 1.541(12) . ? C48 H48A 0.97 . ? C48 H48B 0.97 . ? C49 C50 1.574(15) . ? C49 H49A 0.97 . ? C49 H49B 0.97 . ? C50 C51 1.578(15) . ? C50 H50A 0.97 . ? C50 H50B 0.97 . ? C51 C52 1.530(12) . ? C51 H51A 0.97 . ? C51 H51B 0.97 . ? C52 H52A 0.97 . ? C52 H52B 0.97 . ? 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 N2 Mo1 C1 88.2(3) . . ? N2 Mo1 C7 104.8(3) . . ? C1 Mo1 C7 95.7(3) . . ? N2 Mo1 C4 118.0(3) . . ? C1 Mo1 C4 146.1(2) . . ? C7 Mo1 C4 58.7(3) . . ? N2 Mo1 C3 95.0(3) . . ? C1 Mo1 C3 129.6(3) . . ? C7 Mo1 C3 35.0(2) . . ? C4 Mo1 C3 35.1(3) . . ? N2 Mo1 C6 139.0(3) . . ? C1 Mo1 C6 88.8(3) . . ? C7 Mo1 C6 35.0(3) . . ? C4 Mo1 C6 57.4(2) . . ? C3 Mo1 C6 57.3(3) . . ? N2 Mo1 C5 151.7(3) . . ? C1 Mo1 C5 114.7(3) . . ? C7 Mo1 C5 58.7(3) . . ? C4 Mo1 C5 34.6(2) . . ? C3 Mo1 C5 57.9(3) . . ? C6 Mo1 C5 34.7(3) . . ? N2 Mo1 P1 97.9(2) . . ? C1 Mo1 P1 78.0(2) . . ? C7 Mo1 P1 156.2(2) . . ? C4 Mo1 P1 115.75(19) . . ? C3 Mo1 P1 149.91(18) . . ? C6 Mo1 P1 121.3(2) . . ? C5 Mo1 P1 102.7(2) . . ? N2 Mo1 Mo2 87.4(2) . . ? C1 Mo1 Mo2 126.2(2) . . ? C7 Mo1 Mo2 137.0(2) . . ? C4 Mo1 Mo2 78.99(16) . . ? C3 Mo1 Mo2 104.20(17) . . ? C6 Mo1 Mo2 126.0(2) . . ? C5 Mo1 Mo2 91.35(17) . . ? P1 Mo1 Mo2 49.73(4) . . ? N3 Mo2 C2 89.1(3) . . ? N3 Mo2 C12 103.9(3) . . ? C2 Mo2 C12 81.8(3) . . ? N3 Mo2 C8 95.4(3) . . ? C2 Mo2 C8 116.4(3) . . ? C12 Mo2 C8 35.6(3) . . ? N3 Mo2 C9 119.2(3) . . ? C2 Mo2 C9 134.6(3) . . ? C12 Mo2 C9 58.5(3) . . ? C8 Mo2 C9 34.4(3) . . ? N3 Mo2 C11 137.4(3) . . ? C2 Mo2 C11 78.0(3) . . ? C12 Mo2 C11 34.6(3) . . ? C8 Mo2 C11 57.1(3) . . ? C9 Mo2 C11 56.9(3) . . ? N3 Mo2 P1 96.12(18) . . ? C2 Mo2 P1 84.5(2) . . ? C12 Mo2 P1 155.5(2) . . ? C8 Mo2 P1 156.3(2) . . ? C9 Mo2 P1 122.63(18) . . ? C11 Mo2 P1 122.3(2) . . ? N3 Mo2 C10 151.9(3) . . ? C2 Mo2 C10 107.0(3) . . ? C12 Mo2 C10 57.7(3) . . ? C8 Mo2 C10 57.1(3) . . ? C9 Mo2 C10 34.5(3) . . ? C11 Mo2 C10 33.8(3) . . ? P1 Mo2 C10 107.90(17) . . ? N3 Mo2 Mo1 89.79(18) . . ? C2 Mo2 Mo1 136.7(2) . . ? C12 Mo2 Mo1 139.9(2) . . ? C8 Mo2 Mo1 106.80(19) . . ? C9 Mo2 Mo1 81.86(18) . . ? C11 Mo2 Mo1 126.9(2) . . ? P1 Mo2 Mo1 52.65(5) . . ? C10 Mo2 Mo1 93.36(19) . . ? C13 P1 C19 99.9(3) . . ? C13 P1 Mo2 121.3(2) . . ? C19 P1 Mo2 122.7(2) . . ? C13 P1 Mo1 118.2(2) . . ? C19 P1 Mo1 117.9(2) . . ? Mo2 P1 Mo1 77.61(6) . . ? O2 N2 Mo1 172.7(6) . . ? O3 N3 Mo2 171.3(5) . . ? O1 C1 Mo1 176.6(7) . . ? Mo2 C2 H2A 109.5 . . ? Mo2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Mo2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C7 C3 C4 108.3(6) . . ? C7 C3 Mo1 71.1(4) . . ? C4 C3 Mo1 72.4(4) . . ? C7 C3 H3 125.8 . . ? C4 C3 H3 125.8 . . ? Mo1 C3 H3 122.3 . . ? C5 C4 C3 108.2(6) . . ? C5 C4 Mo1 73.6(4) . . ? C3 C4 Mo1 72.5(4) . . ? C5 C4 H4 125.9 . . ? C3 C4 H4 125.9 . . ? Mo1 C4 H4 119.8 . . ? C4 C5 C6 106.8(7) . . ? C4 C5 Mo1 71.8(4) . . ? C6 C5 Mo1 72.0(4) . . ? C4 C5 H5 126.6 . . ? C6 C5 H5 126.6 . . ? Mo1 C5 H5 121.5 . . ? C7 C6 C5 109.6(6) . . ? C7 C6 Mo1 70.9(4) . . ? C5 C6 Mo1 73.3(4) . . ? C7 C6 H6 125.2 . . ? C5 C6 H6 125.2 . . ? Mo1 C6 H6 122.1 . . ? C3 C7 C6 106.9(7) . . ? C3 C7 Mo1 73.9(4) . . ? C6 C7 Mo1 74.1(4) . . ? C3 C7 H7 126.5 . . ? C6 C7 H7 126.5 . . ? Mo1 C7 H7 117.7 . . ? C9 C8 C12 107.9(7) . . ? C9 C8 Mo2 73.2(4) . . ? C12 C8 Mo2 70.1(4) . . ? C9 C8 H8 126.1 . . ? C12 C8 H8 126.1 . . ? Mo2 C8 H8 122.2 . . ? C8 C9 C10 108.0(7) . . ? C8 C9 Mo2 72.3(4) . . ? C10 C9 Mo2 74.3(4) . . ? C8 C9 H9 126 . . ? C10 C9 H9 126 . . ? Mo2 C9 H9 119.2 . . ? C11 C10 C9 107.2(7) . . ? C11 C10 Mo2 71.6(4) . . ? C9 C10 Mo2 71.2(4) . . ? C11 C10 H10 126.4 . . ? C9 C10 H10 126.4 . . ? Mo2 C10 H10 122.4 . . ? C12 C11 C10 109.8(8) . . ? C12 C11 Mo2 70.0(4) . . ? C10 C11 Mo2 74.5(4) . . ? C12 C11 H11 125.1 . . ? C10 C11 H11 125.1 . . ? Mo2 C11 H11 122 . . ? C11 C12 C8 106.9(8) . . ? C11 C12 Mo2 75.4(4) . . ? C8 C12 Mo2 74.3(4) . . ? C11 C12 H12 126.6 . . ? C8 C12 H12 126.6 . . ? Mo2 C12 H12 116 . . ? C18 C13 C14 107.8(5) . . ? C18 C13 P1 114.1(5) . . ? C14 C13 P1 110.4(4) . . ? C18 C13 H13 108.1 . . ? C14 C13 H13 108.1 . . ? P1 C13 H13 108.1 . . ? C15 C14 C13 112.0(5) . . ? C15 C14 H14A 109.2 . . ? C13 C14 H14A 109.2 . . ? C15 C14 H14B 109.2 . . ? C13 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? C16 C15 C14 109.4(5) . . ? C16 C15 H15A 109.8 . . ? C14 C15 H15A 109.8 . . ? C16 C15 H15B 109.8 . . ? C14 C15 H15B 109.8 . . ? H15A C15 H15B 108.2 . . ? C17 C16 C15 112.8(6) . . ? C17 C16 H16A 109 . . ? C15 C16 H16A 109 . . ? C17 C16 H16B 109 . . ? C15 C16 H16B 109 . . ? H16A C16 H16B 107.8 . . ? C16 C17 C18 109.8(7) . . ? C16 C17 H17A 109.7 . . ? C18 C17 H17A 109.7 . . ? C16 C17 H17B 109.7 . . ? C18 C17 H17B 109.7 . . ? H17A C17 H17B 108.2 . . ? C13 C18 C17 110.8(7) . . ? C13 C18 H18A 109.5 . . ? C17 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 108.1 . . ? C20 C19 C24 108.0(5) . . ? C20 C19 P1 114.9(5) . . ? C24 C19 P1 114.1(5) . . ? C20 C19 H19 106.4 . . ? C24 C19 H19 106.4 . . ? P1 C19 H19 106.4 . . ? C21 C20 C19 111.0(6) . . ? C21 C20 H20A 109.4 . . ? C19 C20 H20A 109.4 . . ? C21 C20 H20B 109.4 . . ? C19 C20 H20B 109.4 . . ? H20A C20 H20B 108 . . ? C20 C21 C22 111.1(6) . . ? C20 C21 H21A 109.4 . . ? C22 C21 H21A 109.4 . . ? C20 C21 H21B 109.4 . . ? C22 C21 H21B 109.4 . . ? H21A C21 H21B 108 . . ? C23 C22 C21 111.2(6) . . ? C23 C22 H22A 109.4 . . ? C21 C22 H22A 109.4 . . ? C23 C22 H22B 109.4 . . ? C21 C22 H22B 109.4 . . ? H22A C22 H22B 108 . . ? C24 C23 C22 112.2(7) . . ? C24 C23 H23A 109.2 . . ? C22 C23 H23A 109.2 . . ? C24 C23 H23B 109.2 . . ? C22 C23 H23B 109.2 . . ? H23A C23 H23B 107.9 . . ? C23 C24 C19 112.1(6) . . ? C23 C24 H24A 109.2 . . ? C19 C24 H24A 109.2 . . ? C23 C24 H24B 109.2 . . ? C19 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? N2B Mo1B C1B 88.0(3) . . ? N2B Mo1B C32 94.9(3) . . ? C1B Mo1B C32 132.0(3) . . ? N2B Mo1B C33 104.3(3) . . ? C1B Mo1B C33 97.3(3) . . ? C32 Mo1B C33 35.8(3) . . ? N2B Mo1B C34 138.7(3) . . ? C1B Mo1B C34 89.0(3) . . ? C32 Mo1B C34 58.5(3) . . ? C33 Mo1B C34 35.5(3) . . ? N2B Mo1B C35 151.9(3) . . ? C1B Mo1B C35 114.3(3) . . ? C32 Mo1B C35 57.7(3) . . ? C33 Mo1B C35 58.0(3) . . ? C34 Mo1B C35 34.1(3) . . ? N2B Mo1B C31 118.1(3) . . ? C1B Mo1B C31 146.3(3) . . ? C32 Mo1B C31 33.6(3) . . ? C33 Mo1B C31 57.7(3) . . ? C34 Mo1B C31 57.4(2) . . ? C35 Mo1B C31 35.0(3) . . ? N2B Mo1B P1B 98.1(2) . . ? C1B Mo1B P1B 77.2(2) . . ? C32 Mo1B P1B 148.5(2) . . ? C33 Mo1B P1B 156.7(2) . . ? C34 Mo1B P1B 121.3(2) . . ? C35 Mo1B P1B 103.3(2) . . ? C31 Mo1B P1B 116.2(2) . . ? N2B Mo1B Mo2B 88.7(2) . . ? C1B Mo1B Mo2B 125.9(2) . . ? C32 Mo1B Mo2B 102.1(2) . . ? C33 Mo1B Mo2B 135.63(19) . . ? C34 Mo1B Mo2B 125.2(2) . . ? C35 Mo1B Mo2B 91.23(17) . . ? C31 Mo1B Mo2B 78.64(18) . . ? P1B Mo1B Mo2B 49.94(4) . . ? N3B Mo2B C2B 90.9(3) . . ? N3B Mo2B C37 93.9(3) . . ? C2B Mo2B C37 118.3(3) . . ? N3B Mo2B C38 103.0(3) . . ? C2B Mo2B C38 85.7(4) . . ? C37 Mo2B C38 33.6(4) . . ? N3B Mo2B P1B 96.34(18) . . ? C2B Mo2B P1B 82.6(2) . . ? C37 Mo2B P1B 156.6(2) . . ? C38 Mo2B P1B 157.5(3) . . ? N3B Mo2B C36 118.4(3) . . ? C2B Mo2B C36 134.6(3) . . ? C37 Mo2B C36 34.3(3) . . ? C38 Mo2B C36 55.8(3) . . ? P1B Mo2B C36 123.43(19) . . ? N3B Mo2B C39 136.5(3) . . ? C2B Mo2B C39 78.4(3) . . ? C37 Mo2B C39 57.4(3) . . ? C38 Mo2B C39 35.0(4) . . ? P1B Mo2B C39 123.2(2) . . ? C36 Mo2B C39 56.4(3) . . ? N3B Mo2B C40 150.8(3) . . ? C2B Mo2B C40 106.3(3) . . ? C37 Mo2B C40 57.3(3) . . ? C38 Mo2B C40 56.4(3) . . ? P1B Mo2B C40 108.96(19) . . ? C36 Mo2B C40 34.3(3) . . ? C39 Mo2B C40 33.4(4) . . ? N3B Mo2B Mo1B 90.66(18) . . ? C2B Mo2B Mo1B 135.1(2) . . ? C37 Mo2B Mo1B 106.3(2) . . ? C38 Mo2B Mo1B 137.2(3) . . ? P1B Mo2B Mo1B 52.69(5) . . ? C36 Mo2B Mo1B 81.9(2) . . ? C39 Mo2B Mo1B 126.4(3) . . ? C40 Mo2B Mo1B 93.2(2) . . ? C41 P1B C47 103.2(3) . . ? C41 P1B Mo2B 122.1(2) . . ? C47 P1B Mo2B 120.2(2) . . ? C41 P1B Mo1B 118.2(3) . . ? C47 P1B Mo1B 115.0(3) . . ? Mo2B P1B Mo1B 77.36(6) . . ? O2B N2B Mo1B 172.4(7) . . ? O3B N3B Mo2B 172.6(5) . . ? O1B C1B Mo1B 174.4(8) . . ? Mo2B C2B H2B1 109.5 . . ? Mo2B C2B H2B2 109.5 . . ? H2B1 C2B H2B2 109.5 . . ? Mo2B C2B H2B3 109.5 . . ? H2B1 C2B H2B3 109.5 . . ? H2B2 C2B H2B3 109.5 . . ? C32 C31 C35 107.8(6) . . ? C32 C31 Mo1B 69.4(5) . . ? C35 C31 Mo1B 72.2(4) . . ? C32 C31 H31 126.1 . . ? C35 C31 H31 126.1 . . ? Mo1B C31 H31 123.9 . . ? C31 C32 C33 109.8(8) . . ? C31 C32 Mo1B 76.9(6) . . ? C33 C32 Mo1B 72.8(5) . . ? C31 C32 H32 125.1 . . ? C33 C32 H32 125.1 . . ? Mo1B C32 H32 116.9 . . ? C32 C33 C34 106.4(8) . . ? C32 C33 Mo1B 71.4(5) . . ? C34 C33 Mo1B 73.7(5) . . ? C32 C33 H33 126.8 . . ? C34 C33 H33 126.8 . . ? Mo1B C33 H33 120 . . ? C35 C34 C33 108.2(6) . . ? C35 C34 Mo1B 74.0(4) . . ? C33 C34 Mo1B 70.8(4) . . ? C35 C34 H34 125.9 . . ? C33 C34 H34 125.9 . . ? Mo1B C34 H34 121 . . ? C34 C35 C31 107.7(7) . . ? C34 C35 Mo1B 71.9(4) . . ? C31 C35 Mo1B 72.8(4) . . ? C34 C35 H35 126.1 . . ? C31 C35 H35 126.1 . . ? Mo1B C35 H35 120.9 . . ? C37 C36 C40 108.5(8) . . ? C37 C36 Mo2B 71.6(5) . . ? C40 C36 Mo2B 73.6(5) . . ? C37 C36 H36 125.8 . . ? C40 C36 H36 125.8 . . ? Mo2B C36 H36 120.8 . . ? C38 C37 C36 107.2(8) . . ? C38 C37 Mo2B 73.3(5) . . ? C36 C37 Mo2B 74.1(4) . . ? C38 C37 H37 126.4 . . ? C36 C37 H37 126.4 . . ? Mo2B C37 H37 118.2 . . ? C37 C38 C39 109.9(9) . . ? C37 C38 Mo2B 73.1(4) . . ? C39 C38 Mo2B 74.0(4) . . ? C37 C38 H38 125.1 . . ? C39 C38 H38 125.1 . . ? Mo2B C38 H38 119.5 . . ? C40 C39 C38 106.5(8) . . ? C40 C39 Mo2B 73.7(4) . . ? C38 C39 Mo2B 71.1(4) . . ? C40 C39 H39 126.7 . . ? C38 C39 H39 126.7 . . ? Mo2B C39 H39 120.4 . . ? C39 C40 C36 107.9(8) . . ? C39 C40 Mo2B 72.9(5) . . ? C36 C40 Mo2B 72.1(4) . . ? C39 C40 H40 126 . . ? C36 C40 H40 126 . . ? Mo2B C40 H40 120.7 . . ? C46 C41 C42 110.1(6) . . ? C46 C41 P1B 115.1(6) . . ? C42 C41 P1B 113.3(5) . . ? C46 C41 H41 105.8 . . ? C42 C41 H41 105.8 . . ? P1B C41 H41 105.8 . . ? C41 C42 C43 109.8(6) . . ? C41 C42 H42A 109.7 . . ? C43 C42 H42A 109.7 . . ? C41 C42 H42B 109.7 . . ? C43 C42 H42B 109.7 . . ? H42A C42 H42B 108.2 . . ? C44 C43 C42 112.3(7) . . ? C44 C43 H43A 109.1 . . ? C42 C43 H43A 109.1 . . ? C44 C43 H43B 109.1 . . ? C42 C43 H43B 109.1 . . ? H43A C43 H43B 107.9 . . ? C43 C44 C45 112.3(6) . . ? C43 C44 H44A 109.1 . . ? C45 C44 H44A 109.1 . . ? C43 C44 H44B 109.1 . . ? C45 C44 H44B 109.1 . . ? H44A C44 H44B 107.9 . . ? C44 C45 C46 110.3(7) . . ? C44 C45 H45A 109.6 . . ? C46 C45 H45A 109.6 . . ? C44 C45 H45B 109.6 . . ? C46 C45 H45B 109.6 . . ? H45A C45 H45B 108.1 . . ? C41 C46 C45 111.2(7) . . ? C41 C46 H46A 109.4 . . ? C45 C46 H46A 109.4 . . ? C41 C46 H46B 109.4 . . ? C45 C46 H46B 109.4 . . ? H46A C46 H46B 108 . . ? C52 C47 C48 116.7(8) . . ? C52 C47 P1B 114.8(6) . . ? C48 C47 P1B 113.5(6) . . ? C52 C47 H47 103.1 . . ? C48 C47 H47 103.1 . . ? P1B C47 H47 103.1 . . ? C47 C48 C49 110.1(8) . . ? C47 C48 H48A 109.6 . . ? C49 C48 H48A 109.6 . . ? C47 C48 H48B 109.6 . . ? C49 C48 H48B 109.6 . . ? H48A C48 H48B 108.2 . . ? C48 C49 C50 109.9(8) . . ? C48 C49 H49A 109.7 . . ? C50 C49 H49A 109.7 . . ? C48 C49 H49B 109.7 . . ? C50 C49 H49B 109.7 . . ? H49A C49 H49B 108.2 . . ? C49 C50 C51 102.3(7) . . ? C49 C50 H50A 111.3 . . ? C51 C50 H50A 111.3 . . ? C49 C50 H50B 111.3 . . ? C51 C50 H50B 111.3 . . ? H50A C50 H50B 109.2 . . ? C52 C51 C50 107.8(10) . . ? C52 C51 H51A 110.2 . . ? C50 C51 H51A 110.2 . . ? C52 C51 H51B 110.2 . . ? C50 C51 H51B 110.2 . . ? H51A C51 H51B 108.5 . . ? C47 C52 C51 116.6(8) . . ? C47 C52 H52A 108.1 . . ? C51 C52 H52A 108.1 . . ? C47 C52 H52B 108.1 . . ? C51 C52 H52B 108.1 . . ? H52A C52 H52B 107.3 . . ? #===END data_compound6b _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C30 H39 Mo2 N2 O3 P1' _chemical_formula_sum 'C30 H39 Mo2 N2 O3 P' _chemical_formula_weight 698.48 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 9.10550(10) _cell_length_b 33.0473(3) _cell_length_c 9.75290(10) _cell_angle_alpha 90 _cell_angle_beta 105.342(2) _cell_angle_gamma 90 _cell_volume 2830.18(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9122 _cell_measurement_theta_min 4.0112 _cell_measurement_theta_max 73.6267 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.639 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 8.065 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.34935 _exptl_absorpt_correction_T_max 0.85 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_type CuK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'ONYX CCD' _diffrn_measurement_method 'CCD' _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 8.2640 _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_av_unetI/netI 0.0314 _diffrn_reflns_number 15257 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 4.89 _diffrn_reflns_theta_max 73.91 _diffrn_reflns_theta_full 70 _diffrn_measured_fraction_theta_full 0.975 _diffrn_measured_fraction_theta_max 0.935 _reflns_number_total 5368 _reflns_number_gt 4464 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0628P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 5368 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0422 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0882 _refine_ls_wR_factor_gt 0.084 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.732 _refine_diff_density_min -1.185 _refine_diff_density_rms 0.106 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.36492(3) 0.114729(7) 0.38662(3) 0.02236(9) Uani 1 1 d . . . Mo2 Mo 0.54989(3) 0.061086(7) 0.23178(3) 0.02336(9) Uani 1 1 d . . . P1 P 0.36909(9) 0.11847(2) 0.14170(9) 0.02263(18) Uani 1 1 d . . . N1 N 0.4159(3) 0.02206(8) 0.2425(3) 0.0260(6) Uani 1 1 d . . . N2 N 0.5178(3) 0.14859(8) 0.4563(3) 0.0275(6) Uani 1 1 d . . . O1 O 0.3391(3) -0.00653(7) 0.2535(3) 0.0325(6) Uani 1 1 d . . . O2 O 0.6214(3) 0.16813(7) 0.5277(3) 0.0332(6) Uani 1 1 d . . . O3 O 0.4544(4) 0.04489(8) -0.0948(3) 0.0400(7) Uani 1 1 d . . . C1 C 0.4897(4) 0.05245(10) 0.0238(4) 0.0312(8) Uani 1 1 d . . . C2 C 0.1608(4) 0.09354(10) 0.4814(4) 0.0284(7) Uani 1 1 d . . . H2 H 0.0632 0.104 0.4466 0.034 Uiso 1 1 calc R . . C3 C 0.2166(4) 0.05856(10) 0.4330(4) 0.0287(7) Uani 1 1 d . . . H3 H 0.1632 0.0418 0.3602 0.034 Uiso 1 1 calc R . . C4 C 0.3685(4) 0.05318(10) 0.5139(4) 0.0284(7) Uani 1 1 d . . . H4 H 0.4332 0.0323 0.5035 0.034 Uiso 1 1 calc R . . C5 C 0.4051(4) 0.08485(10) 0.6131(4) 0.0307(8) Uani 1 1 d . . . H5 H 0.4976 0.0884 0.6809 0.037 Uiso 1 1 calc R . . C6 C 0.2764(4) 0.11031(10) 0.5914(4) 0.0291(7) Uani 1 1 d . . . H6 H 0.2695 0.1339 0.6412 0.035 Uiso 1 1 calc R . . C7 C 0.7752(4) 0.02432(10) 0.3310(4) 0.0319(8) Uani 1 1 d . . . H7 H 0.7734 -0.0038 0.3335 0.038 Uiso 1 1 calc R . . C8 C 0.7535(4) 0.05058(10) 0.4388(4) 0.0277(7) Uani 1 1 d . . . H8 H 0.7347 0.0426 0.5241 0.033 Uiso 1 1 calc R . . C9 C 0.7651(4) 0.09079(11) 0.3948(4) 0.0321(8) Uani 1 1 d . . . H9 H 0.7555 0.114 0.4457 0.039 Uiso 1 1 calc R . . C10 C 0.7941(4) 0.08953(10) 0.2594(4) 0.0298(7) Uani 1 1 d . . . H10 H 0.807 0.1119 0.2059 0.036 Uiso 1 1 calc R . . C11 C 0.8003(4) 0.04822(11) 0.2187(4) 0.0311(8) Uani 1 1 d . . . H11 H 0.8175 0.0388 0.1344 0.037 Uiso 1 1 calc R . . C12 C 0.1944(4) 0.16575(10) 0.3158(4) 0.0278(7) Uani 1 1 d . . . H12A H 0.2346 0.1843 0.2577 0.033 Uiso 1 1 calc R . . H12B H 0.1011 0.1544 0.256 0.033 Uiso 1 1 calc R . . C13 C 0.1564(4) 0.18910(9) 0.4317(4) 0.0290(7) Uani 1 1 d . . . C14 C 0.0109(4) 0.18771(9) 0.4552(4) 0.0292(7) Uani 1 1 d . . . H14 H -0.0644 0.1722 0.3951 0.035 Uiso 1 1 calc R . . C15 C -0.0234(4) 0.20866(10) 0.5643(5) 0.0345(8) Uani 1 1 d . . . H15 H -0.1204 0.2067 0.578 0.041 Uiso 1 1 calc R . . C16 C 0.0852(5) 0.23266(11) 0.6542(5) 0.0390(9) Uani 1 1 d . . . H16 H 0.0626 0.2467 0.7287 0.047 Uiso 1 1 calc R . . C17 C 0.2296(5) 0.23528(11) 0.6301(5) 0.0405(10) Uani 1 1 d . . . H17 H 0.3029 0.2519 0.6879 0.049 Uiso 1 1 calc R . . C18 C 0.2649(4) 0.21373(10) 0.5225(5) 0.0356(9) Uani 1 1 d . . . H18 H 0.3623 0.2156 0.5099 0.043 Uiso 1 1 calc R . . C19 C 0.2022(4) 0.10559(10) -0.0110(4) 0.0267(7) Uani 1 1 d . . . H19 H 0.2426 0.0974 -0.0905 0.032 Uiso 1 1 calc R . . C20 C 0.1135(4) 0.06949(10) 0.0245(4) 0.0308(8) Uani 1 1 d . . . H20A H 0.1821 0.0467 0.0529 0.037 Uiso 1 1 calc R . . H20B H 0.073 0.0765 0.104 0.037 Uiso 1 1 calc R . . C21 C -0.0169(4) 0.05723(11) -0.1018(4) 0.0353(8) Uani 1 1 d . . . H21A H 0.0241 0.048 -0.1785 0.042 Uiso 1 1 calc R . . H21B H -0.0725 0.035 -0.0744 0.042 Uiso 1 1 calc R . . C22 C -0.1250(4) 0.09217(11) -0.1538(4) 0.0332(8) Uani 1 1 d . . . H22A H -0.1754 0.0994 -0.0812 0.04 Uiso 1 1 calc R . . H22B H -0.2025 0.084 -0.2383 0.04 Uiso 1 1 calc R . . C23 C -0.0384(4) 0.12903(11) -0.1884(4) 0.0331(8) Uani 1 1 d . . . H23A H 0.001 0.1227 -0.2692 0.04 Uiso 1 1 calc R . . H23B H -0.1083 0.1516 -0.2149 0.04 Uiso 1 1 calc R . . C24 C 0.0937(4) 0.14149(10) -0.0626(4) 0.0320(8) Uani 1 1 d . . . H24A H 0.0539 0.151 0.0146 0.038 Uiso 1 1 calc R . . H24B H 0.1495 0.1636 -0.091 0.038 Uiso 1 1 calc R . . C25 C 0.4558(4) 0.16259(9) 0.0716(4) 0.0259(7) Uani 1 1 d . . . H25 H 0.3734 0.182 0.0352 0.031 Uiso 1 1 calc R . . C26 C 0.5766(4) 0.18472(10) 0.1852(4) 0.0291(7) Uani 1 1 d . . . H26A H 0.655 0.1657 0.2317 0.035 Uiso 1 1 calc R . . H26B H 0.5303 0.1954 0.2564 0.035 Uiso 1 1 calc R . . C27 C 0.6504(4) 0.21975(10) 0.1222(4) 0.0318(8) Uani 1 1 d . . . H27A H 0.5757 0.241 0.09 0.038 Uiso 1 1 calc R . . H27B H 0.7338 0.231 0.1959 0.038 Uiso 1 1 calc R . . C28 C 0.7099(5) 0.20592(11) -0.0011(5) 0.0365(8) Uani 1 1 d . . . H28A H 0.7926 0.1869 0.0329 0.044 Uiso 1 1 calc R . . H28B H 0.7496 0.229 -0.0413 0.044 Uiso 1 1 calc R . . C29 C 0.5844(5) 0.18588(12) -0.1159(4) 0.0368(9) Uani 1 1 d . . . H29A H 0.626 0.1765 -0.192 0.044 Uiso 1 1 calc R . . H29B H 0.5055 0.2056 -0.1553 0.044 Uiso 1 1 calc R . . C30 C 0.5151(4) 0.15011(11) -0.0550(4) 0.0315(8) Uani 1 1 d . . . H30A H 0.432 0.1389 -0.1288 0.038 Uiso 1 1 calc R . . H30B H 0.5917 0.1292 -0.0252 0.038 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 0.01892(14) 0.02194(13) 0.02518(16) -0.00066(9) 0.00402(11) -0.00072(9) Mo2 0.01948(15) 0.02164(13) 0.02762(16) -0.00104(9) 0.00385(11) 0.00025(9) P1 0.0194(4) 0.0214(3) 0.0255(4) -0.0014(3) 0.0032(3) -0.0012(3) N1 0.0235(15) 0.0243(13) 0.0278(16) -0.0020(10) 0.0028(12) 0.0039(11) N2 0.0237(15) 0.0274(13) 0.0324(17) -0.0040(11) 0.0089(13) -0.0038(11) O1 0.0280(13) 0.0257(11) 0.0417(16) 0.0010(10) 0.0052(12) -0.0051(10) O2 0.0276(13) 0.0373(12) 0.0325(14) -0.0100(10) 0.0041(11) -0.0102(11) O3 0.0546(18) 0.0325(12) 0.0316(16) -0.0062(11) 0.0087(13) 0.0072(12) C1 0.034(2) 0.0211(14) 0.040(2) -0.0017(14) 0.0124(17) 0.0076(14) C2 0.0205(16) 0.0326(16) 0.0325(19) 0.0056(14) 0.0079(15) -0.0016(13) C3 0.0273(18) 0.0283(15) 0.0290(19) 0.0020(13) 0.0048(15) -0.0030(13) C4 0.0292(18) 0.0284(15) 0.0282(19) 0.0068(13) 0.0087(15) 0.0033(14) C5 0.0241(18) 0.0350(17) 0.030(2) 0.0039(14) 0.0022(15) -0.0001(14) C6 0.0300(19) 0.0319(16) 0.0283(19) 0.0041(13) 0.0125(15) 0.0010(14) C7 0.0263(18) 0.0293(16) 0.041(2) 0.0068(14) 0.0094(16) 0.0052(14) C8 0.0160(16) 0.0372(17) 0.0270(18) 0.0014(14) 0.0003(14) -0.0022(13) C9 0.0192(17) 0.0368(17) 0.035(2) -0.0054(15) -0.0020(15) 0.0014(14) C10 0.0183(16) 0.0322(16) 0.037(2) 0.0033(14) 0.0033(15) -0.0018(13) C11 0.0175(17) 0.0354(17) 0.039(2) -0.0003(15) 0.0053(15) 0.0015(13) C12 0.0242(17) 0.0275(15) 0.0309(19) 0.0008(13) 0.0057(15) -0.0003(13) C13 0.0276(18) 0.0220(14) 0.036(2) 0.0037(13) 0.0052(16) 0.0041(13) C14 0.0250(18) 0.0238(14) 0.036(2) 0.0032(13) 0.0040(16) -0.0016(13) C15 0.0267(19) 0.0273(15) 0.052(2) 0.0032(15) 0.0141(17) 0.0053(14) C16 0.040(2) 0.0308(17) 0.045(2) -0.0059(16) 0.0096(19) 0.0104(16) C17 0.030(2) 0.0319(17) 0.052(3) -0.0168(17) -0.0019(18) 0.0019(15) C18 0.0254(18) 0.0281(16) 0.051(3) -0.0045(15) 0.0070(17) -0.0011(14) C19 0.0218(17) 0.0281(14) 0.0281(18) -0.0031(13) 0.0029(14) -0.0013(13) C20 0.0247(18) 0.0274(15) 0.038(2) 0.0018(14) 0.0049(16) -0.0027(14) C21 0.0248(19) 0.0388(18) 0.040(2) -0.0046(16) 0.0055(17) -0.0079(15) C22 0.0212(18) 0.0429(19) 0.034(2) -0.0040(15) 0.0047(15) -0.0059(15) C23 0.0213(18) 0.0400(18) 0.033(2) 0.0017(15) -0.0025(16) 0.0001(14) C24 0.0242(18) 0.0292(16) 0.037(2) 0.0019(14) -0.0012(16) -0.0007(14) C25 0.0214(16) 0.0244(14) 0.0313(19) 0.0019(12) 0.0058(15) -0.0007(12) C26 0.0266(18) 0.0255(15) 0.034(2) -0.0018(13) 0.0059(16) -0.0009(13) C27 0.0283(19) 0.0254(15) 0.041(2) -0.0008(14) 0.0082(16) -0.0064(13) C28 0.032(2) 0.0360(17) 0.042(2) -0.0023(16) 0.0114(17) -0.0079(16) C29 0.039(2) 0.0408(19) 0.030(2) 0.0004(15) 0.0086(18) -0.0080(17) C30 0.0306(19) 0.0351(16) 0.0273(19) -0.0050(14) 0.0052(16) -0.0069(15) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 N2 1.775(3) . ? Mo1 C12 2.272(3) . ? Mo1 C6 2.348(4) . ? Mo1 C5 2.358(4) . ? Mo1 C4 2.379(3) . ? Mo1 C2 2.389(3) . ? Mo1 P1 2.4022(9) . ? Mo1 C3 2.408(3) . ? Mo1 Mo2 3.0993(4) . ? Mo2 N1 1.797(3) . ? Mo2 C1 1.976(4) . ? Mo2 C11 2.356(3) . ? Mo2 C7 2.361(4) . ? Mo2 C10 2.363(3) . ? Mo2 C8 2.378(3) . ? Mo2 C9 2.384(4) . ? Mo2 P1 2.5125(8) . ? P1 C25 1.872(3) . ? P1 C19 1.874(3) . ? N1 O1 1.197(4) . ? N2 O2 1.201(4) . ? O3 C1 1.144(5) . ? C2 C3 1.395(5) . ? C2 C6 1.404(5) . ? C2 H2 0.93 . ? C3 C4 1.411(5) . ? C3 H3 0.93 . ? C4 C5 1.404(5) . ? C4 H4 0.93 . ? C5 C6 1.413(5) . ? C5 H5 0.93 . ? C6 H6 0.93 . ? C7 C8 1.417(5) . ? C7 C11 1.417(5) . ? C7 H7 0.93 . ? C8 C9 1.409(5) . ? C8 H8 0.93 . ? C9 C10 1.414(6) . ? C9 H9 0.93 . ? C10 C11 1.427(5) . ? C10 H10 0.93 . ? C11 H11 0.93 . ? C12 C13 1.483(5) . ? C12 H12A 0.97 . ? C12 H12B 0.97 . ? C13 C18 1.400(5) . ? C13 C14 1.404(5) . ? C14 C15 1.374(5) . ? C14 H14 0.93 . ? C15 C16 1.384(6) . ? C15 H15 0.93 . ? C16 C17 1.398(6) . ? C16 H16 0.93 . ? C17 C18 1.375(6) . ? C17 H17 0.93 . ? C18 H18 0.93 . ? C19 C20 1.531(5) . ? C19 C24 1.541(5) . ? C19 H19 0.98 . ? C20 C21 1.523(5) . ? C20 H20A 0.97 . ? C20 H20B 0.97 . ? C21 C22 1.515(5) . ? C21 H21A 0.97 . ? C21 H21B 0.97 . ? C22 C23 1.537(5) . ? C22 H22A 0.97 . ? C22 H22B 0.97 . ? C23 C24 1.530(5) . ? C23 H23A 0.97 . ? C23 H23B 0.97 . ? C24 H24A 0.97 . ? C24 H24B 0.97 . ? C25 C26 1.525(5) . ? C25 C30 1.529(5) . ? C25 H25 0.98 . ? C26 C27 1.545(5) . ? C26 H26A 0.97 . ? C26 H26B 0.97 . ? C27 C28 1.514(6) . ? C27 H27A 0.97 . ? C27 H27B 0.97 . ? C28 C29 1.523(5) . ? C28 H28A 0.97 . ? C28 H28B 0.97 . ? C29 C30 1.532(5) . ? C29 H29A 0.97 . ? C29 H29B 0.97 . ? C30 H30A 0.97 . ? C30 H30B 0.97 . ? 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 N2 Mo1 C12 92.98(13) . . ? N2 Mo1 C6 97.15(14) . . ? C12 Mo1 C6 86.80(13) . . ? N2 Mo1 C5 89.64(13) . . ? C12 Mo1 C5 121.33(13) . . ? C6 Mo1 C5 34.94(13) . . ? N2 Mo1 C4 115.98(13) . . ? C12 Mo1 C4 135.02(13) . . ? C6 Mo1 C4 57.54(12) . . ? C5 Mo1 C4 34.48(12) . . ? N2 Mo1 C2 130.40(13) . . ? C12 Mo1 C2 78.24(12) . . ? C6 Mo1 C2 34.45(13) . . ? C5 Mo1 C2 57.24(13) . . ? C4 Mo1 C2 56.79(12) . . ? N2 Mo1 P1 97.54(10) . . ? C12 Mo1 P1 81.30(10) . . ? C6 Mo1 P1 161.52(10) . . ? C5 Mo1 P1 156.01(9) . . ? C4 Mo1 P1 124.15(9) . . ? C2 Mo1 P1 128.19(9) . . ? N2 Mo1 C3 146.73(13) . . ? C12 Mo1 C3 104.91(13) . . ? C6 Mo1 C3 57.08(12) . . ? C5 Mo1 C3 57.12(12) . . ? C4 Mo1 C3 34.28(13) . . ? C2 Mo1 C3 33.81(12) . . ? P1 Mo1 C3 112.55(9) . . ? N2 Mo1 Mo2 94.30(9) . . ? C12 Mo1 Mo2 133.78(9) . . ? C6 Mo1 Mo2 137.06(8) . . ? C5 Mo1 Mo2 104.31(9) . . ? C4 Mo1 Mo2 80.27(9) . . ? C2 Mo1 Mo2 126.84(8) . . ? P1 Mo1 Mo2 52.50(2) . . ? C3 Mo1 Mo2 93.13(9) . . ? N1 Mo2 C1 87.02(14) . . ? N1 Mo2 C11 123.73(12) . . ? C1 Mo2 C11 85.85(15) . . ? N1 Mo2 C7 97.85(12) . . ? C1 Mo2 C7 108.74(14) . . ? C11 Mo2 C7 34.98(13) . . ? N1 Mo2 C10 155.73(12) . . ? C1 Mo2 C10 99.87(15) . . ? C11 Mo2 C10 35.20(12) . . ? C7 Mo2 C10 57.88(12) . . ? N1 Mo2 C8 103.56(13) . . ? C1 Mo2 C8 142.42(14) . . ? C11 Mo2 C8 58.10(13) . . ? C7 Mo2 C8 34.81(13) . . ? C10 Mo2 C8 57.49(12) . . ? N1 Mo2 C9 135.03(14) . . ? C1 Mo2 C9 134.39(15) . . ? C11 Mo2 C9 58.26(13) . . ? C7 Mo2 C9 57.76(13) . . ? C10 Mo2 C9 34.66(13) . . ? C8 Mo2 C9 34.42(12) . . ? N1 Mo2 P1 99.78(9) . . ? C1 Mo2 P1 76.83(10) . . ? C11 Mo2 P1 132.16(9) . . ? C7 Mo2 P1 161.79(9) . . ? C10 Mo2 P1 104.45(9) . . ? C8 Mo2 P1 134.32(9) . . ? C9 Mo2 P1 105.63(9) . . ? N1 Mo2 Mo1 85.25(9) . . ? C1 Mo2 Mo1 122.94(10) . . ? C11 Mo2 Mo1 142.02(9) . . ? C7 Mo2 Mo1 128.33(10) . . ? C10 Mo2 Mo1 109.47(9) . . ? C8 Mo2 Mo1 94.11(9) . . ? C9 Mo2 Mo1 84.05(9) . . ? P1 Mo2 Mo1 49.34(2) . . ? C25 P1 C19 102.62(16) . . ? C25 P1 Mo1 121.51(11) . . ? C19 P1 Mo1 123.75(12) . . ? C25 P1 Mo2 114.51(11) . . ? C19 P1 Mo2 115.16(10) . . ? Mo1 P1 Mo2 78.16(3) . . ? O1 N1 Mo2 173.3(3) . . ? O2 N2 Mo1 167.5(3) . . ? O3 C1 Mo2 175.7(3) . . ? C3 C2 C6 108.6(3) . . ? C3 C2 Mo1 73.8(2) . . ? C6 C2 Mo1 71.2(2) . . ? C3 C2 H2 125.7 . . ? C6 C2 H2 125.7 . . ? Mo1 C2 H2 121 . . ? C2 C3 C4 107.8(3) . . ? C2 C3 Mo1 72.39(19) . . ? C4 C3 Mo1 71.7(2) . . ? C2 C3 H3 126.1 . . ? C4 C3 H3 126.1 . . ? Mo1 C3 H3 121.5 . . ? C5 C4 C3 108.1(3) . . ? C5 C4 Mo1 71.94(19) . . ? C3 C4 Mo1 73.97(19) . . ? C5 C4 H4 126 . . ? C3 C4 H4 126 . . ? Mo1 C4 H4 119.9 . . ? C4 C5 C6 107.7(3) . . ? C4 C5 Mo1 73.6(2) . . ? C6 C5 Mo1 72.2(2) . . ? C4 C5 H5 126.1 . . ? C6 C5 H5 126.1 . . ? Mo1 C5 H5 120 . . ? C2 C6 C5 107.7(3) . . ? C2 C6 Mo1 74.4(2) . . ? C5 C6 Mo1 72.9(2) . . ? C2 C6 H6 126.2 . . ? C5 C6 H6 126.2 . . ? Mo1 C6 H6 118.5 . . ? C8 C7 C11 108.4(3) . . ? C8 C7 Mo2 73.3(2) . . ? C11 C7 Mo2 72.3(2) . . ? C8 C7 H7 125.8 . . ? C11 C7 H7 125.8 . . ? Mo2 C7 H7 120.4 . . ? C9 C8 C7 108.3(3) . . ? C9 C8 Mo2 73.0(2) . . ? C7 C8 Mo2 71.9(2) . . ? C9 C8 H8 125.8 . . ? C7 C8 H8 125.8 . . ? Mo2 C8 H8 120.9 . . ? C8 C9 C10 107.7(3) . . ? C8 C9 Mo2 72.6(2) . . ? C10 C9 Mo2 71.9(2) . . ? C8 C9 H9 126.1 . . ? C10 C9 H9 126.1 . . ? Mo2 C9 H9 121.2 . . ? C9 C10 C11 108.6(3) . . ? C9 C10 Mo2 73.5(2) . . ? C11 C10 Mo2 72.12(19) . . ? C9 C10 H10 125.7 . . ? C11 C10 H10 125.7 . . ? Mo2 C10 H10 120.5 . . ? C7 C11 C10 107.0(3) . . ? C7 C11 Mo2 72.7(2) . . ? C10 C11 Mo2 72.7(2) . . ? C7 C11 H11 126.5 . . ? C10 C11 H11 126.5 . . ? Mo2 C11 H11 120 . . ? C13 C12 Mo1 115.6(2) . . ? C13 C12 H12A 108.4 . . ? Mo1 C12 H12A 108.4 . . ? C13 C12 H12B 108.4 . . ? Mo1 C12 H12B 108.4 . . ? H12A C12 H12B 107.4 . . ? C18 C13 C14 117.0(3) . . ? C18 C13 C12 121.1(3) . . ? C14 C13 C12 121.9(3) . . ? C15 C14 C13 121.9(3) . . ? C15 C14 H14 119.1 . . ? C13 C14 H14 119.1 . . ? C14 C15 C16 120.6(4) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C15 C16 C17 118.3(4) . . ? C15 C16 H16 120.8 . . ? C17 C16 H16 120.8 . . ? C18 C17 C16 121.1(4) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C17 C18 C13 121.1(4) . . ? C17 C18 H18 119.5 . . ? C13 C18 H18 119.5 . . ? C20 C19 C24 110.1(3) . . ? C20 C19 P1 111.3(3) . . ? C24 C19 P1 113.6(2) . . ? C20 C19 H19 107.2 . . ? C24 C19 H19 107.2 . . ? P1 C19 H19 107.2 . . ? C21 C20 C19 111.7(3) . . ? C21 C20 H20A 109.3 . . ? C19 C20 H20A 109.3 . . ? C21 C20 H20B 109.3 . . ? C19 C20 H20B 109.3 . . ? H20A C20 H20B 107.9 . . ? C22 C21 C20 111.5(3) . . ? C22 C21 H21A 109.3 . . ? C20 C21 H21A 109.3 . . ? C22 C21 H21B 109.3 . . ? C20 C21 H21B 109.3 . . ? H21A C21 H21B 108 . . ? C21 C22 C23 110.6(3) . . ? C21 C22 H22A 109.5 . . ? C23 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? C23 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? C24 C23 C22 112.2(3) . . ? C24 C23 H23A 109.2 . . ? C22 C23 H23A 109.2 . . ? C24 C23 H23B 109.2 . . ? C22 C23 H23B 109.2 . . ? H23A C23 H23B 107.9 . . ? C23 C24 C19 110.8(3) . . ? C23 C24 H24A 109.5 . . ? C19 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C19 C24 H24B 109.5 . . ? H24A C24 H24B 108.1 . . ? C26 C25 C30 112.0(3) . . ? C26 C25 P1 113.6(2) . . ? C30 C25 P1 111.0(2) . . ? C26 C25 H25 106.6 . . ? C30 C25 H25 106.6 . . ? P1 C25 H25 106.6 . . ? C25 C26 C27 112.1(3) . . ? C25 C26 H26A 109.2 . . ? C27 C26 H26A 109.2 . . ? C25 C26 H26B 109.2 . . ? C27 C26 H26B 109.2 . . ? H26A C26 H26B 107.9 . . ? C28 C27 C26 112.0(3) . . ? C28 C27 H27A 109.2 . . ? C26 C27 H27A 109.2 . . ? C28 C27 H27B 109.2 . . ? C26 C27 H27B 109.2 . . ? H27A C27 H27B 107.9 . . ? C27 C28 C29 111.0(3) . . ? C27 C28 H28A 109.4 . . ? C29 C28 H28A 109.4 . . ? C27 C28 H28B 109.4 . . ? C29 C28 H28B 109.4 . . ? H28A C28 H28B 108 . . ? C28 C29 C30 110.9(3) . . ? C28 C29 H29A 109.5 . . ? C30 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? C30 C29 H29B 109.5 . . ? H29A C29 H29B 108 . . ? C25 C30 C29 112.0(3) . . ? C25 C30 H30A 109.2 . . ? C29 C30 H30A 109.2 . . ? C25 C30 H30B 109.2 . . ? C29 C30 H30B 109.2 . . ? H30A C30 H30B 107.9 . . ? #===END data_compound7a __audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C31 H43 Mo2 N2 O3 P1' _chemical_formula_sum 'C31 H43 Mo2 N2 O3 P' _chemical_formula_weight 714.52 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7525(3) _cell_length_b 12.2232(3) _cell_length_c 14.5532(5) _cell_angle_alpha 87.328(3) _cell_angle_beta 75.793(3) _cell_angle_gamma 82.829(2) _cell_volume 1497.32(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100.0(2) _cell_measurement_reflns_used 11290 _cell_measurement_theta_min 3.1271 _cell_measurement_theta_max 73.6465 _cell_measurement_wavelength 1.5418 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.585 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 732 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 7.634 _exptl_absorpt_correction_T_min 0.55172 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_type CuK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'ONYX CCD' _diffrn_measurement_method 'CCD' _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 8.2640 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_unetI/netI 0.0259 _diffrn_reflns_number 14309 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 73.71 _diffrn_reflns_theta_full 70.00 _diffrn_measured_fraction_theta_full 0.978 _diffrn_measured_fraction_theta_max 0.942 _reflns_number_total 5692 _reflns_number_gt 4984 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+10.4207P] 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_number_reflns 5692 _refine_ls_number_parameters 418 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0462 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.1035 _refine_ls_wR_factor_gt 0.1007 _refine_ls_goodness_of_fit_ref 1.246 _refine_ls_restrained_S_all 1.246 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.715 _refine_diff_density_min -0.684 _refine_diff_density_rms 0.119 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.19399(5) 0.39400(3) 0.84883(3) 0.01865(11) Uani 1 1 d . . . Mo2 Mo 0.51612(5) 0.27690(3) 0.84707(3) 0.02096(11) Uani 1 1 d . . . P1 P 0.33396(15) 0.22867(10) 0.75958(9) 0.0190(3) Uani 1 1 d . . . N1 N 0.1171(5) 0.3025(4) 0.9420(3) 0.0224(9) Uani 1 1 d . . . N2 N 0.6672(6) 0.2951(4) 0.7435(3) 0.0295(11) Uani 1 1 d . . . O1 O 0.0421(5) 0.2433(3) 1.0015(3) 0.0309(9) Uani 1 1 d . . . O2 O 0.7818(5) 0.3028(5) 0.6775(3) 0.0478(13) Uani 1 1 d . . . O3 O 0.3152(4) 0.4800(3) 0.9258(3) 0.0246(8) Uani 1 1 d . . . C1 C 0.4394(6) 0.4438(4) 0.8591(4) 0.0228(11) Uani 1 1 d . . . C2 C 0.5266(7) 0.5332(5) 0.8017(4) 0.0294(12) Uani 1 1 d . . . H2A H 0.4527 0.5972 0.7977 0.044 Uiso 1 1 calc R . . H2B H 0.5769 0.5071 0.739 0.044 Uiso 1 1 calc R . . H2C H 0.6056 0.5521 0.8318 0.044 Uiso 1 1 calc R . . C3 C -0.0470(6) 0.4284(5) 0.8061(4) 0.0252(11) Uani 1 1 d . . . H3 H -0.1171 0.3752 0.818 0.03 Uiso 1 1 calc R . . C4 C 0.0733(7) 0.4390(5) 0.7230(4) 0.0288(13) Uani 1 1 d . . . H4 H 0.0969 0.3935 0.6706 0.035 Uiso 1 1 calc R . . C5 C 0.1527(7) 0.5312(4) 0.7326(4) 0.0249(11) Uani 1 1 d . . . H5 H 0.2366 0.557 0.688 0.03 Uiso 1 1 calc R . . C6 C 0.0799(7) 0.5760(4) 0.8228(4) 0.0271(12) Uani 1 1 d . . . H6 H 0.1082 0.637 0.8479 0.033 Uiso 1 1 calc R . . C7 C -0.0426(6) 0.5133(4) 0.8687(4) 0.0240(11) Uani 1 1 d . . . H7 H -0.1084 0.5252 0.9289 0.029 Uiso 1 1 calc R . . C8 C 0.5856(8) 0.2852(5) 0.9933(4) 0.0334(14) Uani 1 1 d . . . H8 H 0.6156 0.3504 1.0101 0.04 Uiso 1 1 calc R . . C9 C 0.4304(8) 0.2544(5) 1.0164(4) 0.0335(14) Uani 1 1 d . . . H9 H 0.3402 0.2953 1.0518 0.04 Uiso 1 1 calc R . . C10 C 0.4359(7) 0.1507(5) 0.9763(4) 0.0298(13) Uani 1 1 d . . . H10 H 0.3499 0.1117 0.9799 0.036 Uiso 1 1 calc R . . C11 C 0.5949(7) 0.1166(5) 0.9297(4) 0.0302(13) Uani 1 1 d . . . H11 H 0.6323 0.0509 0.8976 0.036 Uiso 1 1 calc R . . C12 C 0.6873(7) 0.1994(5) 0.9402(4) 0.0310(13) Uani 1 1 d . . . H12 H 0.7963 0.1979 0.9164 0.037 Uiso 1 1 calc R . . C13 C 0.2262(6) 0.1058(4) 0.7941(4) 0.0224(11) Uani 1 1 d . . . H13 H 0.1749 0.1153 0.8616 0.027 Uiso 1 1 calc R . . C14 C 0.0902(7) 0.1023(5) 0.7465(4) 0.0321(13) Uani 1 1 d . . . H14A H 0.1327 0.0909 0.6791 0.039 Uiso 1 1 calc R . . H14B H 0.0233 0.1724 0.7545 0.039 Uiso 1 1 calc R . . C15 C -0.0099(7) 0.0092(5) 0.7890(5) 0.0407(16) Uani 1 1 d . . . H15A H -0.0622 0.0253 0.8546 0.049 Uiso 1 1 calc R . . H15B H -0.0913 0.0059 0.7548 0.049 Uiso 1 1 calc R . . C16 C 0.0909(7) -0.1024(5) 0.7842(5) 0.0352(14) Uani 1 1 d . . . H16A H 0.0252 -0.1581 0.8153 0.042 Uiso 1 1 calc R . . H16B H 0.1338 -0.1227 0.7184 0.042 Uiso 1 1 calc R . . C17 C 0.2252(8) -0.0982(5) 0.8317(5) 0.0348(14) Uani 1 1 d . . . H17A H 0.2912 -0.1687 0.8248 0.042 Uiso 1 1 calc R . . H17B H 0.182 -0.0856 0.8988 0.042 Uiso 1 1 calc R . . C18 C 0.3275(7) -0.0066(5) 0.7888(4) 0.0314(13) Uani 1 1 d . . . H18A H 0.4093 -0.004 0.8228 0.038 Uiso 1 1 calc R . . H18B H 0.3791 -0.023 0.7231 0.038 Uiso 1 1 calc R . . C19 C 0.3933(6) 0.2329(4) 0.6278(4) 0.0225(11) Uani 1 1 d . . . H19 H 0.3006 0.2201 0.6052 0.027 Uiso 1 1 calc R . . C20 C 0.4444(7) 0.3444(5) 0.5852(4) 0.0270(12) Uani 1 1 d . . . H20A H 0.3612 0.4031 0.61 0.032 Uiso 1 1 calc R . . H20B H 0.5393 0.3581 0.6038 0.032 Uiso 1 1 calc R . . C21 C 0.4771(7) 0.3448(5) 0.4774(4) 0.0293(12) Uani 1 1 d . . . H21A H 0.3805 0.3353 0.4588 0.035 Uiso 1 1 calc R . . H21B H 0.5099 0.4154 0.4523 0.035 Uiso 1 1 calc R . . C22 C 0.6062(7) 0.2529(5) 0.4357(4) 0.0320(13) Uani 1 1 d . . . H22A H 0.6197 0.2517 0.3676 0.038 Uiso 1 1 calc R . . H22B H 0.706 0.2669 0.4481 0.038 Uiso 1 1 calc R . . C23 C 0.5634(8) 0.1419(5) 0.4786(4) 0.0334(14) Uani 1 1 d . . . H23A H 0.651 0.0856 0.4549 0.04 Uiso 1 1 calc R . . H23B H 0.4715 0.1238 0.459 0.04 Uiso 1 1 calc R . . C24 C 0.5268(7) 0.1419(5) 0.5872(4) 0.0304(13) Uani 1 1 d . . . H24A H 0.4958 0.0709 0.612 0.037 Uiso 1 1 calc R . . H24B H 0.6216 0.1532 0.6071 0.037 Uiso 1 1 calc R . . C70 C -0.0299(19) 0.4111(12) 0.4825(10) 0.048(4) Uani 0.5 1 d P A 1 H70A H 0.0313 0.4724 0.4689 0.072 Uiso 0.5 1 calc PR A 1 H70B H -0.0562 0.3965 0.5496 0.072 Uiso 0.5 1 calc PR A 1 H70C H -0.1257 0.4284 0.4611 0.072 Uiso 0.5 1 calc PR A 1 C71 C 0.065(3) 0.311(3) 0.4320(16) 0.043(6) Uani 0.5 1 d P A 1 C72 C 0.059(2) 0.207(2) 0.4756(12) 0.039(4) Uani 0.5 1 d P A 1 H72 H -0.0104 0.1983 0.5343 0.047 Uiso 0.5 1 calc PR A 1 C73 C 0.157(2) 0.1177(15) 0.4315(15) 0.040(4) Uani 0.5 1 d P A 1 H73 H 0.1567 0.0493 0.4622 0.048 Uiso 0.5 1 calc PR A 1 C74 C 0.254(2) 0.128(2) 0.3430(19) 0.046(5) Uani 0.5 1 d P A 1 H74 H 0.3211 0.0688 0.3132 0.056 Uiso 0.5 1 calc PR A 1 C75 C 0.248(2) 0.232(3) 0.2995(13) 0.057(7) Uani 0.5 1 d P A 1 H75 H 0.3079 0.239 0.2378 0.068 Uiso 0.5 1 calc PR A 1 C76 C 0.162(2) 0.3179(16) 0.3404(13) 0.043(5) Uani 0.5 1 d P A 1 H76 H 0.1657 0.3856 0.3085 0.052 Uiso 0.5 1 calc PR A 1 C80 C 0.291(2) 0.2124(18) 0.2401(19) 0.076(6) Uani 0.5 1 d P B 2 H80A H 0.4011 0.1895 0.2356 0.115 Uiso 0.5 1 calc PR B 2 H80B H 0.2761 0.2892 0.2235 0.115 Uiso 0.5 1 calc PR B 2 H80C H 0.2542 0.1701 0.1975 0.115 Uiso 0.5 1 calc PR B 2 C81 C 0.204(2) 0.195(2) 0.3328(15) 0.046(4) Uani 0.5 1 d P B 2 C82 C 0.108(3) 0.289(2) 0.385(2) 0.053(6) Uani 0.5 1 d P B 2 H82 H 0.108 0.3594 0.3576 0.063 Uiso 0.5 1 calc PR B 2 C83 C 0.022(3) 0.275(2) 0.4723(17) 0.050(5) Uani 0.5 1 d P B 2 H83 H -0.0375 0.3347 0.5062 0.061 Uiso 0.5 1 calc PR B 2 C84 C 0.022(3) 0.1664(19) 0.5142(17) 0.062(5) Uani 0.5 1 d P B 2 H84 H -0.0374 0.1558 0.5757 0.074 Uiso 0.5 1 calc PR B 2 C85 C 0.111(2) 0.0757(19) 0.4616(18) 0.064(5) Uani 0.5 1 d P B 2 H85 H 0.1118 0.0051 0.4884 0.077 Uiso 0.5 1 calc PR B 2 C86 C 0.199(3) 0.093(2) 0.370(3) 0.064(8) Uani 0.5 1 d P B 2 H86 H 0.2536 0.0328 0.3337 0.077 Uiso 0.5 1 calc PR B 2 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 0.0181(2) 0.0180(2) 0.0207(2) -0.00521(15) -0.00534(15) -0.00199(15) Mo2 0.0199(2) 0.0219(2) 0.0236(2) -0.00745(16) -0.00929(16) -0.00124(16) P1 0.0201(6) 0.0174(6) 0.0215(6) -0.0059(5) -0.0070(5) -0.0033(5) N1 0.019(2) 0.021(2) 0.029(2) -0.0092(19) -0.0079(18) -0.0036(18) N2 0.024(2) 0.037(3) 0.032(3) -0.011(2) -0.012(2) -0.007(2) O1 0.033(2) 0.028(2) 0.029(2) -0.0002(17) -0.0013(17) -0.0108(17) O2 0.025(2) 0.089(4) 0.030(2) -0.016(2) 0.0002(18) -0.015(2) O3 0.0238(19) 0.0264(19) 0.0257(19) -0.0102(15) -0.0079(15) -0.0041(15) C1 0.019(3) 0.026(3) 0.026(3) -0.009(2) -0.010(2) 0.000(2) C2 0.028(3) 0.027(3) 0.036(3) -0.007(2) -0.006(2) -0.011(2) C3 0.021(3) 0.024(3) 0.033(3) -0.003(2) -0.011(2) 0.000(2) C4 0.030(3) 0.030(3) 0.028(3) -0.007(2) -0.015(2) 0.008(2) C5 0.026(3) 0.023(3) 0.025(3) 0.003(2) -0.006(2) -0.001(2) C6 0.034(3) 0.019(3) 0.029(3) -0.002(2) -0.014(2) 0.006(2) C7 0.020(3) 0.022(3) 0.030(3) -0.004(2) -0.004(2) -0.001(2) C8 0.046(4) 0.031(3) 0.030(3) -0.007(2) -0.026(3) 0.004(3) C9 0.041(4) 0.037(3) 0.022(3) -0.003(2) -0.012(2) 0.005(3) C10 0.035(3) 0.030(3) 0.030(3) 0.010(2) -0.017(2) -0.009(2) C11 0.034(3) 0.025(3) 0.036(3) -0.004(2) -0.018(3) 0.000(2) C12 0.031(3) 0.030(3) 0.038(3) -0.004(2) -0.021(3) 0.001(2) C13 0.022(3) 0.016(2) 0.032(3) -0.005(2) -0.006(2) -0.010(2) C14 0.030(3) 0.031(3) 0.041(3) 0.002(3) -0.017(3) -0.007(2) C15 0.021(3) 0.032(3) 0.072(5) -0.014(3) -0.011(3) -0.010(3) C16 0.036(3) 0.028(3) 0.043(4) -0.004(3) -0.008(3) -0.007(3) C17 0.043(4) 0.025(3) 0.039(3) 0.001(3) -0.014(3) -0.007(3) C18 0.032(3) 0.025(3) 0.042(3) -0.001(2) -0.017(3) -0.003(2) C19 0.020(3) 0.026(3) 0.025(3) -0.008(2) -0.008(2) -0.007(2) C20 0.027(3) 0.026(3) 0.026(3) -0.005(2) -0.003(2) -0.002(2) C21 0.029(3) 0.029(3) 0.029(3) 0.001(2) -0.006(2) -0.004(2) C22 0.035(3) 0.035(3) 0.024(3) -0.009(2) -0.003(2) -0.006(3) C23 0.047(4) 0.029(3) 0.023(3) -0.008(2) -0.004(3) -0.007(3) C24 0.039(3) 0.024(3) 0.026(3) -0.008(2) -0.006(2) -0.001(2) C70 0.064(10) 0.050(9) 0.037(7) 0.006(6) -0.019(7) -0.018(7) C71 0.032(11) 0.081(18) 0.021(13) 0.020(10) -0.012(9) -0.023(10) C72 0.032(9) 0.059(14) 0.028(9) 0.027(9) -0.013(7) -0.008(9) C73 0.046(11) 0.037(10) 0.045(10) 0.022(8) -0.021(9) -0.023(8) C74 0.018(11) 0.066(17) 0.066(14) -0.012(11) -0.027(10) -0.005(9) C75 0.033(11) 0.13(2) 0.011(9) 0.018(11) -0.002(7) -0.030(12) C76 0.033(9) 0.076(12) 0.024(10) 0.029(9) -0.009(7) -0.025(8) C80 0.049(11) 0.075(14) 0.11(2) -0.008(14) -0.026(13) -0.011(10) C81 0.042(12) 0.069(14) 0.031(11) 0.010(9) -0.016(9) -0.015(11) C82 0.049(15) 0.069(14) 0.047(18) -0.005(14) -0.026(13) -0.005(11) C83 0.044(12) 0.072(17) 0.040(13) -0.019(12) -0.028(10) 0.018(11) C84 0.064(13) 0.066(14) 0.061(13) -0.014(11) -0.037(11) 0.017(11) C85 0.038(11) 0.060(13) 0.097(18) 0.002(12) -0.021(10) -0.006(9) C86 0.032(15) 0.066(17) 0.11(3) -0.021(16) -0.045(16) -0.005(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 N1 1.772(5) . ? Mo1 O3 2.111(3) . ? Mo1 C3 2.326(5) . ? Mo1 C4 2.342(5) . ? Mo1 C7 2.343(5) . ? Mo1 C1 2.345(5) . ? Mo1 C6 2.375(5) . ? Mo1 C5 2.384(5) . ? Mo1 P1 2.4733(13) . ? Mo1 Mo2 2.9931(6) . ? Mo2 N2 1.770(5) . ? Mo2 C1 2.068(5) . ? Mo2 C12 2.346(5) . ? Mo2 C8 2.363(5) . ? Mo2 C11 2.369(6) . ? Mo2 C10 2.400(6) . ? Mo2 C9 2.407(6) . ? Mo2 P1 2.4108(13) . ? P1 C13 1.856(5) . ? P1 C19 1.859(5) . ? N1 O1 1.219(6) . ? N2 O2 1.216(6) . ? O3 C1 1.313(6) . ? C1 C2 1.512(8) . ? C2 H2A 0.96 . ? C2 H2B 0.96 . ? C2 H2C 0.96 . ? C3 C4 1.409(8) . ? C3 C7 1.423(7) . ? C3 H3 0.93 . ? C4 C5 1.425(8) . ? C4 H4 0.93 . ? C5 C6 1.414(7) . ? C5 H5 0.93 . ? C6 C7 1.410(8) . ? C6 H6 0.93 . ? C7 H7 0.93 . ? C8 C9 1.412(9) . ? C8 C12 1.412(8) . ? C8 H8 0.93 . ? C9 C10 1.411(8) . ? C9 H9 0.93 . ? C10 C11 1.410(8) . ? C10 H10 0.93 . ? C11 C12 1.408(8) . ? C11 H11 0.93 . ? C12 H12 0.93 . ? C13 C14 1.523(7) . ? C13 C18 1.534(7) . ? C13 H13 0.98 . ? C14 C15 1.537(8) . ? C14 H14A 0.97 . ? C14 H14B 0.97 . ? C15 C16 1.524(8) . ? C15 H15A 0.97 . ? C15 H15B 0.97 . ? C16 C17 1.509(9) . ? C16 H16A 0.97 . ? C16 H16B 0.97 . ? C17 C18 1.535(8) . ? C17 H17A 0.97 . ? C17 H17B 0.97 . ? C18 H18A 0.97 . ? C18 H18B 0.97 . ? C19 C24 1.533(7) . ? C19 C20 1.542(8) . ? C19 H19 0.98 . ? C20 C21 1.524(8) . ? C20 H20A 0.97 . ? C20 H20B 0.97 . ? C21 C22 1.522(8) . ? C21 H21A 0.97 . ? C21 H21B 0.97 . ? C22 C23 1.517(8) . ? C22 H22A 0.97 . ? C22 H22B 0.97 . ? C23 C24 1.533(8) . ? C23 H23A 0.97 . ? C23 H23B 0.97 . ? C24 H24A 0.97 . ? C24 H24B 0.97 . ? C70 C71 1.50(3) . ? C70 H70A 0.96 . ? C70 H70B 0.96 . ? C70 H70C 0.96 . ? C71 C72 1.39(3) . ? C71 C76 1.40(2) . ? C72 C73 1.38(3) . ? C72 H72 0.93 . ? C73 C74 1.37(3) . ? C73 H73 0.93 . ? C74 C75 1.38(3) . ? C74 H74 0.93 . ? C75 C76 1.29(3) . ? C75 H75 0.93 . ? C76 H76 0.93 . ? C80 C81 1.40(3) . ? C80 H80A 0.96 . ? C80 H80B 0.96 . ? C80 H80C 0.96 . ? C81 C86 1.34(4) . ? C81 C82 1.46(3) . ? C82 C83 1.32(3) . ? C82 H82 0.93 . ? C83 C84 1.43(3) . ? C83 H83 0.93 . ? C84 C85 1.41(3) . ? C84 H84 0.93 . ? C85 C86 1.39(4) . ? C85 H85 0.93 . ? C86 H86 0.93 . ? 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 O3 96.61(17) . . ? N1 Mo1 C3 92.4(2) . . ? O3 Mo1 C3 134.85(16) . . ? N1 Mo1 C4 122.1(2) . . ? O3 Mo1 C4 134.88(18) . . ? C3 Mo1 C4 35.1(2) . . ? N1 Mo1 C7 94.66(19) . . ? O3 Mo1 C7 99.56(16) . . ? C3 Mo1 C7 35.48(18) . . ? C4 Mo1 C7 58.55(19) . . ? N1 Mo1 C1 111.97(19) . . ? O3 Mo1 C1 33.75(16) . . ? C3 Mo1 C1 152.4(2) . . ? C4 Mo1 C1 125.5(2) . . ? C7 Mo1 C1 125.47(18) . . ? N1 Mo1 C6 126.2(2) . . ? O3 Mo1 C6 81.46(17) . . ? C3 Mo1 C6 58.2(2) . . ? C4 Mo1 C6 57.90(19) . . ? C7 Mo1 C6 34.78(19) . . ? C1 Mo1 C6 95.7(2) . . ? N1 Mo1 C5 150.1(2) . . ? O3 Mo1 C5 100.01(17) . . ? C3 Mo1 C5 58.4(2) . . ? C4 Mo1 C5 35.1(2) . . ? C7 Mo1 C5 58.18(19) . . ? C1 Mo1 C5 95.40(19) . . ? C6 Mo1 C5 34.56(18) . . ? N1 Mo1 P1 86.93(14) . . ? O3 Mo1 P1 119.33(10) . . ? C3 Mo1 P1 105.23(14) . . ? C4 Mo1 P1 87.52(14) . . ? C7 Mo1 P1 140.67(13) . . ? C1 Mo1 P1 89.33(13) . . ? C6 Mo1 P1 140.46(14) . . ? C5 Mo1 P1 105.97(13) . . ? N1 Mo1 Mo2 87.32(14) . . ? O3 Mo1 Mo2 68.36(10) . . ? C3 Mo1 Mo2 156.49(13) . . ? C4 Mo1 Mo2 129.67(14) . . ? C7 Mo1 Mo2 167.92(13) . . ? C1 Mo1 Mo2 43.51(13) . . ? C6 Mo1 Mo2 137.73(15) . . ? C5 Mo1 Mo2 121.96(13) . . ? P1 Mo1 Mo2 51.27(3) . . ? N2 Mo2 C1 93.4(2) . . ? N2 Mo2 C12 95.8(2) . . ? C1 Mo2 C12 118.0(2) . . ? N2 Mo2 C8 116.5(2) . . ? C1 Mo2 C8 87.7(2) . . ? C12 Mo2 C8 34.9(2) . . ? N2 Mo2 C11 108.9(2) . . ? C1 Mo2 C11 144.4(2) . . ? C12 Mo2 C11 34.8(2) . . ? C8 Mo2 C11 57.7(2) . . ? N2 Mo2 C10 142.7(2) . . ? C1 Mo2 C10 121.2(2) . . ? C12 Mo2 C10 57.4(2) . . ? C8 Mo2 C10 57.3(2) . . ? C11 Mo2 C10 34.4(2) . . ? N2 Mo2 C9 150.6(2) . . ? C1 Mo2 C9 90.0(2) . . ? C12 Mo2 C9 57.4(2) . . ? C8 Mo2 C9 34.4(2) . . ? C11 Mo2 C9 57.1(2) . . ? C10 Mo2 C9 34.1(2) . . ? N2 Mo2 P1 93.45(15) . . ? C1 Mo2 P1 98.02(14) . . ? C12 Mo2 P1 142.04(15) . . ? C8 Mo2 P1 149.20(17) . . ? C11 Mo2 P1 107.73(14) . . ? C10 Mo2 P1 94.79(14) . . ? C9 Mo2 P1 114.97(16) . . ? N2 Mo2 Mo1 116.20(16) . . ? C1 Mo2 Mo1 51.32(14) . . ? C12 Mo2 Mo1 145.46(16) . . ? C8 Mo2 Mo1 113.05(15) . . ? C11 Mo2 Mo1 131.04(15) . . ? C10 Mo2 Mo1 97.57(14) . . ? C9 Mo2 Mo1 88.39(15) . . ? P1 Mo2 Mo1 53.16(3) . . ? C13 P1 C19 106.7(2) . . ? C13 P1 Mo2 120.78(18) . . ? C19 P1 Mo2 118.97(17) . . ? C13 P1 Mo1 112.13(17) . . ? C19 P1 Mo1 120.50(18) . . ? Mo2 P1 Mo1 75.58(4) . . ? O1 N1 Mo1 169.7(4) . . ? O2 N2 Mo2 173.4(5) . . ? C1 O3 Mo1 82.9(3) . . ? O3 C1 C2 114.6(5) . . ? O3 C1 Mo2 120.5(4) . . ? C2 C1 Mo2 124.6(4) . . ? O3 C1 Mo1 63.3(3) . . ? C2 C1 Mo1 126.4(4) . . ? Mo2 C1 Mo1 85.17(19) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 C7 108.0(5) . . ? C4 C3 Mo1 73.0(3) . . ? C7 C3 Mo1 72.9(3) . . ? C4 C3 H3 126 . . ? C7 C3 H3 126 . . ? Mo1 C3 H3 119.9 . . ? C3 C4 C5 108.4(5) . . ? C3 C4 Mo1 71.8(3) . . ? C5 C4 Mo1 74.1(3) . . ? C3 C4 H4 125.8 . . ? C5 C4 H4 125.8 . . ? Mo1 C4 H4 120.1 . . ? C6 C5 C4 107.1(5) . . ? C6 C5 Mo1 72.4(3) . . ? C4 C5 Mo1 70.8(3) . . ? C6 C5 H5 126.5 . . ? C4 C5 H5 126.5 . . ? Mo1 C5 H5 122.1 . . ? C7 C6 C5 108.9(5) . . ? C7 C6 Mo1 71.3(3) . . ? C5 C6 Mo1 73.1(3) . . ? C7 C6 H6 125.5 . . ? C5 C6 H6 125.5 . . ? Mo1 C6 H6 121.7 . . ? C6 C7 C3 107.6(5) . . ? C6 C7 Mo1 73.9(3) . . ? C3 C7 Mo1 71.6(3) . . ? C6 C7 H7 126.2 . . ? C3 C7 H7 126.2 . . ? Mo1 C7 H7 120.1 . . ? C9 C8 C12 107.8(5) . . ? C9 C8 Mo2 74.5(3) . . ? C12 C8 Mo2 71.9(3) . . ? C9 C8 H8 126.1 . . ? C12 C8 H8 126.1 . . ? Mo2 C8 H8 119.4 . . ? C10 C9 C8 108.0(5) . . ? C10 C9 Mo2 72.7(3) . . ? C8 C9 Mo2 71.1(3) . . ? C10 C9 H9 126 . . ? C8 C9 H9 126 . . ? Mo2 C9 H9 121.9 . . ? C11 C10 C9 108.0(5) . . ? C11 C10 Mo2 71.6(3) . . ? C9 C10 Mo2 73.2(3) . . ? C11 C10 H10 126 . . ? C9 C10 H10 126 . . ? Mo2 C10 H10 121 . . ? C12 C11 C10 108.1(5) . . ? C12 C11 Mo2 71.7(3) . . ? C10 C11 Mo2 74.0(3) . . ? C12 C11 H11 126 . . ? C10 C11 H11 126 . . ? Mo2 C11 H11 120.1 . . ? C11 C12 C8 108.1(6) . . ? C11 C12 Mo2 73.5(3) . . ? C8 C12 Mo2 73.2(3) . . ? C11 C12 H12 126 . . ? C8 C12 H12 126 . . ? Mo2 C12 H12 119.2 . . ? C14 C13 C18 110.7(4) . . ? C14 C13 P1 113.5(4) . . ? C18 C13 P1 116.8(4) . . ? C14 C13 H13 104.8 . . ? C18 C13 H13 104.8 . . ? P1 C13 H13 104.8 . . ? C13 C14 C15 111.0(5) . . ? C13 C14 H14A 109.4 . . ? C15 C14 H14A 109.4 . . ? C13 C14 H14B 109.4 . . ? C15 C14 H14B 109.4 . . ? H14A C14 H14B 108 . . ? C16 C15 C14 111.9(5) . . ? C16 C15 H15A 109.2 . . ? C14 C15 H15A 109.2 . . ? C16 C15 H15B 109.2 . . ? C14 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? C17 C16 C15 110.6(5) . . ? C17 C16 H16A 109.5 . . ? C15 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? C16 C17 C18 111.6(5) . . ? C16 C17 H17A 109.3 . . ? C18 C17 H17A 109.3 . . ? C16 C17 H17B 109.3 . . ? C18 C17 H17B 109.3 . . ? H17A C17 H17B 108 . . ? C13 C18 C17 111.0(5) . . ? C13 C18 H18A 109.4 . . ? C17 C18 H18A 109.4 . . ? C13 C18 H18B 109.4 . . ? C17 C18 H18B 109.4 . . ? H18A C18 H18B 108 . . ? C24 C19 C20 108.2(4) . . ? C24 C19 P1 112.5(4) . . ? C20 C19 P1 114.1(3) . . ? C24 C19 H19 107.2 . . ? C20 C19 H19 107.2 . . ? P1 C19 H19 107.2 . . ? C21 C20 C19 111.0(4) . . ? C21 C20 H20A 109.4 . . ? C19 C20 H20A 109.4 . . ? C21 C20 H20B 109.4 . . ? C19 C20 H20B 109.4 . . ? H20A C20 H20B 108 . . ? C22 C21 C20 111.1(5) . . ? C22 C21 H21A 109.4 . . ? C20 C21 H21A 109.4 . . ? C22 C21 H21B 109.4 . . ? C20 C21 H21B 109.4 . . ? H21A C21 H21B 108 . . ? C23 C22 C21 110.7(5) . . ? C23 C22 H22A 109.5 . . ? C21 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? C22 C23 C24 111.9(5) . . ? C22 C23 H23A 109.2 . . ? C24 C23 H23A 109.2 . . ? C22 C23 H23B 109.2 . . ? C24 C23 H23B 109.2 . . ? H23A C23 H23B 107.9 . . ? C19 C24 C23 111.1(5) . . ? C19 C24 H24A 109.4 . . ? C23 C24 H24A 109.4 . . ? C19 C24 H24B 109.4 . . ? C23 C24 H24B 109.4 . . ? H24A C24 H24B 108 . . ? C72 C71 C76 118(2) . . ? C72 C71 C70 121(2) . . ? C76 C71 C70 122(2) . . ? C73 C72 C71 119.8(17) . . ? C73 C72 H72 120.1 . . ? C71 C72 H72 120.1 . . ? C74 C73 C72 120.7(18) . . ? C74 C73 H73 119.6 . . ? C72 C73 H73 119.6 . . ? C73 C74 C75 117(2) . . ? C73 C74 H74 121.3 . . ? C75 C74 H74 121.3 . . ? C76 C75 C74 123.3(19) . . ? C76 C75 H75 118.4 . . ? C74 C75 H75 118.4 . . ? C75 C76 C71 121(2) . . ? C75 C76 H76 119.6 . . ? C71 C76 H76 119.6 . . ? C81 C80 H80A 109.5 . . ? C81 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C81 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C86 C81 C80 120(3) . . ? C86 C81 C82 121(2) . . ? C80 C81 C82 119(2) . . ? C83 C82 C81 120(2) . . ? C83 C82 H82 120 . . ? C81 C82 H82 120 . . ? C82 C83 C84 120(2) . . ? C82 C83 H83 120.1 . . ? C84 C83 H83 120.1 . . ? C85 C84 C83 120(2) . . ? C85 C84 H84 120.1 . . ? C83 C84 H84 120.1 . . ? C86 C85 C84 120(2) . . ? C86 C85 H85 120.2 . . ? C84 C85 H85 120.2 . . ? C81 C86 C85 120(3) . . ? C81 C86 H86 119.9 . . ? C85 C86 H86 119.9 . . ? #===END data_compound11 _audit_creation_date 2009-03-17T18:18:56-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C28 H37 Mo2 N2 O2 P1' _chemical_formula_sum 'C28 H37 Mo2 N2 O2 P1' _chemical_formula_weight 656.44 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 14.7493(8) _cell_length_b 19.0347(11) _cell_length_c 18.8952(8) _cell_angle_alpha 90 _cell_angle_beta 93.055(2) _cell_angle_gamma 90 _cell_volume 5297.3(5) _cell_formula_units_Z 8 _cell_measurement_temperature 100.0(1) _cell_measurement_reflns_used 1952 _cell_measurement_theta_min 2.4095 _cell_measurement_theta_max 25.8175 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.644 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2664 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.036 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'BRUKER Sadabs' _exptl_absorpt_correction_T_min 0.817 _exptl_absorpt_correction_T_max 0.930 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100.0(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_monochromador graphite _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'BRUKER APPEX-II CCD' _diffrn_measurement_method 'omega/phi scans' _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0573 _diffrn_reflns_av_unetI/netI 0.052 _diffrn_reflns_number 40199 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 26.02 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _reflns_number_total 10434 _reflns_number_gt 8126 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'BRUKER APEX' _computing_cell_refinement 'BRUKER APEX' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0212P)^2^+9.4585P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 10434 _refine_ls_number_parameters 639 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0545 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.0778 _refine_ls_wR_factor_gt 0.0706 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.815 _refine_diff_density_min -0.677 _refine_diff_density_rms 0.113 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.13817(2) 0.190717(17) 0.555127(16) 0.01198(8) Uani 1 1 d . . . Mo2 Mo 0.12058(2) 0.302973(17) 0.445682(16) 0.01144(8) Uani 1 1 d . . . P1 P 0.15029(6) 0.17794(5) 0.42991(5) 0.0106(2) Uani 1 1 d . . . N1 N 0.0255(2) 0.15834(17) 0.54505(15) 0.0136(7) Uani 1 1 d . . . N2 N 0.0101(2) 0.28957(16) 0.40537(16) 0.0153(7) Uani 1 1 d . . . O1 O -0.04861(18) 0.12976(15) 0.54018(13) 0.0205(6) Uani 1 1 d . . . O2 O -0.06524(18) 0.28461(15) 0.37755(14) 0.0244(7) Uani 1 1 d . . . C1 C 0.1026(3) 0.2991(2) 0.56965(19) 0.0162(8) Uani 1 1 d . . . C2 C 0.0171(3) 0.3266(2) 0.5445(2) 0.0202(9) Uani 1 1 d . . . C3 C -0.0102(3) 0.3968(2) 0.5584(2) 0.0260(10) Uani 1 1 d . . . H3 H -0.0661 0.4129 0.54 0.031 Uiso 1 1 calc R . . C4 C 0.0449(3) 0.4408(2) 0.5984(2) 0.0280(11) Uani 1 1 d . . . H4 H 0.0265 0.4864 0.6082 0.034 Uiso 1 1 calc R . . C5 C 0.1305(3) 0.4157(2) 0.6248(2) 0.0244(10) Uani 1 1 d . . . H5 H 0.168 0.4445 0.6533 0.029 Uiso 1 1 calc R . . C6 C 0.1586(3) 0.3493(2) 0.60886(18) 0.0195(9) Uani 1 1 d . . . H6 H 0.2171 0.3358 0.6241 0.023 Uiso 1 1 calc R . . C7 C 0.2871(3) 0.1426(2) 0.5774(2) 0.0195(9) Uani 1 1 d . . . H7 H 0.3245 0.1327 0.5406 0.023 Uiso 1 1 calc R . . C8 C 0.2241(3) 0.0960(2) 0.60548(19) 0.0177(9) Uani 1 1 d . . . H8 H 0.2126 0.0502 0.5904 0.021 Uiso 1 1 calc R . . C9 C 0.1815(3) 0.1309(2) 0.66046(19) 0.0192(9) Uani 1 1 d . . . H9 H 0.1371 0.1124 0.6882 0.023 Uiso 1 1 calc R . . C10 C 0.2185(3) 0.1994(2) 0.66575(19) 0.0184(9) Uani 1 1 d . . . H10 H 0.2025 0.2339 0.6976 0.022 Uiso 1 1 calc R . . C11 C 0.2837(3) 0.2064(2) 0.61445(19) 0.0191(9) Uani 1 1 d . . . H11 H 0.3184 0.2461 0.6065 0.023 Uiso 1 1 calc R . . C12 C 0.2696(3) 0.3288(2) 0.4082(2) 0.0182(9) Uani 1 1 d . . . H12 H 0.3138 0.2944 0.4043 0.022 Uiso 1 1 calc R . . C13 C 0.2041(3) 0.3485(2) 0.3544(2) 0.0199(9) Uani 1 1 d . . . H13 H 0.1968 0.3287 0.3095 0.024 Uiso 1 1 calc R . . C14 C 0.1519(3) 0.4037(2) 0.3813(2) 0.0195(9) Uani 1 1 d . . . H14 H 0.1053 0.4277 0.3567 0.023 Uiso 1 1 calc R . . C15 C 0.1829(3) 0.4159(2) 0.4521(2) 0.0199(9) Uani 1 1 d . . . H15 H 0.1591 0.4484 0.4828 0.024 Uiso 1 1 calc R . . C16 C 0.2569(3) 0.3697(2) 0.4681(2) 0.0189(9) Uani 1 1 d . . . H16 H 0.2908 0.3673 0.511 0.023 Uiso 1 1 calc R . . C17 C 0.2585(2) 0.1457(2) 0.39644(18) 0.0127(8) Uani 1 1 d . . . H17 H 0.3065 0.1697 0.4252 0.015 Uiso 1 1 calc R . . C18 C 0.2774(3) 0.1628(2) 0.31913(18) 0.0165(8) Uani 1 1 d . . . H18A H 0.2687 0.2127 0.3106 0.02 Uiso 1 1 calc R . . H18B H 0.235 0.1374 0.2876 0.02 Uiso 1 1 calc R . . C19 C 0.3751(3) 0.1422(2) 0.3036(2) 0.0221(9) Uani 1 1 d . . . H19A H 0.3853 0.1518 0.2543 0.027 Uiso 1 1 calc R . . H19B H 0.4173 0.1706 0.3325 0.027 Uiso 1 1 calc R . . C20 C 0.3934(3) 0.0654(2) 0.3188(2) 0.0250(10) Uani 1 1 d . . . H20A H 0.4566 0.0551 0.3116 0.03 Uiso 1 1 calc R . . H20B H 0.3563 0.0368 0.2861 0.03 Uiso 1 1 calc R . . C21 C 0.3721(3) 0.0468(2) 0.3952(2) 0.0212(9) Uani 1 1 d . . . H21A H 0.3805 -0.0033 0.4028 0.025 Uiso 1 1 calc R . . H21B H 0.4136 0.0715 0.428 0.025 Uiso 1 1 calc R . . C22 C 0.2747(3) 0.0669(2) 0.4091(2) 0.0171(9) Uani 1 1 d . . . H22A H 0.2624 0.0554 0.4576 0.02 Uiso 1 1 calc R . . H22B H 0.2333 0.0401 0.378 0.02 Uiso 1 1 calc R . . C23 C 0.0537(2) 0.13201(19) 0.38470(18) 0.0123(8) Uani 1 1 d . . . H23 H 0 0.154 0.4038 0.015 Uiso 1 1 calc R . . C24 C 0.0408(3) 0.1429(2) 0.30428(18) 0.0165(8) Uani 1 1 d . . . H24A H 0.047 0.1924 0.2933 0.02 Uiso 1 1 calc R . . H24B H 0.0874 0.1174 0.2806 0.02 Uiso 1 1 calc R . . C25 C -0.0526(3) 0.1172(2) 0.2774(2) 0.0212(9) Uani 1 1 d . . . H25A H -0.0587 0.1224 0.2263 0.025 Uiso 1 1 calc R . . H25B H -0.099 0.1457 0.2979 0.025 Uiso 1 1 calc R . . C26 C -0.0667(3) 0.0402(2) 0.2969(2) 0.0240(10) Uani 1 1 d . . . H26A H -0.1284 0.0265 0.2829 0.029 Uiso 1 1 calc R . . H26B H -0.0258 0.0111 0.2711 0.029 Uiso 1 1 calc R . . C27 C -0.0496(3) 0.0277(2) 0.3763(2) 0.0205(9) Uani 1 1 d . . . H27A H -0.0957 0.0519 0.4018 0.025 Uiso 1 1 calc R . . H27B H -0.0544 -0.0222 0.3861 0.025 Uiso 1 1 calc R . . C28 C 0.0437(3) 0.0537(2) 0.4021(2) 0.0166(8) Uani 1 1 d . . . H28A H 0.0901 0.027 0.3795 0.02 Uiso 1 1 calc R . . H28B H 0.0518 0.0467 0.4529 0.02 Uiso 1 1 calc R . . Mo1B Mo 0.36966(2) -0.218451(18) 0.495285(16) 0.01436(8) Uani 1 1 d . . . Mo2B Mo 0.38219(2) -0.345775(18) 0.399149(16) 0.01378(8) Uani 1 1 d . . . P1B P 0.36182(7) -0.22123(5) 0.36783(5) 0.0158(2) Uani 1 1 d . . . N1B N 0.4895(2) -0.22433(18) 0.49993(15) 0.0182(7) Uani 1 1 d . . . N2B N 0.5013(2) -0.34068(17) 0.39216(15) 0.0176(7) Uani 1 1 d . . . O1B O 0.57110(19) -0.22522(17) 0.50963(15) 0.0302(7) Uani 1 1 d . . . O2B O 0.58031(18) -0.35024(16) 0.37895(14) 0.0255(7) Uani 1 1 d . . . C1B C 0.3510(3) -0.3268(2) 0.51867(18) 0.0162(9) Uani 1 1 d . . . C2B C 0.4228(3) -0.3775(2) 0.52441(19) 0.0185(9) Uani 1 1 d . . . C3B C 0.4098(3) -0.4463(2) 0.55010(19) 0.0224(10) Uani 1 1 d . . . H3B H 0.4585 -0.4774 0.5529 0.027 Uiso 1 1 calc R . . C4B C 0.3277(3) -0.4675(2) 0.5706(2) 0.0229(10) Uani 1 1 d . . . H4B H 0.3202 -0.5123 0.5891 0.027 Uiso 1 1 calc R . . C5B C 0.2529(3) -0.4204(2) 0.56359(19) 0.0223(9) Uani 1 1 d . . . H5B H 0.1961 -0.4346 0.5772 0.027 Uiso 1 1 calc R . . C6B C 0.2641(3) -0.3545(2) 0.53700(19) 0.0190(9) Uani 1 1 d . . . H6B H 0.2132 -0.3259 0.5303 0.023 Uiso 1 1 calc R . . C7B C 0.3656(3) -0.1493(2) 0.59811(19) 0.0226(9) Uani 1 1 d . . . H7B H 0.4162 -0.1491 0.6297 0.027 Uiso 1 1 calc R . . C8B C 0.3500(3) -0.1032(2) 0.5404(2) 0.0248(10) Uani 1 1 d . . . H8B H 0.3888 -0.0677 0.5268 0.03 Uiso 1 1 calc R . . C9B C 0.2653(3) -0.1203(2) 0.5070(2) 0.0221(9) Uani 1 1 d . . . H9B H 0.238 -0.0975 0.4678 0.027 Uiso 1 1 calc R . . C10B C 0.2287(3) -0.1778(2) 0.5429(2) 0.0199(9) Uani 1 1 d . . . H10B H 0.1737 -0.2 0.5315 0.024 Uiso 1 1 calc R . . C11B C 0.2918(3) -0.1956(2) 0.59988(19) 0.0220(9) Uani 1 1 d . . . H11B H 0.2851 -0.2316 0.6325 0.026 Uiso 1 1 calc R . . C12B C 0.2802(3) -0.3737(2) 0.3015(2) 0.0217(9) Uani 1 1 d . . . H12B H 0.2506 -0.3389 0.2745 0.026 Uiso 1 1 calc R . . C13B C 0.2467(3) -0.4068(2) 0.3614(2) 0.0242(10) Uani 1 1 d . . . H13B H 0.191 -0.3982 0.3807 0.029 Uiso 1 1 calc R . . C14B C 0.3132(3) -0.4555(2) 0.3870(2) 0.0273(11) Uani 1 1 d . . . H14B H 0.3095 -0.4841 0.4266 0.033 Uiso 1 1 calc R . . C15B C 0.3858(3) -0.4529(2) 0.3419(2) 0.0275(10) Uani 1 1 d . . . H15B H 0.4381 -0.4802 0.3458 0.033 Uiso 1 1 calc R . . C16B C 0.3653(3) -0.4018(2) 0.2897(2) 0.0226(9) Uani 1 1 d . . . H16B H 0.4022 -0.389 0.2534 0.027 Uiso 1 1 calc R . . C17B C 0.2557(3) -0.1966(2) 0.31526(19) 0.0165(8) Uani 1 1 d . . . H17B H 0.2567 -0.2221 0.2703 0.02 Uiso 1 1 calc R . . C18B C 0.1708(3) -0.2213(2) 0.35143(19) 0.0177(9) Uani 1 1 d . . . H18C H 0.1658 -0.196 0.3956 0.021 Uiso 1 1 calc R . . H18D H 0.1762 -0.2709 0.3623 0.021 Uiso 1 1 calc R . . C19B C 0.0850(3) -0.2088(2) 0.3036(2) 0.0203(9) Uani 1 1 d . . . H19C H 0.088 -0.2368 0.2609 0.024 Uiso 1 1 calc R . . H19D H 0.0321 -0.2235 0.3281 0.024 Uiso 1 1 calc R . . C20B C 0.0755(3) -0.1313(2) 0.2835(2) 0.0236(10) Uani 1 1 d . . . H20C H 0.0236 -0.1254 0.2503 0.028 Uiso 1 1 calc R . . H20D H 0.0647 -0.104 0.3256 0.028 Uiso 1 1 calc R . . C21B C 0.1602(3) -0.1040(2) 0.2502(2) 0.0247(10) Uani 1 1 d . . . H21C H 0.1543 -0.0538 0.2427 0.03 Uiso 1 1 calc R . . H21D H 0.1655 -0.1261 0.2044 0.03 Uiso 1 1 calc R . . C22B C 0.2466(3) -0.1185(2) 0.2964(2) 0.0236(10) Uani 1 1 d . . . H22C H 0.2454 -0.0911 0.3397 0.028 Uiso 1 1 calc R . . H22D H 0.2991 -0.1038 0.2713 0.028 Uiso 1 1 calc R . . C23B C 0.4590(3) -0.1904(2) 0.3170(2) 0.0214(9) Uani 1 1 d . . . H23B H 0.5115 -0.2175 0.3356 0.026 Uiso 1 1 calc R . . C24B C 0.4466(3) -0.2111(2) 0.23889(19) 0.0182(9) Uani 1 1 d . . . H24C H 0.392 -0.1892 0.2183 0.022 Uiso 1 1 calc R . . H24D H 0.4392 -0.2616 0.2352 0.022 Uiso 1 1 calc R . . C25B C 0.5285(3) -0.1882(2) 0.1975(2) 0.0266(10) Uani 1 1 d . . . H25C H 0.5816 -0.2147 0.2142 0.032 Uiso 1 1 calc R . . H25D H 0.5167 -0.1988 0.1476 0.032 Uiso 1 1 calc R . . C26B C 0.5473(3) -0.1118(2) 0.2059(2) 0.0289(11) Uani 1 1 d . . . H26C H 0.4962 -0.0851 0.1858 0.035 Uiso 1 1 calc R . . H26D H 0.6003 -0.0995 0.1803 0.035 Uiso 1 1 calc R . . C27B C 0.5638(3) -0.0923(2) 0.2840(2) 0.0197(9) Uani 1 1 d . . . H27C H 0.6189 -0.1151 0.3026 0.024 Uiso 1 1 calc R . . H27D H 0.5726 -0.042 0.2881 0.024 Uiso 1 1 calc R . . C28B C 0.4851(3) -0.1142(2) 0.3281(2) 0.0249(10) Uani 1 1 d . . . H28C H 0.5019 -0.1066 0.3779 0.03 Uiso 1 1 calc R . . H28D H 0.433 -0.0848 0.3157 0.03 Uiso 1 1 calc R . . H2B H 0.483(3) -0.364(2) 0.5235(19) 0.014(10) Uiso 1 1 d . . . H2 H -0.030(3) 0.299(2) 0.529(2) 0.018(11) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.01439(17) 0.01302(17) 0.00854(15) 0.00084(13) 0.00067(12) -0.00213(14) Mo2 0.01356(17) 0.01039(17) 0.01048(16) 0.00032(13) 0.00159(12) -0.00055(13) P1 0.0109(5) 0.0108(5) 0.0101(4) 0.0004(4) -0.0003(4) -0.0011(4) N1 0.0156(18) 0.0176(18) 0.0079(15) 0.0029(13) 0.0035(13) 0.0022(14) N2 0.0174(18) 0.0138(17) 0.0147(16) 0.0000(13) 0.0018(14) 0.0022(14) O1 0.0156(15) 0.0270(17) 0.0190(14) 0.0001(12) 0.0031(11) -0.0055(13) O2 0.0168(16) 0.0300(18) 0.0257(16) 0.0013(13) -0.0051(12) 0.0052(13) C1 0.021(2) 0.017(2) 0.0110(18) -0.0013(16) 0.0067(16) -0.0031(17) C2 0.022(2) 0.023(2) 0.017(2) 0.0019(17) 0.0088(17) -0.0041(19) C3 0.023(2) 0.032(3) 0.025(2) 0.0019(19) 0.0122(19) 0.007(2) C4 0.040(3) 0.014(2) 0.031(2) -0.0045(19) 0.020(2) 0.001(2) C5 0.041(3) 0.017(2) 0.017(2) -0.0039(17) 0.0135(19) -0.008(2) C6 0.029(2) 0.021(2) 0.0084(18) 0.0019(16) 0.0048(16) -0.0042(19) C7 0.016(2) 0.028(2) 0.0139(19) 0.0071(17) -0.0053(16) 0.0022(18) C8 0.017(2) 0.017(2) 0.018(2) 0.0027(16) -0.0045(16) -0.0011(17) C9 0.023(2) 0.023(2) 0.0108(19) 0.0046(16) -0.0024(16) -0.0061(18) C10 0.026(2) 0.020(2) 0.0086(18) -0.0026(16) -0.0071(16) -0.0015(18) C11 0.022(2) 0.020(2) 0.0150(19) 0.0083(17) -0.0055(16) -0.0045(18) C12 0.016(2) 0.015(2) 0.024(2) 0.0030(17) 0.0091(17) -0.0027(17) C13 0.029(2) 0.020(2) 0.0112(19) 0.0028(16) 0.0064(17) -0.0072(19) C14 0.025(2) 0.013(2) 0.020(2) 0.0070(17) 0.0021(17) -0.0050(18) C15 0.028(2) 0.012(2) 0.021(2) -0.0004(16) 0.0104(18) -0.0028(18) C16 0.022(2) 0.016(2) 0.018(2) 0.0009(16) 0.0045(17) -0.0108(18) C17 0.0135(19) 0.016(2) 0.0088(17) -0.0011(15) 0.0000(15) 0.0002(16) C18 0.018(2) 0.020(2) 0.0114(18) 0.0004(16) 0.0027(15) -0.0003(17) C19 0.026(2) 0.023(2) 0.019(2) -0.0014(17) 0.0104(18) -0.0010(19) C20 0.021(2) 0.026(2) 0.029(2) -0.0020(19) 0.0099(19) 0.0015(19) C21 0.022(2) 0.012(2) 0.031(2) -0.0018(17) 0.0058(18) 0.0039(17) C22 0.021(2) 0.013(2) 0.017(2) 0.0000(16) 0.0035(16) 0.0017(17) C23 0.0107(19) 0.0115(19) 0.0145(18) -0.0004(15) -0.0016(15) -0.0013(15) C24 0.020(2) 0.014(2) 0.0149(19) -0.0012(16) -0.0005(16) -0.0004(17) C25 0.018(2) 0.023(2) 0.021(2) -0.0021(18) -0.0077(17) -0.0024(18) C26 0.023(2) 0.017(2) 0.031(2) -0.0045(18) -0.0110(19) -0.0001(18) C27 0.020(2) 0.013(2) 0.029(2) 0.0006(17) -0.0006(18) -0.0033(17) C28 0.015(2) 0.015(2) 0.020(2) -0.0027(16) -0.0001(16) -0.0009(16) Mo1B 0.01645(18) 0.01704(18) 0.00961(16) -0.00047(13) 0.00103(13) -0.00390(14) Mo2B 0.01302(17) 0.01855(18) 0.00981(16) -0.00077(13) 0.00087(12) -0.00273(14) P1B 0.0189(5) 0.0176(5) 0.0110(5) 0.0003(4) 0.0015(4) -0.0055(4) N1B 0.0206(19) 0.026(2) 0.0078(15) -0.0015(14) 0.0014(13) -0.0089(16) N2B 0.0190(19) 0.0233(19) 0.0106(16) -0.0002(14) 0.0017(13) -0.0034(15) O1B 0.0183(17) 0.047(2) 0.0245(16) -0.0013(14) -0.0017(13) -0.0084(15) O2B 0.0129(15) 0.0385(19) 0.0259(16) -0.0036(14) 0.0070(12) -0.0023(13) C1B 0.024(2) 0.020(2) 0.0052(17) -0.0012(15) 0.0000(15) -0.0058(18) C2B 0.019(2) 0.028(2) 0.0086(18) -0.0036(16) -0.0044(16) -0.0046(19) C3B 0.036(3) 0.020(2) 0.0103(19) -0.0017(17) -0.0059(18) 0.007(2) C4B 0.037(3) 0.015(2) 0.016(2) 0.0007(17) -0.0003(18) -0.007(2) C5B 0.027(2) 0.026(2) 0.015(2) -0.0012(17) 0.0101(17) -0.0080(19) C6B 0.018(2) 0.022(2) 0.017(2) -0.0028(17) 0.0005(16) -0.0037(18) C7B 0.026(2) 0.030(2) 0.0117(19) -0.0107(18) -0.0005(17) 0.002(2) C8B 0.036(3) 0.018(2) 0.021(2) -0.0061(18) 0.0046(19) -0.008(2) C9B 0.032(3) 0.021(2) 0.014(2) 0.0013(17) 0.0015(18) 0.0049(19) C10B 0.021(2) 0.018(2) 0.020(2) -0.0045(17) -0.0006(17) 0.0032(18) C11B 0.030(2) 0.026(2) 0.0102(19) -0.0034(17) 0.0047(17) 0.005(2) C12B 0.028(2) 0.016(2) 0.020(2) -0.0035(17) -0.0096(18) -0.0025(18) C13B 0.022(2) 0.029(3) 0.023(2) -0.0107(19) 0.0048(18) -0.011(2) C14B 0.044(3) 0.019(2) 0.018(2) 0.0013(18) -0.006(2) -0.015(2) C15B 0.030(3) 0.022(2) 0.029(2) -0.0136(19) -0.012(2) 0.008(2) C16B 0.026(2) 0.031(3) 0.0116(19) -0.0067(18) 0.0057(17) -0.004(2) C17B 0.021(2) 0.018(2) 0.0102(18) -0.0005(16) -0.0032(15) -0.0023(17) C18B 0.025(2) 0.012(2) 0.016(2) -0.0013(16) 0.0016(17) -0.0003(17) C19B 0.022(2) 0.021(2) 0.018(2) 0.0001(17) 0.0043(17) 0.0034(18) C20B 0.030(2) 0.023(2) 0.018(2) -0.0030(17) -0.0025(18) 0.0086(19) C21B 0.033(3) 0.023(2) 0.017(2) 0.0026(18) -0.0051(18) 0.002(2) C22B 0.031(3) 0.022(2) 0.018(2) 0.0049(17) -0.0023(18) -0.0024(19) C23B 0.023(2) 0.024(2) 0.018(2) 0.0000(17) 0.0053(17) -0.0047(19) C24B 0.019(2) 0.022(2) 0.0135(19) -0.0001(16) 0.0005(16) -0.0006(18) C25B 0.030(3) 0.033(3) 0.018(2) 0.0026(19) 0.0092(18) -0.002(2) C26B 0.024(2) 0.036(3) 0.027(2) 0.004(2) 0.0103(19) -0.003(2) C27B 0.016(2) 0.016(2) 0.027(2) 0.0043(17) 0.0006(17) -0.0041(17) C28B 0.024(2) 0.031(3) 0.021(2) -0.0072(19) 0.0041(18) -0.008(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 N1 1.773(3) . ? Mo1 C1 2.150(4) . ? Mo1 C9 2.351(4) . ? Mo1 C10 2.353(3) . ? Mo1 C8 2.374(4) . ? Mo1 C11 2.387(4) . ? Mo1 P1 2.3947(10) . ? Mo1 C7 2.396(4) . ? Mo1 Mo2 2.9753(5) . ? Mo2 N2 1.780(3) . ? Mo2 C14 2.329(4) . ? Mo2 C15 2.338(4) . ? Mo2 C13 2.339(4) . ? Mo2 C1 2.372(4) . ? Mo2 C12 2.396(4) . ? Mo2 C16 2.397(4) . ? Mo2 P1 2.4410(10) . ? Mo2 C2 2.514(4) . ? P1 C23 1.843(4) . ? P1 C17 1.853(4) . ? N1 O1 1.220(4) . ? N2 O2 1.207(4) . ? C1 C2 1.423(6) . ? C1 C6 1.442(5) . ? C2 C3 1.424(6) . ? C2 H2 0.91(4) . ? C3 C4 1.368(6) . ? C3 H3 0.93 . ? C4 C5 1.416(6) . ? C4 H4 0.93 . ? C5 C6 1.369(6) . ? C5 H5 0.93 . ? C6 H6 0.93 . ? C7 C11 1.404(6) . ? C7 C8 1.408(5) . ? C7 H7 0.93 . ? C8 C9 1.409(5) . ? C8 H8 0.93 . ? C9 C10 1.414(5) . ? C9 H9 0.93 . ? C10 C11 1.409(5) . ? C10 H10 0.93 . ? C11 H11 0.93 . ? C12 C16 1.395(5) . ? C12 C13 1.415(5) . ? C12 H12 0.93 . ? C13 C14 1.413(6) . ? C13 H13 0.93 . ? C14 C15 1.409(5) . ? C14 H14 0.93 . ? C15 C16 1.421(6) . ? C15 H15 0.93 . ? C16 H16 0.93 . ? C17 C22 1.536(5) . ? C17 C18 1.536(5) . ? C17 H17 0.98 . ? C18 C19 1.537(5) . ? C18 H18A 0.97 . ? C18 H18B 0.97 . ? C19 C20 1.512(6) . ? C19 H19A 0.97 . ? C19 H19B 0.97 . ? C20 C21 1.534(5) . ? C20 H20A 0.97 . ? C20 H20B 0.97 . ? C21 C22 1.523(5) . ? C21 H21A 0.97 . ? C21 H21B 0.97 . ? C22 H22A 0.97 . ? C22 H22B 0.97 . ? C23 C24 1.535(5) . ? C23 C28 1.536(5) . ? C23 H23 0.98 . ? C24 C25 1.524(5) . ? C24 H24A 0.97 . ? C24 H24B 0.97 . ? C25 C26 1.528(5) . ? C25 H25A 0.97 . ? C25 H25B 0.97 . ? C26 C27 1.526(5) . ? C26 H26A 0.97 . ? C26 H26B 0.97 . ? C27 C28 1.518(5) . ? C27 H27A 0.97 . ? C27 H27B 0.97 . ? C28 H28A 0.97 . ? C28 H28B 0.97 . ? Mo1B N1B 1.769(3) . ? Mo1B C1B 2.129(4) . ? Mo1B C7B 2.350(4) . ? Mo1B C8B 2.377(4) . ? Mo1B C11B 2.378(4) . ? Mo1B P1B 2.4055(10) . ? Mo1B C10B 2.435(4) . ? Mo1B C9B 2.438(4) . ? Mo1B Mo2B 3.0403(5) . ? Mo2B N2B 1.772(3) . ? Mo2B C15B 2.311(4) . ? Mo2B C16B 2.329(4) . ? Mo2B C14B 2.329(4) . ? Mo2B C1B 2.357(3) . ? Mo2B C12B 2.377(4) . ? Mo2B C13B 2.387(4) . ? Mo2B P1B 2.4580(11) . ? Mo2B C2B 2.485(4) . ? P1B C23B 1.862(4) . ? P1B C17B 1.868(4) . ? N1B O1B 1.208(4) . ? N2B O2B 1.218(4) . ? C1B C2B 1.433(6) . ? C1B C6B 1.445(5) . ? C2B C3B 1.412(6) . ? C2B H2B 0.92(4) . ? C3B C4B 1.354(6) . ? C3B H3B 0.93 . ? C4B C5B 1.422(6) . ? C4B H4B 0.93 . ? C5B C6B 1.365(6) . ? C5B H5B 0.93 . ? C6B H6B 0.93 . ? C7B C11B 1.402(6) . ? C7B C8B 1.410(6) . ? C7B H7B 0.93 . ? C8B C9B 1.408(6) . ? C8B H8B 0.93 . ? C9B C10B 1.410(6) . ? C9B H9B 0.93 . ? C10B C11B 1.426(5) . ? C10B H10B 0.93 . ? C11B H11B 0.93 . ? C12B C16B 1.393(6) . ? C12B C13B 1.408(6) . ? C12B H12B 0.93 . ? C13B C14B 1.416(6) . ? C13B H13B 0.93 . ? C14B C15B 1.404(6) . ? C14B H14B 0.93 . ? C15B C16B 1.407(6) . ? C15B H15B 0.93 . ? C16B H16B 0.93 . ? C17B C18B 1.532(5) . ? C17B C22B 1.532(5) . ? C17B H17B 0.98 . ? C18B C19B 1.533(5) . ? C18B H18C 0.97 . ? C18B H18D 0.97 . ? C19B C20B 1.527(5) . ? C19B H19C 0.97 . ? C19B H19D 0.97 . ? C20B C21B 1.520(6) . ? C20B H20C 0.97 . ? C20B H20D 0.97 . ? C21B C22B 1.531(5) . ? C21B H21C 0.97 . ? C21B H21D 0.97 . ? C22B H22C 0.97 . ? C22B H22D 0.97 . ? C23B C28B 1.514(6) . ? C23B C24B 1.529(5) . ? C23B H23B 0.98 . ? C24B C25B 1.537(5) . ? C24B H24C 0.97 . ? C24B H24D 0.97 . ? C25B C26B 1.489(6) . ? C25B H25C 0.97 . ? C25B H25D 0.97 . ? C26B C27B 1.528(6) . ? C26B H26C 0.97 . ? C26B H26D 0.97 . ? C27B C28B 1.522(5) . ? C27B H27C 0.97 . ? C27B H27D 0.97 . ? C28B H28C 0.97 . ? C28B H28D 0.97 . ? 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 C1 96.52(15) . . ? N1 Mo1 C9 97.66(14) . . ? C1 Mo1 C9 114.43(14) . . ? N1 Mo1 C10 122.97(13) . . ? C1 Mo1 C10 86.22(14) . . ? C9 Mo1 C10 34.99(13) . . ? N1 Mo1 C8 104.84(14) . . ? C1 Mo1 C8 143.77(14) . . ? C9 Mo1 C8 34.71(13) . . ? C10 Mo1 C8 57.62(14) . . ? N1 Mo1 C11 155.25(13) . . ? C1 Mo1 C11 92.28(14) . . ? C9 Mo1 C11 57.74(13) . . ? C10 Mo1 C11 34.56(13) . . ? C8 Mo1 C11 57.26(13) . . ? N1 Mo1 P1 88.71(9) . . ? C1 Mo1 P1 104.78(10) . . ? C9 Mo1 P1 139.11(10) . . ? C10 Mo1 P1 145.53(10) . . ? C8 Mo1 P1 104.63(10) . . ? C11 Mo1 P1 111.35(10) . . ? N1 Mo1 C7 136.95(14) . . ? C1 Mo1 C7 124.91(14) . . ? C9 Mo1 C7 57.40(14) . . ? C10 Mo1 C7 57.15(14) . . ? C8 Mo1 C7 34.34(13) . . ? C11 Mo1 C7 34.14(13) . . ? P1 Mo1 C7 91.07(9) . . ? N1 Mo1 Mo2 97.39(9) . . ? C1 Mo1 Mo2 52.17(9) . . ? C9 Mo1 Mo2 161.02(10) . . ? C10 Mo1 Mo2 126.04(10) . . ? C8 Mo1 Mo2 148.12(9) . . ? C11 Mo1 Mo2 106.23(9) . . ? P1 Mo1 Mo2 52.74(2) . . ? C7 Mo1 Mo2 116.23(9) . . ? N2 Mo2 C14 95.57(14) . . ? N2 Mo2 C15 120.14(14) . . ? C14 Mo2 C15 35.13(13) . . ? N2 Mo2 C13 104.12(14) . . ? C14 Mo2 C13 35.24(14) . . ? C15 Mo2 C13 58.43(14) . . ? N2 Mo2 C1 105.66(14) . . ? C14 Mo2 C1 125.21(13) . . ? C15 Mo2 C1 92.39(13) . . ? C13 Mo2 C1 146.15(14) . . ? N2 Mo2 C12 137.43(13) . . ? C14 Mo2 C12 57.74(14) . . ? C15 Mo2 C12 57.48(14) . . ? C13 Mo2 C12 34.75(13) . . ? C1 Mo2 C12 116.79(13) . . ? N2 Mo2 C16 153.09(14) . . ? C14 Mo2 C16 57.87(14) . . ? C15 Mo2 C16 34.90(14) . . ? C13 Mo2 C16 57.59(13) . . ? C1 Mo2 C16 88.77(13) . . ? C12 Mo2 C16 33.85(13) . . ? N2 Mo2 P1 88.52(10) . . ? C14 Mo2 P1 134.16(10) . . ? C15 Mo2 P1 146.10(11) . . ? C13 Mo2 P1 99.57(10) . . ? C1 Mo2 P1 96.92(10) . . ? C12 Mo2 P1 89.47(10) . . ? C16 Mo2 P1 112.60(10) . . ? N2 Mo2 C2 76.42(14) . . ? C14 Mo2 C2 112.67(14) . . ? C15 Mo2 C2 92.84(14) . . ? C13 Mo2 C2 147.76(14) . . ? C1 Mo2 C2 33.72(13) . . ? C12 Mo2 C2 141.76(14) . . ? C16 Mo2 C2 108.08(14) . . ? P1 Mo2 C2 112.65(10) . . ? N2 Mo2 Mo1 103.79(10) . . ? C14 Mo2 Mo1 160.29(10) . . ? C15 Mo2 Mo1 127.21(10) . . ? C13 Mo2 Mo1 138.48(10) . . ? C1 Mo2 Mo1 45.71(10) . . ? C12 Mo2 Mo1 107.78(9) . . ? C16 Mo2 Mo1 102.51(10) . . ? P1 Mo2 Mo1 51.33(2) . . ? C2 Mo2 Mo1 69.29(10) . . ? C23 P1 C17 110.13(17) . . ? C23 P1 Mo1 114.18(12) . . ? C17 P1 Mo1 118.81(11) . . ? C23 P1 Mo2 112.32(12) . . ? C17 P1 Mo2 121.85(13) . . ? Mo1 P1 Mo2 75.94(3) . . ? O1 N1 Mo1 173.7(3) . . ? O2 N2 Mo2 176.2(3) . . ? C2 C1 C6 113.7(4) . . ? C2 C1 Mo1 121.9(3) . . ? C6 C1 Mo1 124.3(3) . . ? C2 C1 Mo2 78.6(2) . . ? C6 C1 Mo2 113.3(2) . . ? Mo1 C1 Mo2 82.12(12) . . ? C1 C2 C3 122.5(4) . . ? C1 C2 Mo2 67.7(2) . . ? C3 C2 Mo2 119.6(3) . . ? C1 C2 H2 123(3) . . ? C3 C2 H2 113(3) . . ? Mo2 C2 H2 98(2) . . ? C4 C3 C2 120.8(4) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 118.7(4) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? C6 C5 C4 120.6(4) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C5 C6 C1 123.6(4) . . ? C5 C6 H6 118.2 . . ? C1 C6 H6 118.2 . . ? C11 C7 C8 108.4(4) . . ? C11 C7 Mo1 72.6(2) . . ? C8 C7 Mo1 72.0(2) . . ? C11 C7 H7 125.8 . . ? C8 C7 H7 125.8 . . ? Mo1 C7 H7 121.4 . . ? C7 C8 C9 108.0(4) . . ? C7 C8 Mo1 73.7(2) . . ? C9 C8 Mo1 71.8(2) . . ? C7 C8 H8 126 . . ? C9 C8 H8 126 . . ? Mo1 C8 H8 120.3 . . ? C8 C9 C10 107.5(4) . . ? C8 C9 Mo1 73.5(2) . . ? C10 C9 Mo1 72.6(2) . . ? C8 C9 H9 126.2 . . ? C10 C9 H9 126.2 . . ? Mo1 C9 H9 119.6 . . ? C11 C10 C9 108.3(4) . . ? C11 C10 Mo1 74.1(2) . . ? C9 C10 Mo1 72.4(2) . . ? C11 C10 H10 125.8 . . ? C9 C10 H10 125.9 . . ? Mo1 C10 H10 119.5 . . ? C7 C11 C10 107.7(4) . . ? C7 C11 Mo1 73.3(2) . . ? C10 C11 Mo1 71.4(2) . . ? C7 C11 H11 126.1 . . ? C10 C11 H11 126.1 . . ? Mo1 C11 H11 121 . . ? C16 C12 C13 108.6(4) . . ? C16 C12 Mo2 73.1(2) . . ? C13 C12 Mo2 70.4(2) . . ? C16 C12 H12 125.7 . . ? C13 C12 H12 125.7 . . ? Mo2 C12 H12 122.4 . . ? C14 C13 C12 107.6(3) . . ? C14 C13 Mo2 72.0(2) . . ? C12 C13 Mo2 74.8(2) . . ? C14 C13 H13 126.2 . . ? C12 C13 H13 126.2 . . ? Mo2 C13 H13 118.9 . . ? C15 C14 C13 108.0(4) . . ? C15 C14 Mo2 72.8(2) . . ? C13 C14 Mo2 72.7(2) . . ? C15 C14 H14 126 . . ? C13 C14 H14 126 . . ? Mo2 C14 H14 120.3 . . ? C14 C15 C16 107.9(3) . . ? C14 C15 Mo2 72.1(2) . . ? C16 C15 Mo2 74.8(2) . . ? C14 C15 H15 126.1 . . ? C16 C15 H15 126.1 . . ? Mo2 C15 H15 118.9 . . ? C12 C16 C15 107.9(3) . . ? C12 C16 Mo2 73.0(2) . . ? C15 C16 Mo2 70.3(2) . . ? C12 C16 H16 126 . . ? C15 C16 H16 126 . . ? Mo2 C16 H16 122.3 . . ? C22 C17 C18 108.7(3) . . ? C22 C17 P1 113.6(3) . . ? C18 C17 P1 117.2(3) . . ? C22 C17 H17 105.5 . . ? C18 C17 H17 105.5 . . ? P1 C17 H17 105.5 . . ? C17 C18 C19 110.3(3) . . ? C17 C18 H18A 109.6 . . ? C19 C18 H18A 109.6 . . ? C17 C18 H18B 109.6 . . ? C19 C18 H18B 109.6 . . ? H18A C18 H18B 108.1 . . ? C20 C19 C18 111.8(3) . . ? C20 C19 H19A 109.3 . . ? C18 C19 H19A 109.3 . . ? C20 C19 H19B 109.3 . . ? C18 C19 H19B 109.3 . . ? H19A C19 H19B 107.9 . . ? C19 C20 C21 111.0(3) . . ? C19 C20 H20A 109.4 . . ? C21 C20 H20A 109.4 . . ? C19 C20 H20B 109.4 . . ? C21 C20 H20B 109.4 . . ? H20A C20 H20B 108 . . ? C22 C21 C20 110.2(3) . . ? C22 C21 H21A 109.6 . . ? C20 C21 H21A 109.6 . . ? C22 C21 H21B 109.6 . . ? C20 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? C21 C22 C17 111.1(3) . . ? C21 C22 H22A 109.4 . . ? C17 C22 H22A 109.4 . . ? C21 C22 H22B 109.4 . . ? C17 C22 H22B 109.4 . . ? H22A C22 H22B 108 . . ? C24 C23 C28 109.6(3) . . ? C24 C23 P1 116.5(3) . . ? C28 C23 P1 116.2(2) . . ? C24 C23 H23 104.3 . . ? C28 C23 H23 104.3 . . ? P1 C23 H23 104.3 . . ? C25 C24 C23 110.3(3) . . ? C25 C24 H24A 109.6 . . ? C23 C24 H24A 109.6 . . ? C25 C24 H24B 109.6 . . ? C23 C24 H24B 109.6 . . ? H24A C24 H24B 108.1 . . ? C24 C25 C26 111.1(3) . . ? C24 C25 H25A 109.4 . . ? C26 C25 H25A 109.4 . . ? C24 C25 H25B 109.4 . . ? C26 C25 H25B 109.4 . . ? H25A C25 H25B 108 . . ? C27 C26 C25 111.7(3) . . ? C27 C26 H26A 109.3 . . ? C25 C26 H26A 109.3 . . ? C27 C26 H26B 109.3 . . ? C25 C26 H26B 109.3 . . ? H26A C26 H26B 107.9 . . ? C28 C27 C26 111.4(3) . . ? C28 C27 H27A 109.4 . . ? C26 C27 H27A 109.4 . . ? C28 C27 H27B 109.4 . . ? C26 C27 H27B 109.4 . . ? H27A C27 H27B 108 . . ? C27 C28 C23 110.1(3) . . ? C27 C28 H28A 109.6 . . ? C23 C28 H28A 109.6 . . ? C27 C28 H28B 109.6 . . ? C23 C28 H28B 109.6 . . ? H28A C28 H28B 108.2 . . ? N1B Mo1B C1B 93.90(15) . . ? N1B Mo1B C7B 93.68(14) . . ? C1B Mo1B C7B 111.17(14) . . ? N1B Mo1B C8B 100.43(15) . . ? C1B Mo1B C8B 143.12(14) . . ? C7B Mo1B C8B 34.71(14) . . ? N1B Mo1B C11B 119.75(14) . . ? C1B Mo1B C11B 86.03(14) . . ? C7B Mo1B C11B 34.50(14) . . ? C8B Mo1B C11B 57.34(15) . . ? N1B Mo1B P1B 92.46(10) . . ? C1B Mo1B P1B 100.76(9) . . ? C7B Mo1B P1B 146.94(11) . . ? C8B Mo1B P1B 112.26(10) . . ? C11B Mo1B P1B 146.76(10) . . ? N1B Mo1B C10B 150.75(14) . . ? C1B Mo1B C10B 96.26(14) . . ? C7B Mo1B C10B 57.08(14) . . ? C8B Mo1B C10B 56.74(14) . . ? C11B Mo1B C10B 34.44(13) . . ? P1B Mo1B C10B 112.35(9) . . ? N1B Mo1B C9B 132.70(15) . . ? C1B Mo1B C9B 129.34(15) . . ? C7B Mo1B C9B 56.77(14) . . ? C8B Mo1B C9B 33.98(14) . . ? C11B Mo1B C9B 56.61(13) . . ? P1B Mo1B C9B 96.35(9) . . ? C10B Mo1B C9B 33.63(13) . . ? N1B Mo1B Mo2B 83.50(10) . . ? C1B Mo1B Mo2B 50.57(9) . . ? C7B Mo1B Mo2B 160.97(11) . . ? C8B Mo1B Mo2B 164.24(10) . . ? C11B Mo1B Mo2B 133.58(11) . . ? P1B Mo1B Mo2B 52.09(3) . . ? C10B Mo1B Mo2B 123.67(10) . . ? C9B Mo1B Mo2B 136.36(10) . . ? N2B Mo2B C15B 88.05(15) . . ? N2B Mo2B C16B 91.06(14) . . ? C15B Mo2B C16B 35.30(14) . . ? N2B Mo2B C14B 118.12(16) . . ? C15B Mo2B C14B 35.21(15) . . ? C16B Mo2B C14B 58.41(14) . . ? N2B Mo2B C1B 107.93(13) . . ? C15B Mo2B C1B 126.50(15) . . ? C16B Mo2B C1B 154.75(14) . . ? C14B Mo2B C1B 97.23(14) . . ? N2B Mo2B C12B 122.91(14) . . ? C15B Mo2B C12B 57.91(14) . . ? C16B Mo2B C12B 34.42(14) . . ? C14B Mo2B C12B 57.88(14) . . ? C1B Mo2B C12B 129.07(14) . . ? N2B Mo2B C13B 145.29(15) . . ? C15B Mo2B C13B 58.01(15) . . ? C16B Mo2B C13B 57.56(14) . . ? C14B Mo2B C13B 34.92(15) . . ? C1B Mo2B C13B 99.10(13) . . ? C12B Mo2B C13B 34.37(14) . . ? N2B Mo2B P1B 92.20(11) . . ? C15B Mo2B P1B 138.09(11) . . ? C16B Mo2B P1B 102.83(11) . . ? C14B Mo2B P1B 142.56(11) . . ? C1B Mo2B P1B 93.15(10) . . ? C12B Mo2B P1B 87.96(10) . . ? C13B Mo2B P1B 107.92(11) . . ? N2B Mo2B C2B 83.96(14) . . ? C15B Mo2B C2B 102.76(14) . . ? C16B Mo2B C2B 138.04(14) . . ? C14B Mo2B C2B 87.57(14) . . ? C1B Mo2B C2B 34.30(13) . . ? C12B Mo2B C2B 142.67(14) . . ? C13B Mo2B C2B 108.76(14) . . ? P1B Mo2B C2B 118.95(10) . . ? N2B Mo2B Mo1B 95.34(10) . . ? C15B Mo2B Mo1B 170.75(11) . . ? C16B Mo2B Mo1B 152.72(11) . . ? C14B Mo2B Mo1B 137.19(11) . . ? C1B Mo2B Mo1B 44.25(9) . . ? C12B Mo2B Mo1B 125.85(10) . . ? C13B Mo2B Mo1B 119.32(10) . . ? P1B Mo2B Mo1B 50.54(2) . . ? C2B Mo2B Mo1B 69.15(10) . . ? C23B P1B C17B 107.03(18) . . ? C23B P1B Mo1B 120.82(13) . . ? C17B P1B Mo1B 121.39(13) . . ? C23B P1B Mo2B 109.88(14) . . ? C17B P1B Mo2B 117.29(13) . . ? Mo1B P1B Mo2B 77.37(3) . . ? O1B N1B Mo1B 173.5(3) . . ? O2B N2B Mo2B 166.0(3) . . ? C2B C1B C6B 113.4(4) . . ? C2B C1B Mo1B 124.5(3) . . ? C6B C1B Mo1B 121.9(3) . . ? C2B C1B Mo2B 77.8(2) . . ? C6B C1B Mo2B 113.2(2) . . ? Mo1B C1B Mo2B 85.18(12) . . ? C3B C2B C1B 122.6(4) . . ? C3B C2B Mo2B 121.5(3) . . ? C1B C2B Mo2B 67.9(2) . . ? C3B C2B H2B 114(2) . . ? C1B C2B H2B 121(2) . . ? Mo2B C2B H2B 96(2) . . ? C4B C3B C2B 121.0(4) . . ? C4B C3B H3B 119.5 . . ? C2B C3B H3B 119.5 . . ? C3B C4B C5B 119.1(4) . . ? C3B C4B H4B 120.5 . . ? C5B C4B H4B 120.5 . . ? C6B C5B C4B 120.4(4) . . ? C6B C5B H5B 119.8 . . ? C4B C5B H5B 119.8 . . ? C5B C6B C1B 123.4(4) . . ? C5B C6B H6B 118.3 . . ? C1B C6B H6B 118.3 . . ? C11B C7B C8B 108.4(4) . . ? C11B C7B Mo1B 73.9(2) . . ? C8B C7B Mo1B 73.7(2) . . ? C11B C7B H7B 125.8 . . ? C8B C7B H7B 125.8 . . ? Mo1B C7B H7B 118.5 . . ? C9B C8B C7B 107.8(4) . . ? C9B C8B Mo1B 75.4(2) . . ? C7B C8B Mo1B 71.6(2) . . ? C9B C8B H8B 126.1 . . ? C7B C8B H8B 126.1 . . ? Mo1B C8B H8B 118.9 . . ? C8B C9B C10B 108.5(4) . . ? C8B C9B Mo1B 70.6(2) . . ? C10B C9B Mo1B 73.0(2) . . ? C8B C9B H9B 125.7 . . ? C10B C9B H9B 125.7 . . ? Mo1B C9B H9B 122.2 . . ? C9B C10B C11B 107.3(4) . . ? C9B C10B Mo1B 73.3(2) . . ? C11B C10B Mo1B 70.6(2) . . ? C9B C10B H10B 126.3 . . ? C11B C10B H10B 126.3 . . ? Mo1B C10B H10B 121.5 . . ? C7B C11B C10B 107.9(4) . . ? C7B C11B Mo1B 71.6(2) . . ? C10B C11B Mo1B 74.9(2) . . ? C7B C11B H11B 126 . . ? C10B C11B H11B 126 . . ? Mo1B C11B H11B 119.2 . . ? C16B C12B C13B 108.3(4) . . ? C16B C12B Mo2B 70.9(2) . . ? C13B C12B Mo2B 73.2(2) . . ? C16B C12B H12B 125.8 . . ? C13B C12B H12B 125.8 . . ? Mo2B C12B H12B 121.8 . . ? C12B C13B C14B 107.5(4) . . ? C12B C13B Mo2B 72.4(2) . . ? C14B C13B Mo2B 70.3(2) . . ? C12B C13B H13B 126.2 . . ? C14B C13B H13B 126.2 . . ? Mo2B C13B H13B 122.7 . . ? C15B C14B C13B 107.8(4) . . ? C15B C14B Mo2B 71.7(2) . . ? C13B C14B Mo2B 74.8(2) . . ? C15B C14B H14B 126.1 . . ? C13B C14B H14B 126.1 . . ? Mo2B C14B H14B 119.3 . . ? C14B C15B C16B 107.9(4) . . ? C14B C15B Mo2B 73.1(2) . . ? C16B C15B Mo2B 73.0(2) . . ? C14B C15B H15B 126 . . ? C16B C15B H15B 126 . . ? Mo2B C15B H15B 119.7 . . ? C12B C16B C15B 108.3(4) . . ? C12B C16B Mo2B 74.7(2) . . ? C15B C16B Mo2B 71.7(2) . . ? C12B C16B H16B 125.8 . . ? C15B C16B H16B 125.8 . . ? Mo2B C16B H16B 119.6 . . ? C18B C17B C22B 109.7(3) . . ? C18B C17B P1B 111.6(2) . . ? C22B C17B P1B 115.3(3) . . ? C18B C17B H17B 106.6 . . ? C22B C17B H17B 106.6 . . ? P1B C17B H17B 106.6 . . ? C17B C18B C19B 111.0(3) . . ? C17B C18B H18C 109.4 . . ? C19B C18B H18C 109.4 . . ? C17B C18B H18D 109.4 . . ? C19B C18B H18D 109.4 . . ? H18C C18B H18D 108 . . ? C20B C19B C18B 111.0(3) . . ? C20B C19B H19C 109.4 . . ? C18B C19B H19C 109.4 . . ? C20B C19B H19D 109.4 . . ? C18B C19B H19D 109.4 . . ? H19C C19B H19D 108 . . ? C21B C20B C19B 111.5(3) . . ? C21B C20B H20C 109.3 . . ? C19B C20B H20C 109.3 . . ? C21B C20B H20D 109.3 . . ? C19B C20B H20D 109.3 . . ? H20C C20B H20D 108 . . ? C20B C21B C22B 112.3(3) . . ? C20B C21B H21C 109.1 . . ? C22B C21B H21C 109.1 . . ? C20B C21B H21D 109.1 . . ? C22B C21B H21D 109.1 . . ? H21C C21B H21D 107.9 . . ? C21B C22B C17B 111.6(3) . . ? C21B C22B H22C 109.3 . . ? C17B C22B H22C 109.3 . . ? C21B C22B H22D 109.3 . . ? C17B C22B H22D 109.3 . . ? H22C C22B H22D 108 . . ? C28B C23B C24B 113.4(3) . . ? C28B C23B P1B 115.3(3) . . ? C24B C23B P1B 111.1(3) . . ? C28B C23B H23B 105.3 . . ? C24B C23B H23B 105.3 . . ? P1B C23B H23B 105.3 . . ? C23B C24B C25B 111.2(3) . . ? C23B C24B H24C 109.4 . . ? C25B C24B H24C 109.4 . . ? C23B C24B H24D 109.4 . . ? C25B C24B H24D 109.4 . . ? H24C C24B H24D 108 . . ? C26B C25B C24B 111.7(4) . . ? C26B C25B H25C 109.3 . . ? C24B C25B H25C 109.3 . . ? C26B C25B H25D 109.3 . . ? C24B C25B H25D 109.3 . . ? H25C C25B H25D 107.9 . . ? C25B C26B C27B 111.1(3) . . ? C25B C26B H26C 109.4 . . ? C27B C26B H26C 109.4 . . ? C25B C26B H26D 109.4 . . ? C27B C26B H26D 109.4 . . ? H26C C26B H26D 108 . . ? C28B C27B C26B 112.1(3) . . ? C28B C27B H27C 109.2 . . ? C26B C27B H27C 109.2 . . ? C28B C27B H27D 109.2 . . ? C26B C27B H27D 109.2 . . ? H27C C27B H27D 107.9 . . ? C23B C28B C27B 112.4(3) . . ? C23B C28B H28C 109.1 . . ? C27B C28B H28C 109.1 . . ? C23B C28B H28D 109.1 . . ? C27B C28B H28D 109.1 . . ? H28C C28B H28D 107.9 . . ?