# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_12036 #TrackingRef '13597_web_deposit_cif_file_0_DanielTofan_1346189895.MoP3_12036.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H60 Cl Mo N2 O11 P7' _chemical_formula_weight 1477.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 23.790(3) _cell_length_b 13.7091(15) _cell_length_c 22.003(2) _cell_angle_alpha 90.00 _cell_angle_beta 112.902(2) _cell_angle_gamma 90.00 _cell_volume 6610.1(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9632 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 30.79 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.485 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3032 _exptl_absorpt_coefficient_mu 0.473 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7980 _exptl_absorpt_correction_T_max 0.9543 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; 'Siemens three-circle diffractometer, Bruker APEX CCD' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 174550 _diffrn_reflns_av_R_equivalents 0.0742 _diffrn_reflns_av_sigmaI/netI 0.0394 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 29.57 _reflns_number_total 18472 _reflns_number_gt 14501 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2011.4.0 (Bruker-AXS, 2011)' _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2011)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0278P)^2^+6.2666P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18472 _refine_ls_number_parameters 884 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.0534 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0831 _refine_ls_wR_factor_gt 0.0738 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo -0.24546(3) 0.65607(2) 0.188997(18) 0.01302(8) Uani 0.949(3) 1 d P A 1 O1 O -0.1901(2) 0.5706(2) 0.2101(2) 0.0212(7) Uani 0.949(3) 1 d P A 1 O2 O -0.25017(10) 0.68215(19) 0.26214(10) 0.0203(5) Uani 0.949(3) 1 d P A 1 Cl1 Cl -0.32943(4) 0.54804(5) 0.15118(5) 0.02056(17) Uani 0.949(3) 1 d P A 1 Mo1A Mo -0.2712(8) 0.6573(5) 0.1758(5) 0.0306(19) Uani 0.051(3) 1 d PU A 2 O1A O -0.330(2) 0.577(3) 0.143(3) 0.026(7) Uani 0.051(3) 1 d PU A 2 O2A O -0.271(2) 0.680(4) 0.248(2) 0.020(6) Uani 0.051(3) 1 d PU A 2 Cl1A Cl -0.1897(18) 0.5453(17) 0.2072(15) 0.028(4) Uani 0.051(3) 1 d PU A 2 O10 O -0.24974(6) 0.65357(9) 0.08747(6) 0.0150(3) Uani 1 1 d U . . O20 O -0.31368(6) 0.76903(9) 0.14104(6) 0.0143(3) Uani 1 1 d U . . O30 O -0.18652(6) 0.76985(10) 0.19699(6) 0.0161(3) Uani 1 1 d U . . P2 P -0.31460(2) 0.85245(3) 0.09608(2) 0.01228(9) Uani 1 1 d . A . P3 P -0.18574(2) 0.85350(3) 0.15188(2) 0.01345(9) Uani 1 1 d . A . P11 P -0.35141(2) 0.17074(3) 0.22468(2) 0.01038(9) Uani 1 1 d . . . P22 P 0.14176(2) 0.87933(3) 0.50070(2) 0.01128(9) Uani 1 1 d . . . P12 P -0.42342(2) 0.32287(3) 0.26022(2) 0.01090(9) Uani 1 1 d . . . P1 P -0.24935(2) 0.73457(3) 0.04140(2) 0.01311(9) Uani 1 1 d . A . P21 P 0.08313(2) 0.69239(3) 0.51992(2) 0.01178(9) Uani 1 1 d . . . O12 O -0.30571(6) 0.80653(9) 0.03286(6) 0.0138(3) Uani 1 1 d . . . O23 O -0.24998(6) 0.90910(9) 0.13117(6) 0.0136(3) Uani 1 1 d . . . O13 O -0.19224(6) 0.80480(9) 0.08293(6) 0.0146(3) Uani 1 1 d . . . O33 O -0.13502(6) 0.92211(10) 0.17562(7) 0.0218(3) Uani 1 1 d . . . O11 O -0.24855(7) 0.71194(10) -0.02304(7) 0.0204(3) Uani 1 1 d . . . O22 O -0.36459(6) 0.92251(10) 0.07563(7) 0.0184(3) Uani 1 1 d . . . N1 N -0.36868(7) 0.25453(11) 0.26386(8) 0.0131(3) Uani 1 1 d . . . N2 N 0.12467(7) 0.78495(11) 0.53040(8) 0.0157(3) Uani 1 1 d . . . C131 C -0.40723(8) 0.14758(13) 0.14313(9) 0.0126(3) Uani 1 1 d . . . C262 C 0.23918(9) 0.76873(14) 0.50089(9) 0.0163(4) Uani 1 1 d . . . H262 H 0.2188 0.7148 0.5103 0.020 Uiso 1 1 calc R . . C121 C -0.33915(8) 0.05621(13) 0.26740(9) 0.0120(3) Uani 1 1 d . . . C211 C 0.03889(9) 0.70243(13) 0.56970(9) 0.0143(3) Uani 1 1 d . . . C123 C -0.33208(8) -0.11964(13) 0.26335(9) 0.0145(3) Uani 1 1 d . . . H123 H -0.3363 -0.1781 0.2387 0.017 Uiso 1 1 calc R . . C161 C -0.39451(8) 0.43548(13) 0.30248(9) 0.0124(3) Uani 1 1 d . . . C136 C -0.39344(9) 0.15687(14) 0.08756(9) 0.0157(4) Uani 1 1 d . . . H136 H -0.3533 0.1737 0.0921 0.019 Uiso 1 1 calc R . . C261 C 0.21396(8) 0.86206(13) 0.49390(9) 0.0125(3) Uani 1 1 d . . . C124 C -0.31152(8) -0.12318(14) 0.33169(9) 0.0144(3) Uani 1 1 d . . . H124 H -0.3016 -0.1842 0.3538 0.017 Uiso 1 1 calc R . . C116 C -0.26093(9) 0.29870(14) 0.22521(10) 0.0182(4) Uani 1 1 d . . . H116 H -0.2840 0.3477 0.2356 0.022 Uiso 1 1 calc R . . C145 C -0.57618(9) 0.35833(15) 0.09020(10) 0.0200(4) Uani 1 1 d . . . H145 H -0.6192 0.3526 0.0763 0.024 Uiso 1 1 calc R . . C221 C 0.03174(8) 0.67311(13) 0.43550(9) 0.0132(3) Uani 1 1 d . . . C222 C -0.03087(9) 0.66085(14) 0.41787(10) 0.0165(4) Uani 1 1 d . . . H222 H -0.0471 0.6593 0.4510 0.020 Uiso 1 1 calc R . . C142 C -0.45018(9) 0.37566(13) 0.13068(9) 0.0153(4) Uani 1 1 d . . . H142 H -0.4072 0.3818 0.1444 0.018 Uiso 1 1 calc R . . C141 C -0.47515(8) 0.35054(13) 0.17675(9) 0.0133(3) Uani 1 1 d . . . C162 C -0.39966(9) 0.52362(14) 0.26960(10) 0.0184(4) Uani 1 1 d . . . H162 H -0.4181 0.5256 0.2228 0.022 Uiso 1 1 calc R . . C166 C -0.36676(10) 0.43405(15) 0.37137(10) 0.0220(4) Uani 1 1 d . . . H166 H -0.3624 0.3739 0.3943 0.026 Uiso 1 1 calc R . . C241 C 0.14780(8) 0.97913(13) 0.55550(9) 0.0130(3) Uani 1 1 d . . . C122 C -0.34647(8) -0.03018(13) 0.23113(9) 0.0139(3) Uani 1 1 d . . . H122 H -0.3613 -0.0277 0.1843 0.017 Uiso 1 1 calc R . . C265 C 0.29943(9) 0.92721(15) 0.47420(10) 0.0193(4) Uani 1 1 d . . . H265 H 0.3202 0.9811 0.4654 0.023 Uiso 1 1 calc R . . C252 C 0.10422(9) 0.93003(14) 0.36694(9) 0.0167(4) Uani 1 1 d . . . H252 H 0.1461 0.9297 0.3735 0.020 Uiso 1 1 calc R . . C254 C -0.00134(9) 0.94762(15) 0.29446(10) 0.0211(4) Uani 1 1 d . . . H254 H -0.0316 0.9585 0.2516 0.025 Uiso 1 1 calc R . . C151 C -0.46613(8) 0.27078(13) 0.30445(9) 0.0130(3) Uani 1 1 d . . . C242 C 0.16467(8) 0.96033(14) 0.62286(9) 0.0159(4) Uani 1 1 d . . . H242 H 0.1710 0.8952 0.6388 0.019 Uiso 1 1 calc R . . C224 C -0.04598(10) 0.65374(15) 0.30335(10) 0.0210(4) Uani 1 1 d . . . H224 H -0.0726 0.6479 0.2583 0.025 Uiso 1 1 calc R . . C112 C -0.24724(9) 0.13056(14) 0.20095(10) 0.0173(4) Uani 1 1 d . . . H112 H -0.2613 0.0650 0.1945 0.021 Uiso 1 1 calc R . . C251 C 0.08736(8) 0.91266(13) 0.42011(9) 0.0135(3) Uani 1 1 d . . . C152 C -0.50742(9) 0.32790(14) 0.32014(9) 0.0164(4) Uani 1 1 d . . . H152 H -0.5143 0.3939 0.3061 0.020 Uiso 1 1 calc R . . C223 C -0.06947(9) 0.65086(15) 0.35190(10) 0.0203(4) Uani 1 1 d . . . H223 H -0.1120 0.6420 0.3401 0.024 Uiso 1 1 calc R . . C245 C 0.14580(9) 1.15142(14) 0.57663(11) 0.0212(4) Uani 1 1 d . . . H245 H 0.1393 1.2167 0.5610 0.025 Uiso 1 1 calc R . . C226 C 0.05545(9) 0.67453(14) 0.38633(10) 0.0176(4) Uani 1 1 d . . . H226 H 0.0981 0.6819 0.3981 0.021 Uiso 1 1 calc R . . C135 C -0.43851(9) 0.14142(15) 0.02536(10) 0.0203(4) Uani 1 1 d . . . H135 H -0.4291 0.1478 -0.0126 0.024 Uiso 1 1 calc R . . C111 C -0.28102(8) 0.20226(13) 0.21682(9) 0.0122(3) Uani 1 1 d . . . C264 C 0.32442(9) 0.83401(16) 0.48135(10) 0.0223(4) Uani 1 1 d . . . H264 H 0.3625 0.8244 0.4776 0.027 Uiso 1 1 calc R . . C146 C -0.53856(9) 0.34264(14) 0.15590(9) 0.0165(4) Uani 1 1 d . . . H146 H -0.5560 0.3265 0.1868 0.020 Uiso 1 1 calc R . . C113 C -0.19325(9) 0.15481(15) 0.19464(11) 0.0219(4) Uani 1 1 d . . . H113 H -0.1702 0.1060 0.1841 0.026 Uiso 1 1 calc R . . C266 C 0.24415(8) 0.94091(13) 0.47998(9) 0.0145(4) Uani 1 1 d . . . H266 H 0.2266 1.0042 0.4745 0.017 Uiso 1 1 calc R . . C125 C -0.30539(8) -0.03802(13) 0.36779(9) 0.0142(3) Uani 1 1 d . . . H125 H -0.2923 -0.0412 0.4144 0.017 Uiso 1 1 calc R . . C134 C -0.49697(9) 0.11688(15) 0.01834(10) 0.0198(4) Uani 1 1 d . . . H134 H -0.5277 0.1067 -0.0244 0.024 Uiso 1 1 calc R . . C156 C -0.45537(9) 0.17470(14) 0.32620(10) 0.0170(4) Uani 1 1 d . . . H156 H -0.4274 0.1358 0.3157 0.020 Uiso 1 1 calc R . . C212 C 0.01858(9) 0.61914(14) 0.59161(10) 0.0185(4) Uani 1 1 d . . . H212 H 0.0288 0.5563 0.5808 0.022 Uiso 1 1 calc R . . C115 C -0.20672(10) 0.32294(15) 0.21819(11) 0.0239(4) Uani 1 1 d . . . H115 H -0.1931 0.3887 0.2233 0.029 Uiso 1 1 calc R . . C144 C -0.55094(10) 0.38238(15) 0.04485(10) 0.0209(4) Uani 1 1 d . . . H144 H -0.5767 0.3926 -0.0001 0.025 Uiso 1 1 calc R . . C143 C -0.48796(9) 0.39157(14) 0.06517(10) 0.0187(4) Uani 1 1 d . . . H143 H -0.4709 0.4087 0.0342 0.022 Uiso 1 1 calc R . . C216 C 0.02413(9) 0.79456(14) 0.58645(10) 0.0188(4) Uani 1 1 d . . . H216 H 0.0382 0.8516 0.5723 0.023 Uiso 1 1 calc R . . C244 C 0.16263(9) 1.13260(15) 0.64313(11) 0.0206(4) Uani 1 1 d . . . H244 H 0.1678 1.1850 0.6731 0.025 Uiso 1 1 calc R . . C126 C -0.31826(8) 0.05197(13) 0.33623(9) 0.0131(3) Uani 1 1 d . . . H126 H -0.3129 0.1102 0.3612 0.016 Uiso 1 1 calc R . . C133 C -0.51094(9) 0.10702(15) 0.07384(10) 0.0203(4) Uani 1 1 d . . . H133 H -0.5512 0.0901 0.0689 0.024 Uiso 1 1 calc R . . C236 C 0.17259(10) 0.58307(15) 0.61258(10) 0.0220(4) Uani 1 1 d . . . H236 H 0.1775 0.6382 0.6404 0.026 Uiso 1 1 calc R . . C246 C 0.13835(9) 1.07513(14) 0.53254(10) 0.0172(4) Uani 1 1 d . . . H246 H 0.1268 1.0883 0.4869 0.021 Uiso 1 1 calc R . . C263 C 0.29414(9) 0.75522(15) 0.49396(10) 0.0211(4) Uani 1 1 d . . . H263 H 0.3111 0.6917 0.4979 0.025 Uiso 1 1 calc R . . C214 C -0.03126(10) 0.71928(17) 0.64522(10) 0.0234(4) Uani 1 1 d . . . H214 H -0.0552 0.7250 0.6709 0.028 Uiso 1 1 calc R . . C231 C 0.12942(8) 0.58532(13) 0.54754(9) 0.0138(3) Uani 1 1 d . . . C164 C -0.35154(9) 0.60704(15) 0.37315(10) 0.0203(4) Uani 1 1 d . . . H164 H -0.3374 0.6657 0.3972 0.024 Uiso 1 1 calc R . . C132 C -0.46648(9) 0.12178(14) 0.13622(10) 0.0165(4) Uani 1 1 d . . . H132 H -0.4760 0.1145 0.1741 0.020 Uiso 1 1 calc R . . C234 C 0.20084(9) 0.42023(15) 0.59557(11) 0.0205(4) Uani 1 1 d . . . H234 H 0.2249 0.3635 0.6121 0.025 Uiso 1 1 calc R . . C255 C -0.01840(9) 0.93148(15) 0.34732(11) 0.0220(4) Uani 1 1 d . . . H255 H -0.0604 0.9320 0.3405 0.026 Uiso 1 1 calc R . . C155 C -0.48562(10) 0.13561(15) 0.36336(10) 0.0220(4) Uani 1 1 d . . . H155 H -0.4779 0.0703 0.3788 0.026 Uiso 1 1 calc R . . C233 C 0.15905(9) 0.42249(14) 0.53129(10) 0.0195(4) Uani 1 1 d . . . H233 H 0.1548 0.3676 0.5034 0.023 Uiso 1 1 calc R . . C256 C 0.02550(9) 0.91461(14) 0.40985(10) 0.0187(4) Uani 1 1 d . . . H256 H 0.0136 0.9043 0.4459 0.022 Uiso 1 1 calc R . . C232 C 0.12311(9) 0.50479(14) 0.50698(10) 0.0167(4) Uani 1 1 d . . . H232 H 0.0942 0.5060 0.4626 0.020 Uiso 1 1 calc R . . C165 C -0.34571(10) 0.51909(15) 0.40642(10) 0.0235(4) Uani 1 1 d . . . H165 H -0.3272 0.5175 0.4532 0.028 Uiso 1 1 calc R . . C154 C -0.52705(9) 0.19188(17) 0.37791(10) 0.0227(4) Uani 1 1 d . . . H154 H -0.5480 0.1647 0.4029 0.027 Uiso 1 1 calc R . . C153 C -0.53820(9) 0.28787(16) 0.35623(10) 0.0206(4) Uani 1 1 d . . . H153 H -0.5669 0.3260 0.3661 0.025 Uiso 1 1 calc R . . C253 C 0.05983(9) 0.94785(15) 0.30451(10) 0.0205(4) Uani 1 1 d . . . H253 H 0.0715 0.9602 0.2686 0.025 Uiso 1 1 calc R . . C235 C 0.20801(10) 0.50093(15) 0.63643(11) 0.0250(4) Uani 1 1 d . . . H235 H 0.2372 0.4995 0.6806 0.030 Uiso 1 1 calc R . . C243 C 0.17204(9) 1.03736(15) 0.66630(10) 0.0188(4) Uani 1 1 d . . . H243 H 0.1836 1.0248 0.7120 0.023 Uiso 1 1 calc R . . C215 C -0.01120(10) 0.80260(16) 0.62396(11) 0.0242(4) Uani 1 1 d . . . H215 H -0.0216 0.8652 0.6350 0.029 Uiso 1 1 calc R . . C163 C -0.37784(10) 0.60915(14) 0.30515(11) 0.0227(4) Uani 1 1 d . . . H163 H -0.3811 0.6692 0.2825 0.027 Uiso 1 1 calc R . . C225 C 0.01663(10) 0.66518(15) 0.32042(10) 0.0209(4) Uani 1 1 d . . . H225 H 0.0327 0.6666 0.2870 0.025 Uiso 1 1 calc R . . C114 C -0.17300(10) 0.25094(16) 0.20385(11) 0.0249(5) Uani 1 1 d . . . H114 H -0.1356 0.2674 0.2003 0.030 Uiso 1 1 calc R . . C213 C -0.01648(10) 0.62785(16) 0.62911(10) 0.0221(4) Uani 1 1 d . . . H213 H -0.0303 0.5710 0.6437 0.027 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 0.01692(18) 0.01070(9) 0.01147(12) 0.00106(7) 0.00554(12) 0.00144(10) O1 0.0213(11) 0.0140(14) 0.0262(13) 0.0028(12) 0.0069(9) 0.0051(12) O2 0.0303(14) 0.0175(8) 0.0133(10) 0.0029(7) 0.0088(9) 0.0023(10) Cl1 0.0246(3) 0.0163(3) 0.0248(3) -0.0007(3) 0.0139(2) -0.0055(3) Mo1A 0.043(6) 0.021(2) 0.033(3) 0.005(2) 0.020(4) 0.002(3) O1A 0.045(10) 0.013(11) 0.03(2) 0.004(15) 0.027(13) -0.005(10) O2A 0.019(19) 0.024(17) 0.019(9) 0.009(9) 0.008(13) 0.004(11) Cl1A 0.047(9) 0.022(8) 0.016(6) 0.004(7) 0.014(6) 0.014(8) O10 0.0196(7) 0.0118(6) 0.0151(6) -0.0017(5) 0.0084(5) -0.0007(5) O20 0.0151(6) 0.0149(6) 0.0147(6) -0.0001(5) 0.0075(5) 0.0006(5) O30 0.0171(7) 0.0148(6) 0.0130(7) -0.0017(5) 0.0022(5) 0.0007(5) P2 0.0116(2) 0.0133(2) 0.0116(2) -0.00104(17) 0.00417(18) 0.00129(17) P3 0.0119(2) 0.0122(2) 0.0146(2) -0.00248(17) 0.00340(18) -0.00054(17) P11 0.0110(2) 0.0093(2) 0.0109(2) -0.00009(16) 0.00442(17) 0.00016(16) P22 0.0124(2) 0.0096(2) 0.0124(2) 0.00041(16) 0.00548(18) -0.00058(16) P12 0.0120(2) 0.0097(2) 0.0116(2) -0.00002(16) 0.00525(18) 0.00034(16) P1 0.0159(2) 0.0128(2) 0.0120(2) -0.00232(17) 0.00689(19) -0.00047(17) P21 0.0143(2) 0.0093(2) 0.0123(2) 0.00033(16) 0.00583(18) -0.00103(17) O12 0.0141(6) 0.0156(6) 0.0107(6) -0.0018(5) 0.0038(5) 0.0006(5) O23 0.0147(6) 0.0109(6) 0.0144(6) -0.0019(5) 0.0048(5) 0.0000(5) O13 0.0140(6) 0.0145(6) 0.0169(7) -0.0018(5) 0.0079(5) -0.0011(5) O33 0.0163(7) 0.0191(7) 0.0269(8) -0.0059(6) 0.0051(6) -0.0040(6) O11 0.0285(8) 0.0214(7) 0.0146(7) -0.0041(5) 0.0120(6) -0.0006(6) O22 0.0151(6) 0.0192(7) 0.0192(7) 0.0008(5) 0.0047(6) 0.0059(5) N1 0.0133(7) 0.0121(7) 0.0134(8) -0.0015(6) 0.0047(6) 0.0019(6) N2 0.0187(8) 0.0124(7) 0.0152(8) 0.0003(6) 0.0058(7) -0.0038(6) C131 0.0132(8) 0.0093(8) 0.0137(8) -0.0013(6) 0.0036(7) 0.0002(6) C262 0.0193(9) 0.0140(8) 0.0159(9) 0.0033(7) 0.0072(8) 0.0026(7) C121 0.0112(8) 0.0108(8) 0.0141(9) 0.0017(6) 0.0052(7) 0.0017(6) C211 0.0169(9) 0.0145(8) 0.0126(9) -0.0016(7) 0.0068(7) -0.0028(7) C123 0.0166(9) 0.0121(8) 0.0146(9) -0.0015(7) 0.0061(7) -0.0006(7) C161 0.0139(8) 0.0110(8) 0.0137(9) -0.0009(6) 0.0068(7) 0.0004(6) C136 0.0144(8) 0.0172(9) 0.0158(9) -0.0002(7) 0.0063(7) 0.0014(7) C261 0.0135(8) 0.0125(8) 0.0107(8) -0.0001(6) 0.0039(7) 0.0004(6) C124 0.0129(8) 0.0138(8) 0.0163(9) 0.0032(7) 0.0054(7) -0.0005(7) C116 0.0201(10) 0.0136(9) 0.0236(10) -0.0027(7) 0.0114(8) -0.0004(7) C145 0.0146(9) 0.0254(10) 0.0187(10) -0.0038(8) 0.0050(8) 0.0024(8) C221 0.0160(9) 0.0097(8) 0.0134(9) -0.0001(6) 0.0052(7) -0.0009(6) C222 0.0168(9) 0.0148(9) 0.0190(9) 0.0014(7) 0.0081(8) -0.0004(7) C142 0.0183(9) 0.0124(8) 0.0164(9) 0.0011(7) 0.0082(8) 0.0027(7) C141 0.0145(8) 0.0109(8) 0.0137(9) 0.0002(6) 0.0047(7) 0.0020(7) C162 0.0242(10) 0.0151(9) 0.0150(9) 0.0017(7) 0.0067(8) -0.0006(8) C166 0.0310(11) 0.0146(9) 0.0163(10) 0.0006(7) 0.0047(9) -0.0016(8) C241 0.0105(8) 0.0125(8) 0.0172(9) -0.0011(7) 0.0067(7) -0.0013(6) C122 0.0162(9) 0.0145(8) 0.0114(8) -0.0008(7) 0.0058(7) -0.0013(7) C265 0.0173(9) 0.0232(10) 0.0185(10) -0.0004(8) 0.0083(8) -0.0034(8) C252 0.0143(9) 0.0197(9) 0.0145(9) -0.0003(7) 0.0040(7) 0.0012(7) C254 0.0197(10) 0.0194(9) 0.0171(10) -0.0001(8) -0.0004(8) 0.0017(8) C151 0.0131(8) 0.0144(8) 0.0115(8) 0.0000(6) 0.0049(7) -0.0025(7) C242 0.0148(9) 0.0168(9) 0.0168(9) 0.0002(7) 0.0070(7) -0.0010(7) C224 0.0222(10) 0.0197(9) 0.0160(10) -0.0003(8) 0.0018(8) -0.0019(8) C112 0.0184(9) 0.0134(8) 0.0224(10) 0.0017(7) 0.0103(8) 0.0013(7) C251 0.0132(8) 0.0105(8) 0.0156(9) -0.0002(7) 0.0044(7) -0.0005(6) C152 0.0156(9) 0.0200(9) 0.0144(9) 0.0003(7) 0.0067(7) 0.0020(7) C223 0.0152(9) 0.0186(9) 0.0236(10) 0.0018(8) 0.0039(8) -0.0004(7) C245 0.0235(10) 0.0118(8) 0.0331(12) -0.0028(8) 0.0161(9) -0.0011(8) C226 0.0178(9) 0.0186(9) 0.0174(9) -0.0008(7) 0.0079(8) -0.0017(7) C135 0.0234(10) 0.0225(10) 0.0143(9) 0.0009(7) 0.0067(8) 0.0016(8) C111 0.0114(8) 0.0139(8) 0.0106(8) 0.0010(6) 0.0036(7) -0.0003(6) C264 0.0156(9) 0.0305(11) 0.0235(11) 0.0001(9) 0.0105(8) 0.0043(8) C146 0.0158(9) 0.0189(9) 0.0160(9) -0.0003(7) 0.0074(7) 0.0010(7) C113 0.0211(10) 0.0193(10) 0.0304(11) 0.0010(8) 0.0157(9) 0.0032(8) C266 0.0146(9) 0.0139(8) 0.0141(9) -0.0007(7) 0.0047(7) -0.0005(7) C125 0.0141(8) 0.0165(9) 0.0112(8) 0.0010(7) 0.0039(7) -0.0011(7) C134 0.0190(9) 0.0190(9) 0.0148(9) -0.0022(7) -0.0004(8) 0.0013(8) C156 0.0154(9) 0.0159(9) 0.0191(10) 0.0014(7) 0.0062(8) -0.0015(7) C212 0.0264(10) 0.0150(9) 0.0163(9) -0.0014(7) 0.0109(8) -0.0044(8) C115 0.0248(11) 0.0161(9) 0.0354(12) -0.0043(8) 0.0165(10) -0.0065(8) C144 0.0228(10) 0.0241(10) 0.0134(9) 0.0002(8) 0.0046(8) 0.0070(8) C143 0.0239(10) 0.0186(9) 0.0162(10) 0.0027(7) 0.0108(8) 0.0040(8) C216 0.0220(10) 0.0149(9) 0.0220(10) -0.0007(7) 0.0115(8) -0.0014(7) C244 0.0185(9) 0.0197(10) 0.0271(11) -0.0098(8) 0.0126(9) -0.0030(8) C126 0.0122(8) 0.0132(8) 0.0135(9) -0.0022(7) 0.0046(7) -0.0006(7) C133 0.0148(9) 0.0211(10) 0.0217(10) -0.0023(8) 0.0035(8) -0.0021(8) C236 0.0281(11) 0.0143(9) 0.0175(10) -0.0013(7) 0.0022(9) -0.0009(8) C246 0.0192(9) 0.0138(9) 0.0206(10) 0.0014(7) 0.0100(8) 0.0000(7) C263 0.0222(10) 0.0214(10) 0.0214(10) 0.0025(8) 0.0104(9) 0.0086(8) C214 0.0230(10) 0.0336(12) 0.0176(10) -0.0070(8) 0.0121(9) -0.0069(9) C231 0.0150(8) 0.0111(8) 0.0166(9) 0.0004(7) 0.0076(7) -0.0004(7) C164 0.0218(10) 0.0159(9) 0.0246(11) -0.0075(8) 0.0104(9) -0.0033(8) C132 0.0167(9) 0.0167(9) 0.0169(9) -0.0007(7) 0.0075(8) -0.0009(7) C234 0.0184(9) 0.0173(9) 0.0277(11) 0.0072(8) 0.0111(9) 0.0051(8) C255 0.0119(9) 0.0223(10) 0.0290(11) 0.0048(8) 0.0051(8) 0.0011(8) C155 0.0226(10) 0.0211(10) 0.0205(10) 0.0058(8) 0.0065(8) -0.0051(8) C233 0.0264(10) 0.0130(9) 0.0246(11) -0.0005(7) 0.0159(9) 0.0027(8) C256 0.0162(9) 0.0183(9) 0.0228(10) 0.0046(8) 0.0089(8) 0.0006(7) C232 0.0208(9) 0.0137(8) 0.0160(9) 0.0004(7) 0.0077(8) 0.0002(7) C165 0.0301(11) 0.0215(10) 0.0150(10) -0.0029(8) 0.0045(9) -0.0034(9) C154 0.0197(10) 0.0354(12) 0.0142(10) 0.0025(8) 0.0078(8) -0.0089(9) C153 0.0135(9) 0.0346(11) 0.0141(9) -0.0012(8) 0.0058(8) 0.0002(8) C253 0.0220(10) 0.0250(10) 0.0129(9) 0.0009(8) 0.0052(8) 0.0037(8) C235 0.0269(11) 0.0203(10) 0.0199(10) 0.0042(8) 0.0005(9) 0.0021(9) C243 0.0156(9) 0.0244(10) 0.0162(9) -0.0044(8) 0.0061(8) 0.0000(8) C215 0.0269(11) 0.0231(10) 0.0270(11) -0.0066(9) 0.0154(9) 0.0006(9) C163 0.0323(12) 0.0114(9) 0.0248(11) 0.0001(8) 0.0116(9) -0.0012(8) C225 0.0255(10) 0.0228(10) 0.0155(9) -0.0007(8) 0.0092(8) -0.0032(8) C114 0.0208(10) 0.0250(11) 0.0347(13) -0.0002(9) 0.0171(10) -0.0041(8) C213 0.0278(11) 0.0249(10) 0.0164(10) -0.0023(8) 0.0116(9) -0.0109(9) _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 O1 1.687(3) . ? Mo1 O2 1.694(2) . ? Mo1 O30 2.0586(14) . ? Mo1 O20 2.1938(14) . ? Mo1 O10 2.1965(13) . ? Mo1 Cl1 2.3628(9) . ? Mo1A O2A 1.61(5) . ? Mo1A O1A 1.70(6) . ? Mo1A O20 1.831(11) . ? Mo1A O10 2.193(7) . ? Mo1A Cl1A 2.36(4) . ? Mo1A O30 2.434(14) . ? O10 P1 1.5059(14) . ? O20 P2 1.5068(14) . ? O30 P3 1.5215(14) . ? P2 O22 1.4570(14) . ? P2 O12 1.6139(13) . ? P2 O23 1.6244(14) . ? P3 O33 1.4570(14) . ? P3 O23 1.6069(13) . ? P3 O13 1.6090(14) . ? P11 N1 1.5833(15) . ? P11 C121 1.7946(18) . ? P11 C131 1.7970(19) . ? P11 C111 1.8018(18) . ? P22 N2 1.5727(16) . ? P22 C241 1.7921(19) . ? P22 C261 1.7968(19) . ? P22 C251 1.8005(19) . ? P12 N1 1.5808(15) . ? P12 C161 1.7954(18) . ? P12 C151 1.8051(18) . ? P12 C141 1.8088(19) . ? P1 O11 1.4586(14) . ? P1 O12 1.6157(14) . ? P1 O13 1.6252(14) . ? P21 N2 1.5691(16) . ? P21 C231 1.7933(19) . ? P21 C211 1.7955(19) . ? P21 C221 1.8020(19) . ? C131 C136 1.390(3) . ? C131 C132 1.403(3) . ? C262 C263 1.386(3) . ? C262 C261 1.396(2) . ? C121 C126 1.399(3) . ? C121 C122 1.401(2) . ? C211 C212 1.397(3) . ? C211 C216 1.398(3) . ? C123 C124 1.389(3) . ? C123 C122 1.391(3) . ? C161 C162 1.389(3) . ? C161 C166 1.398(3) . ? C136 C135 1.388(3) . ? C261 C266 1.396(2) . ? C124 C125 1.387(3) . ? C116 C111 1.393(3) . ? C116 C115 1.397(3) . ? C145 C146 1.389(3) . ? C145 C144 1.390(3) . ? C221 C222 1.396(3) . ? C221 C226 1.401(3) . ? C222 C223 1.390(3) . ? C142 C143 1.387(3) . ? C142 C141 1.403(2) . ? C141 C146 1.400(3) . ? C162 C163 1.393(3) . ? C166 C165 1.380(3) . ? C241 C246 1.396(3) . ? C241 C242 1.400(3) . ? C265 C266 1.383(3) . ? C265 C264 1.392(3) . ? C252 C253 1.390(3) . ? C252 C251 1.397(3) . ? C254 C253 1.384(3) . ? C254 C255 1.391(3) . ? C151 C156 1.391(3) . ? C151 C152 1.400(3) . ? C242 C243 1.389(3) . ? C224 C223 1.386(3) . ? C224 C225 1.396(3) . ? C112 C113 1.385(3) . ? C112 C111 1.397(3) . ? C251 C256 1.400(3) . ? C152 C153 1.386(3) . ? C245 C244 1.383(3) . ? C245 C246 1.390(3) . ? C226 C225 1.389(3) . ? C135 C134 1.380(3) . ? C264 C263 1.385(3) . ? C113 C114 1.391(3) . ? C125 C126 1.390(3) . ? C134 C133 1.391(3) . ? C156 C155 1.390(3) . ? C212 C213 1.388(3) . ? C115 C114 1.383(3) . ? C144 C143 1.393(3) . ? C216 C215 1.393(3) . ? C244 C243 1.388(3) . ? C133 C132 1.383(3) . ? C236 C235 1.382(3) . ? C236 C231 1.400(3) . ? C214 C213 1.385(3) . ? C214 C215 1.388(3) . ? C231 C232 1.390(3) . ? C164 C163 1.379(3) . ? C164 C165 1.389(3) . ? C234 C233 1.377(3) . ? C234 C235 1.394(3) . ? C255 C256 1.385(3) . ? C155 C154 1.384(3) . ? C233 C232 1.391(3) . ? C154 C153 1.390(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mo1 O2 102.60(18) . . ? O1 Mo1 O30 94.00(14) . . ? O2 Mo1 O30 93.07(9) . . ? O1 Mo1 O20 167.08(17) . . ? O2 Mo1 O20 89.88(8) . . ? O30 Mo1 O20 81.84(5) . . ? O1 Mo1 O10 89.51(16) . . ? O2 Mo1 O10 167.23(9) . . ? O30 Mo1 O10 81.91(5) . . ? O20 Mo1 O10 77.82(5) . . ? O1 Mo1 Cl1 97.13(14) . . ? O2 Mo1 Cl1 96.16(8) . . ? O30 Mo1 Cl1 163.62(5) . . ? O20 Mo1 Cl1 84.68(4) . . ? O10 Mo1 Cl1 86.21(4) . . ? O2A Mo1A O1A 103(3) . . ? O2A Mo1A O20 92.1(19) . . ? O1A Mo1A O20 98.0(16) . . ? O2A Mo1A O10 163.9(18) . . ? O1A Mo1A O10 92.6(19) . . ? O20 Mo1A O10 86.0(3) . . ? O2A Mo1A Cl1A 98.6(19) . . ? O1A Mo1A Cl1A 98.3(18) . . ? O20 Mo1A Cl1A 157.8(10) . . ? O10 Mo1A Cl1A 78.3(9) . . ? O2A Mo1A O30 89.9(17) . . ? O1A Mo1A O30 166.5(19) . . ? O20 Mo1A O30 80.3(3) . . ? O10 Mo1A O30 74.0(3) . . ? Cl1A Mo1A O30 80.3(9) . . ? P1 O10 Mo1A 130.1(2) . . ? P1 O10 Mo1 131.53(8) . . ? Mo1A O10 Mo1 14.8(5) . . ? P2 O20 Mo1A 140.7(3) . . ? P2 O20 Mo1 132.11(8) . . ? Mo1A O20 Mo1 12.4(5) . . ? P3 O30 Mo1 134.12(8) . . ? P3 O30 Mo1A 124.9(3) . . ? Mo1 O30 Mo1A 10.9(3) . . ? O22 P2 O20 120.31(8) . . ? O22 P2 O12 110.86(8) . . ? O20 P2 O12 107.25(7) . . ? O22 P2 O23 109.83(8) . . ? O20 P2 O23 106.36(7) . . ? O12 P2 O23 100.31(7) . . ? O33 P3 O30 118.12(8) . . ? O33 P3 O23 111.04(8) . . ? O30 P3 O23 106.91(7) . . ? O33 P3 O13 111.60(8) . . ? O30 P3 O13 106.33(7) . . ? O23 P3 O13 101.40(7) . . ? N1 P11 C121 111.92(8) . . ? N1 P11 C131 115.11(8) . . ? C121 P11 C131 105.94(8) . . ? N1 P11 C111 109.03(8) . . ? C121 P11 C111 107.00(8) . . ? C131 P11 C111 107.45(8) . . ? N2 P22 C241 108.34(9) . . ? N2 P22 C261 109.65(9) . . ? C241 P22 C261 109.12(8) . . ? N2 P22 C251 114.52(9) . . ? C241 P22 C251 107.91(9) . . ? C261 P22 C251 107.18(8) . . ? N1 P12 C161 109.95(8) . . ? N1 P12 C151 111.32(9) . . ? C161 P12 C151 104.10(8) . . ? N1 P12 C141 113.41(8) . . ? C161 P12 C141 108.52(8) . . ? C151 P12 C141 109.09(9) . . ? O11 P1 O10 120.21(8) . . ? O11 P1 O12 109.93(8) . . ? O10 P1 O12 107.83(7) . . ? O11 P1 O13 110.38(8) . . ? O10 P1 O13 106.33(7) . . ? O12 P1 O13 100.26(7) . . ? N2 P21 C231 110.09(9) . . ? N2 P21 C211 109.47(9) . . ? C231 P21 C211 106.53(9) . . ? N2 P21 C221 113.95(9) . . ? C231 P21 C221 108.07(9) . . ? C211 P21 C221 108.45(9) . . ? P2 O12 P1 121.27(8) . . ? P3 O23 P2 121.85(8) . . ? P3 O13 P1 121.90(8) . . ? P12 N1 P11 141.76(11) . . ? P21 N2 P22 148.65(12) . . ? C136 C131 C132 119.93(17) . . ? C136 C131 P11 121.78(14) . . ? C132 C131 P11 118.27(14) . . ? C263 C262 C261 119.58(18) . . ? C126 C121 C122 119.65(16) . . ? C126 C121 P11 121.33(14) . . ? C122 C121 P11 118.85(14) . . ? C212 C211 C216 119.44(17) . . ? C212 C211 P21 120.76(14) . . ? C216 C211 P21 119.80(14) . . ? C124 C123 C122 119.71(17) . . ? C162 C161 C166 119.06(17) . . ? C162 C161 P12 122.68(14) . . ? C166 C161 P12 118.26(14) . . ? C135 C136 C131 119.83(18) . . ? C262 C261 C266 119.87(17) . . ? C262 C261 P22 119.70(14) . . ? C266 C261 P22 120.41(14) . . ? C125 C124 C123 120.30(17) . . ? C111 C116 C115 119.65(18) . . ? C146 C145 C144 120.03(19) . . ? C222 C221 C226 119.59(17) . . ? C222 C221 P21 121.79(14) . . ? C226 C221 P21 118.56(14) . . ? C223 C222 C221 120.14(18) . . ? C143 C142 C141 120.27(18) . . ? C146 C141 C142 119.19(17) . . ? C146 C141 P12 122.49(14) . . ? C142 C141 P12 118.23(14) . . ? C161 C162 C163 120.11(18) . . ? C165 C166 C161 120.63(19) . . ? C246 C241 C242 119.73(17) . . ? C246 C241 P22 121.12(15) . . ? C242 C241 P22 119.10(14) . . ? C123 C122 C121 120.24(17) . . ? C266 C265 C264 119.60(18) . . ? C253 C252 C251 120.14(18) . . ? C253 C254 C255 119.85(19) . . ? C156 C151 C152 119.84(17) . . ? C156 C151 P12 119.56(14) . . ? C152 C151 P12 120.50(14) . . ? C243 C242 C241 119.72(18) . . ? C223 C224 C225 120.26(19) . . ? C113 C112 C111 120.15(18) . . ? C252 C251 C256 119.22(17) . . ? C252 C251 P22 122.51(14) . . ? C256 C251 P22 118.12(14) . . ? C153 C152 C151 119.84(18) . . ? C224 C223 C222 120.12(19) . . ? C244 C245 C246 120.26(19) . . ? C225 C226 C221 120.05(18) . . ? C134 C135 C136 120.39(19) . . ? C116 C111 C112 119.97(17) . . ? C116 C111 P11 119.90(14) . . ? C112 C111 P11 120.11(14) . . ? C263 C264 C265 120.39(18) . . ? C145 C146 C141 120.32(18) . . ? C112 C113 C114 119.66(19) . . ? C265 C266 C261 120.26(18) . . ? C124 C125 C126 120.47(17) . . ? C135 C134 C133 120.00(18) . . ? C155 C156 C151 119.97(18) . . ? C213 C212 C211 120.23(19) . . ? C114 C115 C116 119.84(19) . . ? C145 C144 C143 120.17(19) . . ? C142 C143 C144 120.03(18) . . ? C215 C216 C211 119.94(18) . . ? C245 C244 C243 120.20(18) . . ? C125 C126 C121 119.60(17) . . ? C132 C133 C134 120.34(18) . . ? C235 C236 C231 120.17(19) . . ? C245 C246 C241 119.85(19) . . ? C264 C263 C262 120.28(19) . . ? C213 C214 C215 120.26(19) . . ? C232 C231 C236 119.45(18) . . ? C232 C231 P21 122.26(15) . . ? C236 C231 P21 118.29(14) . . ? C163 C164 C165 119.99(19) . . ? C133 C132 C131 119.50(18) . . ? C233 C234 C235 120.20(19) . . ? C256 C255 C254 120.30(18) . . ? C154 C155 C156 119.98(19) . . ? C234 C233 C232 120.23(18) . . ? C255 C256 C251 120.17(18) . . ? C231 C232 C233 120.04(18) . . ? C166 C165 C164 119.91(19) . . ? C155 C154 C153 120.43(18) . . ? C152 C153 C154 119.93(19) . . ? C254 C253 C252 120.30(19) . . ? C236 C235 C234 119.9(2) . . ? C244 C243 C242 120.23(19) . . ? C214 C215 C216 120.04(19) . . ? C164 C163 C162 120.28(19) . . ? C226 C225 C224 119.84(19) . . ? C115 C114 C113 120.71(19) . . ? C214 C213 C212 120.09(19) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 29.57 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.519 _refine_diff_density_min -0.526 _refine_diff_density_rms 0.078 _database_code_depnum_ccdc_archive 'CCDC 898619' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_12083 #TrackingRef '13598_web_deposit_cif_file_1_DanielTofan_1346189895.MoP3_12083.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H60 Cl2 Mo N2 O10 P7' _chemical_formula_weight 1496.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8738(14) _cell_length_b 12.8662(16) _cell_length_c 13.5974(17) _cell_angle_alpha 63.331(2) _cell_angle_beta 87.802(2) _cell_angle_gamma 80.090(2) _cell_volume 1673.0(4) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9209 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 31.52 _exptl_crystal_description Plate _exptl_crystal_colour green _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.486 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 767 _exptl_absorpt_coefficient_mu 0.505 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8798 _exptl_absorpt_correction_T_max 0.9559 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; 'Siemens three-circle diffractometer, Bruker APEX CCD' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 46986 _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_sigmaI/netI 0.0217 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 30.51 _reflns_number_total 10155 _reflns_number_gt 9675 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2011.4.0 (Bruker-AXS, 2011)' _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2011)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0010P)^2^+9.5499P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10155 _refine_ls_number_parameters 533 _refine_ls_number_restraints 51 _refine_ls_R_factor_all 0.0697 _refine_ls_R_factor_gt 0.0676 _refine_ls_wR_factor_ref 0.1673 _refine_ls_wR_factor_gt 0.1664 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.113 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1B Mo 0.4691(12) -0.0832(13) 0.5669(11) 0.0216(16) Uani 0.158(7) 1 d PU A -2 Cl1B Cl 0.2526(9) -0.0757(11) 0.5839(9) 0.023(2) Uani 0.158(7) 1 d PU A -2 O1B O 0.509(3) -0.231(4) 0.597(3) 0.029(8) Uani 0.158(7) 1 d PU A -2 Cl2B Cl 0.480(4) -0.105(4) 0.747(3) 0.028(5) Uani 0.158(7) 1 d PU A -2 Mo1A Mo 0.4439(5) -0.0739(6) 0.5610(5) 0.0169(6) Uani 0.342(7) 1 d PU A -1 Cl1A Cl 0.5249(4) -0.2694(4) 0.5956(3) 0.0244(10) Uani 0.342(7) 1 d PU A -1 O1A O 0.2886(19) -0.0826(17) 0.5711(16) 0.024(3) Uani 0.342(7) 1 d PU A -1 Cl2A Cl 0.4930(16) -0.1138(17) 0.7435(13) 0.0213(17) Uani 0.342(7) 1 d PU A -1 O1 O 0.6391(4) -0.0466(4) 0.5307(4) 0.0164(8) Uani 0.50 1 d PU A -1 O2 O 0.4408(4) -0.0240(4) 0.3937(4) 0.0182(8) Uani 0.50 1 d PU A -1 O3 O 0.4210(4) 0.1059(4) 0.5168(4) 0.0176(8) Uani 0.50 1 d PU A -1 P1 P 0.6923(3) 0.0500(2) 0.4369(2) 0.0137(4) Uani 0.50 1 d P A -1 P2 P 0.4902(2) 0.0758(2) 0.29907(19) 0.0150(4) Uani 0.50 1 d P A -1 P3 P 0.4692(3) 0.2062(3) 0.4222(2) 0.0142(5) Uani 0.50 1 d P A -1 O33 O 0.4298(5) 0.3273(5) 0.4060(4) 0.0216(9) Uani 0.50 1 d P A -1 O13 O 0.6202(4) 0.1741(4) 0.4305(4) 0.0184(8) Uani 0.50 1 d P A -1 O12 O 0.6381(4) 0.0593(4) 0.3233(4) 0.0166(8) Uani 0.50 1 d P A -1 O23 O 0.4412(4) 0.1953(4) 0.3110(4) 0.0172(8) Uani 0.50 1 d P A -1 O11 O 0.8274(5) 0.0488(4) 0.4331(4) 0.0213(9) Uani 0.50 1 d P A -1 O22 O 0.4650(5) 0.0956(5) 0.1864(4) 0.0229(10) Uani 0.50 1 d P A -1 P12 P -0.13985(7) 0.28862(7) -0.00998(6) 0.01358(14) Uani 1 1 d . . . P11 P -0.04153(7) 0.39919(7) -0.23704(6) 0.01355(14) Uani 1 1 d . . . N1 N -0.0613(3) 0.3586(3) -0.1102(2) 0.0193(5) Uani 1 1 d . . . C41 C -0.0352(3) 0.1913(3) 0.1061(2) 0.0182(6) Uani 1 1 d . . . C61 C -0.2357(3) 0.2009(3) -0.0343(2) 0.0167(5) Uani 1 1 d . . . C21 C -0.0348(3) 0.5537(3) -0.3071(2) 0.0162(5) Uani 1 1 d . . . C31 C 0.1064(3) 0.3250(3) -0.2568(2) 0.0152(5) Uani 1 1 d . . . C51 C -0.2395(3) 0.3892(3) 0.0299(3) 0.0156(5) Uani 1 1 d . . . C16 C -0.1355(3) 0.3167(3) -0.3729(3) 0.0206(6) Uani 1 1 d . . . H16 H -0.0511 0.2902 -0.3831 0.025 Uiso 1 1 calc R . . C66 C -0.3643(3) 0.2145(3) -0.0216(3) 0.0194(6) Uani 1 1 d . . . H66 H -0.4030 0.2656 0.0081 0.023 Uiso 1 1 calc R . . C56 C -0.2985(3) 0.3456(3) 0.1306(3) 0.0197(6) Uani 1 1 d . . . H56 H -0.2889 0.2629 0.1760 0.024 Uiso 1 1 calc R . . C52 C -0.2551(3) 0.5105(3) -0.0376(3) 0.0234(6) Uani 1 1 d . . . H52 H -0.2158 0.5404 -0.1061 0.028 Uiso 1 1 calc R . . C11 C -0.1627(3) 0.3735(3) -0.3061(2) 0.0168(5) Uani 1 1 d . . . C12 C -0.2876(3) 0.4138(3) -0.2924(3) 0.0214(6) Uani 1 1 d . . . H12 H -0.3065 0.4530 -0.2474 0.026 Uiso 1 1 calc R . . C36 C 0.1716(3) 0.3791(3) -0.3521(3) 0.0198(6) Uani 1 1 d . . . H36 H 0.1387 0.4566 -0.4063 0.024 Uiso 1 1 calc R . . C42 C -0.0653(4) 0.0844(3) 0.1855(3) 0.0259(7) Uani 1 1 d . . . H42 H -0.1398 0.0593 0.1772 0.031 Uiso 1 1 calc R . . C26 C -0.1203(3) 0.6327(3) -0.3930(3) 0.0214(6) Uani 1 1 d . . . H26 H -0.1858 0.6052 -0.4137 0.026 Uiso 1 1 calc R . . C32 C 0.1562(3) 0.2114(3) -0.1772(3) 0.0220(6) Uani 1 1 d . . . H32 H 0.1140 0.1748 -0.1112 0.026 Uiso 1 1 calc R . . C46 C 0.0740(3) 0.2274(3) 0.1186(3) 0.0225(6) Uani 1 1 d . . . H46 H 0.0946 0.2996 0.0642 0.027 Uiso 1 1 calc R . . C64 C -0.3799(4) 0.0774(3) -0.0945(3) 0.0258(7) Uani 1 1 d . . . H64 H -0.4292 0.0368 -0.1167 0.031 Uiso 1 1 calc R . . C62 C -0.1784(3) 0.1220(3) -0.0741(3) 0.0239(7) Uani 1 1 d . . . H62 H -0.0904 0.1101 -0.0806 0.029 Uiso 1 1 calc R . . C24 C -0.0135(4) 0.7910(3) -0.4189(3) 0.0248(7) Uani 1 1 d . . . H24 H -0.0053 0.8718 -0.4579 0.030 Uiso 1 1 calc R . . C55 C -0.3704(3) 0.4225(3) 0.1642(3) 0.0260(7) Uani 1 1 d . . . H55 H -0.4096 0.3929 0.2327 0.031 Uiso 1 1 calc R . . C35 C 0.2843(3) 0.3198(3) -0.3679(3) 0.0241(7) Uani 1 1 d . . . H35 H 0.3291 0.3576 -0.4320 0.029 Uiso 1 1 calc R . . C44 C 0.1245(4) 0.0515(4) 0.2893(3) 0.0384(11) Uani 1 1 d . . . H44 H 0.1795 0.0032 0.3518 0.046 Uiso 1 1 calc R . . C65 C -0.4365(3) 0.1533(3) -0.0524(3) 0.0233(6) Uani 1 1 d . . . H65 H -0.5243 0.1635 -0.0445 0.028 Uiso 1 1 calc R . . C63 C -0.2514(4) 0.0610(3) -0.1040(3) 0.0295(8) Uani 1 1 d . . . H63 H -0.2128 0.0076 -0.1312 0.035 Uiso 1 1 calc R . . C25 C -0.1097(4) 0.7511(3) -0.4481(3) 0.0250(7) Uani 1 1 d . . . H25 H -0.1685 0.8048 -0.5059 0.030 Uiso 1 1 calc R . . C22 C 0.0607(3) 0.5954(3) -0.2761(3) 0.0226(6) Uani 1 1 d . . . H22 H 0.1180 0.5429 -0.2165 0.027 Uiso 1 1 calc R . . C33 C 0.2677(3) 0.1518(3) -0.1950(3) 0.0253(7) Uani 1 1 d . . . H33 H 0.3004 0.0739 -0.1417 0.030 Uiso 1 1 calc R . . C54 C -0.3850(3) 0.5436(3) 0.0969(4) 0.0297(8) Uani 1 1 d . . . H54 H -0.4339 0.5965 0.1201 0.036 Uiso 1 1 calc R . . C34 C 0.3313(3) 0.2059(3) -0.2904(3) 0.0245(7) Uani 1 1 d . . . H34 H 0.4070 0.1647 -0.3024 0.029 Uiso 1 1 calc R . . C23 C 0.0708(4) 0.7139(3) -0.3333(3) 0.0277(7) Uani 1 1 d . . . H23 H 0.1361 0.7422 -0.3134 0.033 Uiso 1 1 calc R . . C15 C -0.2324(4) 0.2989(4) -0.4247(3) 0.0279(7) Uani 1 1 d . . . H15 H -0.2140 0.2590 -0.4691 0.034 Uiso 1 1 calc R . . C53 C -0.3288(4) 0.5878(3) -0.0038(3) 0.0305(8) Uani 1 1 d . . . H53 H -0.3405 0.6705 -0.0497 0.037 Uiso 1 1 calc R . . C13 C -0.3836(3) 0.3959(3) -0.3451(3) 0.0274(7) Uani 1 1 d . . . H13 H -0.4682 0.4225 -0.3357 0.033 Uiso 1 1 calc R . . C14 C -0.3551(4) 0.3390(4) -0.4115(3) 0.0310(8) Uani 1 1 d . . . H14 H -0.4207 0.3277 -0.4480 0.037 Uiso 1 1 calc R . . C45 C 0.1532(4) 0.1571(4) 0.2115(3) 0.0330(9) Uani 1 1 d . . . H45 H 0.2272 0.1822 0.2211 0.040 Uiso 1 1 calc R . . C43 C 0.0165(4) 0.0155(3) 0.2771(3) 0.0345(9) Uani 1 1 d . . . H43 H -0.0027 -0.0573 0.3317 0.041 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 Mo1B 0.024(4) 0.0169(18) 0.0199(17) -0.0032(13) 0.004(2) -0.009(2) Cl1B 0.019(4) 0.028(3) 0.018(3) -0.006(2) 0.007(3) -0.009(4) O1B 0.040(15) 0.021(11) 0.019(13) -0.004(11) 0.022(10) -0.005(12) Cl2B 0.038(9) 0.026(8) 0.020(6) -0.009(5) 0.016(5) -0.008(6) Mo1A 0.0214(16) 0.0185(11) 0.0138(8) -0.0076(8) 0.0063(9) -0.0116(11) Cl1A 0.037(2) 0.0141(19) 0.0232(13) -0.0079(13) 0.0081(12) -0.0101(15) O1A 0.028(6) 0.028(7) 0.024(6) -0.014(6) 0.007(5) -0.017(6) Cl2A 0.025(3) 0.024(3) 0.014(3) -0.007(2) 0.002(3) -0.006(3) O1 0.0195(19) 0.0138(19) 0.0141(19) -0.0046(16) 0.0022(15) -0.0038(15) O2 0.021(2) 0.020(2) 0.0163(19) -0.0091(17) 0.0037(16) -0.0093(17) O3 0.021(2) 0.019(2) 0.0142(19) -0.0085(16) 0.0040(16) -0.0025(16) P1 0.0141(11) 0.0110(10) 0.0153(8) -0.0049(8) 0.0024(8) -0.0039(7) P2 0.0180(9) 0.0153(9) 0.0125(9) -0.0062(7) 0.0028(8) -0.0055(7) P3 0.0159(10) 0.0135(13) 0.0135(11) -0.0065(9) 0.0027(8) -0.0024(7) O33 0.025(2) 0.016(2) 0.025(2) -0.011(2) 0.0022(19) -0.002(2) O13 0.020(2) 0.019(2) 0.016(2) -0.0081(17) -0.0012(16) -0.0046(17) O12 0.019(2) 0.020(2) 0.0147(19) -0.0107(17) 0.0023(15) -0.0041(16) O23 0.019(2) 0.020(2) 0.0132(19) -0.0089(17) -0.0039(15) -0.0011(16) O11 0.016(3) 0.016(2) 0.025(2) -0.0044(18) 0.0009(18) -0.0017(18) O22 0.028(2) 0.030(3) 0.019(2) -0.016(2) 0.0027(18) -0.010(2) P12 0.0138(3) 0.0142(3) 0.0123(3) -0.0052(3) 0.0017(2) -0.0040(3) P11 0.0134(3) 0.0140(3) 0.0115(3) -0.0042(3) 0.0006(2) -0.0023(3) N1 0.0202(12) 0.0258(13) 0.0118(11) -0.0067(10) 0.0031(9) -0.0092(10) C41 0.0210(14) 0.0177(13) 0.0142(13) -0.0070(11) 0.0008(10) 0.0001(11) C61 0.0187(13) 0.0170(13) 0.0158(13) -0.0077(11) 0.0033(10) -0.0067(11) C21 0.0206(14) 0.0142(12) 0.0125(12) -0.0056(10) 0.0019(10) -0.0011(10) C31 0.0147(12) 0.0146(12) 0.0151(12) -0.0059(10) -0.0013(10) -0.0015(10) C51 0.0139(12) 0.0157(13) 0.0181(13) -0.0077(11) 0.0002(10) -0.0040(10) C16 0.0220(15) 0.0229(15) 0.0192(14) -0.0109(12) 0.0020(11) -0.0061(12) C66 0.0175(14) 0.0207(14) 0.0221(14) -0.0106(12) 0.0014(11) -0.0059(11) C56 0.0189(14) 0.0201(14) 0.0233(15) -0.0116(12) 0.0051(11) -0.0066(11) C52 0.0246(16) 0.0177(14) 0.0244(16) -0.0067(12) 0.0006(12) -0.0026(12) C11 0.0176(13) 0.0178(13) 0.0140(12) -0.0060(11) 0.0001(10) -0.0041(11) C12 0.0189(14) 0.0243(15) 0.0211(15) -0.0109(13) -0.0017(11) -0.0015(12) C36 0.0193(14) 0.0213(14) 0.0158(13) -0.0071(11) -0.0001(11) -0.0001(11) C42 0.0371(19) 0.0189(15) 0.0168(14) -0.0048(12) 0.0038(13) -0.0020(13) C26 0.0206(14) 0.0208(15) 0.0177(14) -0.0052(12) -0.0005(11) -0.0005(12) C32 0.0173(14) 0.0175(14) 0.0237(15) -0.0031(12) 0.0002(11) -0.0019(11) C46 0.0224(15) 0.0244(16) 0.0203(15) -0.0115(13) -0.0047(12) 0.0024(12) C64 0.0366(19) 0.0215(15) 0.0231(16) -0.0097(13) 0.0013(13) -0.0155(14) C62 0.0247(16) 0.0230(15) 0.0274(16) -0.0139(13) 0.0090(13) -0.0074(13) C24 0.047(2) 0.0125(13) 0.0150(14) -0.0062(11) 0.0033(13) -0.0049(13) C55 0.0215(16) 0.0286(17) 0.0317(18) -0.0170(15) 0.0076(13) -0.0058(13) C35 0.0194(15) 0.0335(18) 0.0175(14) -0.0109(13) 0.0021(11) -0.0014(13) C44 0.050(2) 0.039(2) 0.0218(17) -0.0183(16) -0.0162(16) 0.0221(19) C65 0.0214(15) 0.0244(16) 0.0265(16) -0.0112(13) -0.0001(12) -0.0098(12) C63 0.041(2) 0.0267(17) 0.0301(18) -0.0187(15) 0.0134(15) -0.0150(15) C25 0.0328(18) 0.0178(15) 0.0169(14) -0.0034(12) 0.0007(12) 0.0016(13) C22 0.0306(17) 0.0177(14) 0.0183(14) -0.0064(12) -0.0033(12) -0.0050(12) C33 0.0196(15) 0.0173(14) 0.0326(18) -0.0067(13) -0.0044(13) 0.0013(12) C54 0.0229(16) 0.0285(18) 0.043(2) -0.0226(17) 0.0041(15) 0.0001(14) C34 0.0172(14) 0.0295(17) 0.0287(17) -0.0167(14) -0.0018(12) 0.0025(12) C23 0.044(2) 0.0191(15) 0.0222(16) -0.0092(13) -0.0019(14) -0.0108(14) C15 0.0312(18) 0.0356(19) 0.0247(16) -0.0181(15) 0.0015(14) -0.0120(15) C53 0.0311(19) 0.0187(16) 0.037(2) -0.0109(15) -0.0001(15) 0.0021(14) C13 0.0183(15) 0.0326(18) 0.0289(17) -0.0117(15) -0.0035(13) -0.0033(13) C14 0.0256(17) 0.042(2) 0.0292(18) -0.0166(17) -0.0034(14) -0.0133(16) C45 0.0298(19) 0.040(2) 0.033(2) -0.0248(18) -0.0140(15) 0.0115(16) C43 0.054(3) 0.0219(17) 0.0160(15) -0.0032(13) 0.0009(15) 0.0088(16) _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 Mo1B O1B 1.73(5) . ? Mo1B Cl1B 2.347(18) . ? Mo1B Cl2B 2.35(4) . ? Mo1A O1A 1.71(2) . ? Mo1A O2 2.068(7) . ? Mo1A O3 2.083(8) . ? Mo1A O1 2.204(7) . ? Mo1A Cl1A 2.352(8) . ? Mo1A Cl2A 2.360(15) . ? O1 P1 1.507(5) . ? O2 P2 1.514(5) . ? O3 P3 1.512(5) . ? P1 O11 1.466(6) . ? P1 O13 1.620(5) . ? P1 O12 1.620(5) . ? P2 O22 1.464(5) . ? P2 O12 1.613(5) . ? P2 O23 1.616(5) . ? P3 O33 1.459(7) . ? P3 O13 1.618(5) . ? P3 O23 1.625(5) . ? P12 N1 1.572(3) . ? P12 C41 1.796(3) . ? P12 C61 1.799(3) . ? P12 C51 1.801(3) . ? P11 N1 1.580(3) . ? P11 C21 1.792(3) . ? P11 C31 1.800(3) . ? P11 C11 1.803(3) . ? C41 C46 1.391(5) . ? C41 C42 1.399(5) . ? C61 C66 1.393(4) . ? C61 C62 1.401(4) . ? C21 C26 1.398(4) . ? C21 C22 1.405(5) . ? C31 C32 1.398(4) . ? C31 C36 1.398(4) . ? C51 C52 1.394(4) . ? C51 C56 1.403(4) . ? C16 C15 1.394(5) . ? C16 C11 1.397(4) . ? C66 C65 1.394(4) . ? C56 C55 1.381(5) . ? C52 C53 1.396(5) . ? C11 C12 1.404(4) . ? C12 C13 1.394(5) . ? C36 C35 1.391(5) . ? C42 C43 1.397(5) . ? C26 C25 1.387(5) . ? C32 C33 1.393(5) . ? C46 C45 1.395(5) . ? C64 C63 1.387(6) . ? C64 C65 1.388(5) . ? C62 C63 1.391(5) . ? C24 C23 1.383(5) . ? C24 C25 1.385(5) . ? C55 C54 1.391(5) . ? C35 C34 1.384(5) . ? C44 C43 1.376(7) . ? C44 C45 1.376(7) . ? C22 C23 1.389(5) . ? C33 C34 1.390(5) . ? C54 C53 1.388(6) . ? C15 C14 1.380(6) . ? C13 C14 1.393(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1B Mo1B Cl1B 97.6(14) . . ? O1B Mo1B Cl2B 98.4(18) . . ? Cl1B Mo1B Cl2B 87.7(11) . . ? O1A Mo1A O2 93.4(7) . . ? O1A Mo1A O3 96.1(7) . . ? O2 Mo1A O3 85.8(3) . . ? O1A Mo1A O1 173.9(8) . . ? O2 Mo1A O1 81.6(3) . . ? O3 Mo1A O1 80.0(3) . . ? O1A Mo1A Cl1A 99.1(7) . . ? O2 Mo1A Cl1A 89.7(2) . . ? O3 Mo1A Cl1A 164.4(3) . . ? O1 Mo1A Cl1A 84.6(2) . . ? O1A Mo1A Cl2A 99.7(8) . . ? O2 Mo1A Cl2A 166.3(5) . . ? O3 Mo1A Cl2A 88.8(5) . . ? O1 Mo1A Cl2A 85.0(5) . . ? Cl1A Mo1A Cl2A 92.1(5) . . ? P1 O1 Mo1A 130.0(3) . . ? P2 O2 Mo1A 131.2(3) . . ? P3 O3 Mo1A 131.8(3) . . ? O11 P1 O1 120.4(3) . . ? O11 P1 O13 109.8(3) . . ? O1 P1 O13 106.9(3) . . ? O11 P1 O12 110.5(3) . . ? O1 P1 O12 107.4(3) . . ? O13 P1 O12 100.0(3) . . ? O22 P2 O2 118.8(3) . . ? O22 P2 O12 110.7(3) . . ? O2 P2 O12 107.7(3) . . ? O22 P2 O23 110.2(3) . . ? O2 P2 O23 107.5(3) . . ? O12 P2 O23 100.4(2) . . ? O33 P3 O3 120.1(3) . . ? O33 P3 O13 109.7(3) . . ? O3 P3 O13 107.5(3) . . ? O33 P3 O23 110.8(3) . . ? O3 P3 O23 106.8(3) . . ? O13 P3 O23 99.9(3) . . ? P3 O13 P1 121.3(3) . . ? P2 O12 P1 121.5(3) . . ? P2 O23 P3 122.0(3) . . ? N1 P12 C41 108.95(15) . . ? N1 P12 C61 114.72(14) . . ? C41 P12 C61 107.69(15) . . ? N1 P12 C51 110.16(15) . . ? C41 P12 C51 106.92(14) . . ? C61 P12 C51 108.09(14) . . ? N1 P11 C21 110.73(15) . . ? N1 P11 C31 110.31(15) . . ? C21 P11 C31 105.79(14) . . ? N1 P11 C11 113.79(14) . . ? C21 P11 C11 107.37(14) . . ? C31 P11 C11 108.50(14) . . ? P12 N1 P11 144.82(19) . . ? C46 C41 C42 120.4(3) . . ? C46 C41 P12 118.4(2) . . ? C42 C41 P12 121.2(3) . . ? C66 C61 C62 119.7(3) . . ? C66 C61 P12 122.3(2) . . ? C62 C61 P12 117.8(2) . . ? C26 C21 C22 119.5(3) . . ? C26 C21 P11 121.6(3) . . ? C22 C21 P11 118.8(2) . . ? C32 C31 C36 119.4(3) . . ? C32 C31 P11 119.9(2) . . ? C36 C31 P11 120.7(2) . . ? C52 C51 C56 119.9(3) . . ? C52 C51 P12 120.1(2) . . ? C56 C51 P12 120.0(2) . . ? C15 C16 C11 119.8(3) . . ? C61 C66 C65 120.2(3) . . ? C55 C56 C51 120.3(3) . . ? C51 C52 C53 119.5(3) . . ? C16 C11 C12 119.9(3) . . ? C16 C11 P11 121.9(2) . . ? C12 C11 P11 118.2(2) . . ? C13 C12 C11 119.7(3) . . ? C35 C36 C31 120.3(3) . . ? C43 C42 C41 118.6(4) . . ? C25 C26 C21 120.2(3) . . ? C33 C32 C31 119.9(3) . . ? C41 C46 C45 119.7(4) . . ? C63 C64 C65 119.9(3) . . ? C63 C62 C61 119.5(3) . . ? C23 C24 C25 120.3(3) . . ? C56 C55 C54 119.6(3) . . ? C34 C35 C36 120.2(3) . . ? C43 C44 C45 120.3(3) . . ? C64 C65 C66 120.0(3) . . ? C64 C63 C62 120.7(3) . . ? C24 C25 C26 120.0(3) . . ? C23 C22 C21 119.4(3) . . ? C34 C33 C32 120.3(3) . . ? C53 C54 C55 120.7(3) . . ? C35 C34 C33 120.0(3) . . ? C24 C23 C22 120.5(3) . . ? C14 C15 C16 120.2(3) . . ? C54 C53 C52 120.0(3) . . ? C14 C13 C12 119.9(3) . . ? C15 C14 C13 120.5(3) . . ? C44 C45 C46 120.1(4) . . ? C44 C43 C42 120.9(4) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.509 _refine_diff_density_min -0.678 _refine_diff_density_rms 0.105 _database_code_depnum_ccdc_archive 'CCDC 898620' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_12008-cut #TrackingRef '13599_web_deposit_cif_file_2_DanielTofan_1346189895.MoP4_12008-cut.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C216 H460 Cl8 Mo4 N12 O56 P16' _chemical_formula_weight 5284.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.1845(16) _cell_length_b 23.687(3) _cell_length_c 23.769(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6860.1(15) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9815 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 24.87 _exptl_crystal_description Plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.279 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2832 _exptl_absorpt_coefficient_mu 0.420 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8500 _exptl_absorpt_correction_T_max 0.9793 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; 'Siemens three-circle diffractometer, Bruker APEX CCD' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 113188 _diffrn_reflns_av_R_equivalents 0.0607 _diffrn_reflns_av_sigmaI/netI 0.0323 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.03 _reflns_number_total 12130 _reflns_number_gt 10667 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2009.9.0 (Bruker-AXS, 2009)' _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2009)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0551P)^2^+20.0105P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(5) _refine_ls_number_reflns 12130 _refine_ls_number_parameters 810 _refine_ls_number_restraints 234 _refine_ls_R_factor_all 0.0726 _refine_ls_R_factor_gt 0.0617 _refine_ls_wR_factor_ref 0.1503 _refine_ls_wR_factor_gt 0.1425 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo -0.55332(5) 0.50327(2) 0.64583(2) 0.04688(16) Uani 1 1 d . . . P1 P -0.59513(12) 0.48867(5) 0.78217(6) 0.0312(3) Uani 1 1 d . . . P2 P -0.56407(10) 0.60468(5) 0.75295(5) 0.0243(3) Uani 1 1 d . . . P3 P -0.36347(12) 0.48540(6) 0.74735(8) 0.0458(4) Uani 1 1 d . . . P4 P -0.32725(10) 0.60429(6) 0.78535(6) 0.0292(3) Uani 1 1 d . . . O1P O -0.6249(3) 0.47121(15) 0.72360(15) 0.0330(8) Uani 1 1 d . A . O11 O -0.6470(4) 0.45982(16) 0.83013(16) 0.0440(10) Uani 1 1 d . A . O41 O -0.2746(3) 0.64908(16) 0.75231(17) 0.0366(8) Uani 1 1 d . A . O2P O -0.5276(4) 0.57956(15) 0.69816(16) 0.0458(11) Uani 1 1 d . A . O3P O -0.4074(4) 0.47180(17) 0.69042(19) 0.0510(11) Uani 1 1 d . A . O12 O -0.6214(3) 0.55520(15) 0.78833(16) 0.0389(9) Uani 1 1 d . A . O13 O -0.4652(3) 0.48658(15) 0.78979(16) 0.0401(9) Uani 1 1 d . A . O24 O -0.4571(3) 0.61444(15) 0.79087(17) 0.0383(9) Uani 1 1 d . A . O34 O -0.3177(3) 0.54756(16) 0.7486(2) 0.0498(11) Uani 1 1 d . A . O21 O -0.6314(3) 0.65432(16) 0.7566(2) 0.0463(11) Uani 1 1 d . A . O31 O -0.2827(5) 0.4464(2) 0.7725(3) 0.0804(18) Uani 1 1 d . A . O42 O -0.2872(3) 0.59039(18) 0.84265(18) 0.0469(10) Uani 1 1 d . A . C1S C -0.2686(7) 0.6377(4) 0.6239(3) 0.070(2) Uani 1 1 d . . . H1S1 H -0.2728 0.6459 0.6647 0.084 Uiso 1 1 calc R . . H1S2 H -0.3418 0.6246 0.6114 0.084 Uiso 1 1 calc RD . . Cl2 Cl -0.17280(18) 0.58481(10) 0.61235(8) 0.0754(6) Uani 1 1 d . . . Cl1 Cl -0.2336(3) 0.69874(13) 0.58779(11) 0.1195(11) Uani 1 1 d . . . N1 N -0.0709(3) 0.49366(19) 0.46094(16) 0.0321(9) Uani 1 1 d . . . C111 C -0.1449(5) 0.5255(2) 0.4218(2) 0.0393(13) Uani 1 1 d . . . H11A H -0.1923 0.4981 0.4018 0.047 Uiso 1 1 calc R . . H11B H -0.0992 0.5449 0.3932 0.047 Uiso 1 1 calc R . . C112 C -0.2175(5) 0.5691(3) 0.4507(3) 0.0498(16) Uani 1 1 d . . . H11C H -0.2617 0.5499 0.4800 0.060 Uiso 1 1 calc R . . H11D H -0.1702 0.5972 0.4696 0.060 Uiso 1 1 calc R . . C113 C -0.2946(6) 0.5998(3) 0.4106(3) 0.0573(18) Uani 1 1 d . . . H11E H -0.2507 0.6211 0.3827 0.069 Uiso 1 1 calc R . . H11F H -0.3393 0.5717 0.3899 0.069 Uiso 1 1 calc R . . C114 C -0.3706(6) 0.6403(3) 0.4411(4) 0.068(2) Uani 1 1 d . . . H11G H -0.4235 0.6189 0.4636 0.103 Uiso 1 1 calc R . . H11H H -0.4099 0.6635 0.4135 0.103 Uiso 1 1 calc R . . H11I H -0.3273 0.6648 0.4659 0.103 Uiso 1 1 calc R . . C121 C 0.0050(4) 0.5325(2) 0.4935(2) 0.0349(12) Uani 1 1 d . . . H12A H -0.0399 0.5547 0.5203 0.042 Uiso 1 1 calc R . . H12B H 0.0558 0.5089 0.5160 0.042 Uiso 1 1 calc R . . C122 C 0.0724(5) 0.5731(3) 0.4590(3) 0.0429(14) Uani 1 1 d . . . H12C H 0.0232 0.5972 0.4361 0.051 Uiso 1 1 calc R . . H12D H 0.1206 0.5518 0.4330 0.051 Uiso 1 1 calc R . . C123 C 0.1421(6) 0.6099(3) 0.4974(3) 0.0539(17) Uani 1 1 d . . . H12E H 0.0925 0.6328 0.5213 0.065 Uiso 1 1 calc R . . H12F H 0.1852 0.5851 0.5226 0.065 Uiso 1 1 calc R . . C124 C 0.2203(7) 0.6494(3) 0.4672(4) 0.071(2) Uani 1 1 d . . . H12G H 0.2656 0.6276 0.4409 0.106 Uiso 1 1 calc R . . H12H H 0.2676 0.6682 0.4948 0.106 Uiso 1 1 calc R . . H12I H 0.1782 0.6777 0.4464 0.106 Uiso 1 1 calc R . . C131 C -0.0046(5) 0.4532(2) 0.4240(2) 0.0363(13) Uani 1 1 d . . . H13A H -0.0560 0.4337 0.3983 0.044 Uiso 1 1 calc R . . H13B H 0.0460 0.4758 0.4005 0.044 Uiso 1 1 calc R . . C132 C 0.0625(5) 0.4085(2) 0.4546(2) 0.0370(12) Uani 1 1 d . . . H13C H 0.0129 0.3832 0.4758 0.044 Uiso 1 1 calc R . . H13D H 0.1127 0.4269 0.4817 0.044 Uiso 1 1 calc R . . C133 C 0.1288(5) 0.3743(3) 0.4122(3) 0.0439(14) Uani 1 1 d . . . H13E H 0.0782 0.3562 0.3850 0.053 Uiso 1 1 calc R . . H13F H 0.1778 0.3999 0.3909 0.053 Uiso 1 1 calc R . . C134 C 0.1963(6) 0.3298(3) 0.4404(3) 0.0540(17) Uani 1 1 d . . . H13G H 0.2477 0.3476 0.4666 0.081 Uiso 1 1 calc R . . H13H H 0.2375 0.3086 0.4119 0.081 Uiso 1 1 calc R . . H13I H 0.1480 0.3040 0.4610 0.081 Uiso 1 1 calc R . . C141 C -0.1356(5) 0.4608(2) 0.5051(2) 0.0362(13) Uani 1 1 d . . . H14A H -0.0832 0.4393 0.5287 0.043 Uiso 1 1 calc R . . H14B H -0.1736 0.4881 0.5299 0.043 Uiso 1 1 calc R . . C142 C -0.2193(5) 0.4203(2) 0.4818(3) 0.0421(14) Uani 1 1 d . . . H14C H -0.1860 0.3977 0.4512 0.050 Uiso 1 1 calc R . . H14D H -0.2819 0.4417 0.4659 0.050 Uiso 1 1 calc R . . C143 C -0.2600(5) 0.3812(3) 0.5284(3) 0.0504(16) Uani 1 1 d . . . H14E H -0.1977 0.3580 0.5418 0.061 Uiso 1 1 calc R . . H14F H -0.2856 0.4044 0.5604 0.061 Uiso 1 1 calc R . . C144 C -0.3511(6) 0.3428(3) 0.5105(4) 0.079(3) Uani 1 1 d . . . H14G H -0.4130 0.3653 0.4967 0.119 Uiso 1 1 calc R . . H14H H -0.3749 0.3199 0.5426 0.119 Uiso 1 1 calc R . . H14I H -0.3251 0.3179 0.4804 0.119 Uiso 1 1 calc R . . N2 N 0.4624(4) 0.4221(3) 0.2801(3) 0.073(2) Uani 1 1 d . . . C211 C 0.5376(6) 0.3781(4) 0.3075(4) 0.088(3) Uani 1 1 d . . . H21A H 0.5760 0.3574 0.2772 0.105 Uiso 1 1 calc R . . H21B H 0.5942 0.3984 0.3295 0.105 Uiso 1 1 calc R . . C212 C 0.4845(7) 0.3355(5) 0.3455(4) 0.100(3) Uani 1 1 d . . . H21C H 0.4195 0.3190 0.3267 0.119 Uiso 1 1 calc R . . H21D H 0.4598 0.3541 0.3806 0.119 Uiso 1 1 calc R . . C213 C 0.5681(9) 0.2879(6) 0.3599(6) 0.128(5) Uani 1 1 d . . . H21E H 0.5885 0.2682 0.3247 0.153 Uiso 1 1 calc R . . H21F H 0.6354 0.3054 0.3754 0.153 Uiso 1 1 calc R . . C214 C 0.5256(11) 0.2451(7) 0.4016(7) 0.152(6) Uani 1 1 d . . . H21G H 0.5059 0.2641 0.4367 0.228 Uiso 1 1 calc R . . H21H H 0.5826 0.2169 0.4090 0.228 Uiso 1 1 calc R . . H21I H 0.4606 0.2263 0.3860 0.228 Uiso 1 1 calc R . . C221 C 0.5351(6) 0.4612(4) 0.2448(4) 0.084(2) Uani 1 1 d U . . H22A H 0.5900 0.4789 0.2700 0.101 Uiso 1 1 calc R . . H22B H 0.5756 0.4380 0.2171 0.101 Uiso 1 1 calc R . . C222 C 0.4753(6) 0.5074(5) 0.2137(3) 0.093(3) Uani 1 1 d U . . H22C H 0.4179 0.4900 0.1898 0.111 Uiso 1 1 calc R . . H22D H 0.4381 0.5320 0.2415 0.111 Uiso 1 1 calc R . . C223 C 0.5460(10) 0.5428(4) 0.1779(6) 0.131(4) Uani 1 1 d U . . H22E H 0.6032 0.5600 0.2020 0.157 Uiso 1 1 calc R . . H22F H 0.5837 0.5179 0.1506 0.157 Uiso 1 1 calc R . . C224 C 0.4927(10) 0.5878(5) 0.1466(5) 0.120(4) Uani 1 1 d U . . H22G H 0.4695 0.5735 0.1098 0.181 Uiso 1 1 calc R . . H22H H 0.5442 0.6191 0.1414 0.181 Uiso 1 1 calc R . . H22I H 0.4283 0.6010 0.1675 0.181 Uiso 1 1 calc R . . C231 C 0.4007(6) 0.4558(4) 0.3241(3) 0.071(2) Uani 1 1 d . . . H23A H 0.3491 0.4814 0.3045 0.085 Uiso 1 1 calc R . . H23B H 0.3562 0.4293 0.3469 0.085 Uiso 1 1 calc R . . C232 C 0.4701(6) 0.4905(4) 0.3635(3) 0.090(3) Uani 1 1 d . . . H23C H 0.5114 0.5189 0.3415 0.108 Uiso 1 1 calc R . . H23D H 0.5241 0.4656 0.3823 0.108 Uiso 1 1 calc R . . C233 C 0.4009(7) 0.5203(4) 0.4079(3) 0.079(3) Uani 1 1 d . . . H23E H 0.4489 0.5463 0.4293 0.095 Uiso 1 1 calc R . . H23F H 0.3448 0.5435 0.3886 0.095 Uiso 1 1 calc R . . C234 C 0.3455(9) 0.4830(5) 0.4477(4) 0.101(4) Uani 1 1 d . . . H23G H 0.2850 0.4635 0.4286 0.152 Uiso 1 1 calc R . . H23H H 0.3163 0.5053 0.4790 0.152 Uiso 1 1 calc R . . H23I H 0.3978 0.4551 0.4621 0.152 Uiso 1 1 calc R . . C241 C 0.3786(5) 0.3921(4) 0.2434(3) 0.068(2) Uani 1 1 d . . . H24A H 0.3376 0.4209 0.2218 0.081 Uiso 1 1 calc R . . H24B H 0.3254 0.3727 0.2682 0.081 Uiso 1 1 calc R . . C242 C 0.4246(5) 0.3487(4) 0.2019(3) 0.069(2) Uani 1 1 d . . . H24C H 0.4891 0.3650 0.1824 0.082 Uiso 1 1 calc R . . H24D H 0.4492 0.3149 0.2228 0.082 Uiso 1 1 calc R . . C243 C 0.3395(6) 0.3318(3) 0.1589(3) 0.0555(17) Uani 1 1 d . . . H24E H 0.2715 0.3203 0.1786 0.067 Uiso 1 1 calc R . . H24F H 0.3219 0.3648 0.1350 0.067 Uiso 1 1 calc R . . C244 C 0.3772(7) 0.2841(3) 0.1221(3) 0.064(2) Uani 1 1 d . . . H24G H 0.4451 0.2950 0.1028 0.095 Uiso 1 1 calc R . . H24H H 0.3204 0.2755 0.0942 0.095 Uiso 1 1 calc R . . H24I H 0.3909 0.2506 0.1453 0.095 Uiso 1 1 calc R . . N3 N 0.0384(5) 0.70707(19) 0.2511(3) 0.0618(16) Uani 1 1 d . . . C311 C -0.0662(9) 0.6721(3) 0.2332(5) 0.112(4) Uani 1 1 d U . . H31A H -0.1068 0.6611 0.2676 0.134 Uiso 1 1 calc R . . H31B H -0.0417 0.6370 0.2145 0.134 Uiso 1 1 calc R . . C312 C -0.1482(10) 0.7045(5) 0.1922(6) 0.132(4) Uani 1 1 d U . . H31C H -0.1622 0.7427 0.2076 0.159 Uiso 1 1 calc R . . H31D H -0.1122 0.7092 0.1551 0.159 Uiso 1 1 calc R . . C313 C -0.2557(10) 0.6752(5) 0.1838(6) 0.117(4) Uani 1 1 d U . . H31E H -0.2997 0.6942 0.1543 0.140 Uiso 1 1 calc R . . H31F H -0.2446 0.6353 0.1730 0.140 Uiso 1 1 calc R . . C314 C -0.3101(11) 0.6795(5) 0.2392(6) 0.119(4) Uani 1 1 d U . . H31G H -0.2543 0.6833 0.2687 0.178 Uiso 1 1 calc R . . H31H H -0.3538 0.6455 0.2460 0.178 Uiso 1 1 calc R . . H31I H -0.3582 0.7127 0.2397 0.178 Uiso 1 1 calc R . . C321 C 0.0696(7) 0.7470(3) 0.2039(3) 0.067(2) Uani 1 1 d . . . H32A H 0.0054 0.7712 0.1954 0.080 Uiso 1 1 calc R . . H32B H 0.1290 0.7720 0.2175 0.080 Uiso 1 1 calc R . . C322 C 0.1067(8) 0.7198(3) 0.1505(4) 0.078(2) Uani 1 1 d . . . H32C H 0.0575 0.6880 0.1410 0.094 Uiso 1 1 calc R . . H32D H 0.1820 0.7048 0.1552 0.094 Uiso 1 1 calc R . . C323 C 0.1048(8) 0.7631(3) 0.1041(4) 0.084(3) Uani 1 1 d . . . H32E H 0.0288 0.7770 0.0992 0.101 Uiso 1 1 calc R . . H32F H 0.1512 0.7956 0.1151 0.101 Uiso 1 1 calc R . . C324 C 0.1452(9) 0.7399(4) 0.0493(4) 0.098(3) Uani 1 1 d . . . H32G H 0.2233 0.7307 0.0524 0.148 Uiso 1 1 calc R . . H32H H 0.1347 0.7681 0.0196 0.148 Uiso 1 1 calc R . . H32I H 0.1039 0.7057 0.0399 0.148 Uiso 1 1 calc R . . C331 C 0.0118(6) 0.7451(3) 0.3003(4) 0.064(2) Uani 1 1 d . . . H33A H -0.0497 0.7700 0.2892 0.077 Uiso 1 1 calc R . . H33B H 0.0763 0.7696 0.3074 0.077 Uiso 1 1 calc R . . C332 C -0.0187(6) 0.7161(3) 0.3549(4) 0.073(2) Uani 1 1 d . . . H33C H 0.0422 0.6913 0.3671 0.087 Uiso 1 1 calc R . . H33D H -0.0846 0.6923 0.3491 0.087 Uiso 1 1 calc R . . C333 C -0.0418(6) 0.7597(3) 0.4001(4) 0.081(3) Uani 1 1 d . . . H33E H -0.1035 0.7838 0.3874 0.097 Uiso 1 1 calc R . . H33F H 0.0235 0.7843 0.4041 0.097 Uiso 1 1 calc R . . C334 C -0.0701(8) 0.7353(4) 0.4576(5) 0.101(4) Uani 1 1 d . . . H33G H -0.1391 0.7142 0.4551 0.151 Uiso 1 1 calc R . . H33H H -0.0781 0.7660 0.4849 0.151 Uiso 1 1 calc R . . H33I H -0.0112 0.7099 0.4698 0.151 Uiso 1 1 calc R . . C341 C 0.1291(7) 0.6664(3) 0.2641(4) 0.066(2) Uani 1 1 d . . . H34A H 0.1033 0.6396 0.2932 0.080 Uiso 1 1 calc R . . H34B H 0.1457 0.6443 0.2297 0.080 Uiso 1 1 calc R . . C342 C 0.2318(7) 0.6935(3) 0.2840(4) 0.070(2) Uani 1 1 d . . . H34C H 0.2208 0.7105 0.3216 0.084 Uiso 1 1 calc R . . H34D H 0.2553 0.7234 0.2576 0.084 Uiso 1 1 calc R . . C343 C 0.3189(7) 0.6460(3) 0.2868(4) 0.076(2) Uani 1 1 d . . . H34E H 0.2924 0.6149 0.3112 0.091 Uiso 1 1 calc R . . H34F H 0.3323 0.6305 0.2487 0.091 Uiso 1 1 calc R . . C344 C 0.4203(8) 0.6695(5) 0.3097(6) 0.129(5) Uani 1 1 d . . . H34G H 0.4429 0.7020 0.2870 0.194 Uiso 1 1 calc R . . H34H H 0.4781 0.6407 0.3087 0.194 Uiso 1 1 calc R . . H34I H 0.4081 0.6815 0.3486 0.194 Uiso 1 1 calc R . . C1A C -0.6185(13) 0.5678(5) 0.5895(6) 0.042(3) Uani 0.521(8) 1 d PDU A 1 H1A1 H -0.593(3) 0.5477(18) 0.5568(14) 0.051 Uiso 0.521(8) 1 d PD A 1 H1A2 H -0.601(3) 0.6052(9) 0.599(2) 0.051 Uiso 0.521(8) 1 d PD A 1 C2A C -0.6976(14) 0.5364(7) 0.6272(7) 0.040(4) Uani 0.521(8) 1 d PDU A 1 H2A H -0.732(6) 0.553(4) 0.6588(19) 0.048 Uiso 0.521(8) 1 d PD A 1 C3A C -0.7124(11) 0.4824(7) 0.6114(5) 0.047(3) Uani 0.521(8) 1 d PDU A 1 H3A1 H -0.682(5) 0.461(2) 0.5802(18) 0.056 Uiso 0.521(8) 1 d PD A 1 H3A2 H -0.756(4) 0.4521(18) 0.627(2) 0.056 Uiso 0.521(8) 1 d PD A 1 C4A C -0.5358(12) 0.4313(4) 0.6045(5) 0.033(3) Uani 0.521(8) 1 d PU A 1 O4A O -0.5376(10) 0.3919(4) 0.5743(4) 0.059(3) Uani 0.521(8) 1 d PU A 1 C5A C -0.4438(11) 0.5159(6) 0.5823(6) 0.035(3) Uani 0.521(8) 1 d PU A 1 O5A O -0.3963(7) 0.5234(3) 0.5412(4) 0.053(3) Uani 0.521(8) 1 d PU A 1 C1B C -0.5632(13) 0.5752(6) 0.5799(6) 0.041(3) Uani 0.479(8) 1 d PDU A 2 H1B1 H -0.628(3) 0.563(5) 0.560(3) 0.049 Uiso 0.479(8) 1 d PD A 2 H1B2 H -0.587(7) 0.612(3) 0.589(3) 0.049 Uiso 0.479(8) 1 d PD A 2 C2B C -0.4655(14) 0.5478(8) 0.5892(6) 0.057(4) Uani 0.479(8) 1 d PDU A 2 H2B H -0.392(3) 0.5444(10) 0.604(3) 0.068 Uiso 0.479(8) 1 d PD A 2 C3B C -0.4559(16) 0.4896(9) 0.5719(7) 0.066(5) Uani 0.479(8) 1 d PDU A 2 H3B1 H -0.509(5) 0.468(2) 0.554(2) 0.079 Uiso 0.479(8) 1 d PD A 2 H3B2 H -0.396(4) 0.4665(19) 0.575(3) 0.079 Uiso 0.479(8) 1 d PD A 2 C4B C -0.6062(16) 0.4357(5) 0.6062(5) 0.045(4) Uani 0.479(8) 1 d PU A 2 O4B O -0.6300(19) 0.3986(5) 0.5761(6) 0.106(6) Uani 0.479(8) 1 d PU A 2 C5B C -0.7179(16) 0.5185(8) 0.6141(7) 0.031(3) Uani 0.479(8) 1 d PU A 2 O5B O -0.8054(7) 0.5191(4) 0.5966(4) 0.047(3) Uani 0.479(8) 1 d PU 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 0.0745(4) 0.0371(3) 0.0291(2) -0.0047(2) 0.0033(2) -0.0244(3) P1 0.0431(8) 0.0199(7) 0.0305(7) 0.0024(5) -0.0026(6) -0.0084(6) P2 0.0231(6) 0.0200(5) 0.0297(6) -0.0012(5) -0.0036(5) -0.0020(5) P3 0.0353(8) 0.0371(8) 0.0651(10) -0.0158(7) -0.0056(8) 0.0158(6) P4 0.0186(6) 0.0337(7) 0.0351(7) -0.0008(6) 0.0025(5) -0.0043(5) O1P 0.040(2) 0.0286(18) 0.0308(19) 0.0031(15) -0.0030(16) -0.0065(16) O11 0.064(3) 0.038(2) 0.030(2) 0.0042(16) 0.0012(19) -0.013(2) O41 0.0327(19) 0.035(2) 0.042(2) 0.0042(17) 0.0094(18) 0.0044(16) O2P 0.078(3) 0.0260(19) 0.034(2) -0.0013(16) 0.001(2) -0.005(2) O3P 0.053(3) 0.041(2) 0.059(3) -0.012(2) 0.007(2) 0.005(2) O12 0.053(2) 0.0252(19) 0.039(2) -0.0022(16) 0.0112(19) -0.0039(17) O13 0.042(2) 0.034(2) 0.044(2) 0.0111(16) -0.0098(18) -0.0072(17) O24 0.0222(18) 0.039(2) 0.054(2) -0.0096(17) 0.0007(18) -0.0004(17) O34 0.028(2) 0.031(2) 0.091(3) -0.003(2) 0.020(2) 0.0096(16) O21 0.0275(19) 0.026(2) 0.085(3) -0.002(2) -0.011(2) 0.0071(16) O31 0.062(3) 0.047(3) 0.132(5) -0.008(3) -0.018(3) 0.027(3) O42 0.033(2) 0.055(3) 0.053(3) 0.009(2) -0.0016(19) -0.0092(18) C1S 0.067(5) 0.093(6) 0.050(4) -0.016(4) -0.004(4) 0.035(5) Cl2 0.0793(13) 0.1030(16) 0.0438(9) -0.0203(10) -0.0094(9) 0.0497(12) Cl1 0.182(3) 0.105(2) 0.0719(15) 0.0246(14) 0.0229(18) 0.049(2) N1 0.032(2) 0.035(2) 0.030(2) -0.0008(19) 0.0002(17) -0.005(2) C111 0.039(3) 0.043(3) 0.037(3) 0.001(2) -0.009(3) -0.004(3) C112 0.044(4) 0.048(4) 0.057(4) 0.004(3) -0.013(3) 0.004(3) C113 0.047(4) 0.055(4) 0.070(5) 0.016(4) -0.022(3) -0.007(3) C114 0.054(4) 0.048(4) 0.104(6) 0.010(4) -0.019(4) 0.011(3) C121 0.030(3) 0.041(3) 0.034(3) -0.011(2) -0.001(2) -0.003(2) C122 0.044(4) 0.043(3) 0.041(3) -0.008(3) 0.008(3) -0.009(3) C123 0.047(4) 0.052(4) 0.062(4) -0.004(3) -0.016(3) -0.013(3) C124 0.058(5) 0.061(5) 0.093(6) -0.009(4) -0.003(4) -0.026(4) C131 0.038(3) 0.043(3) 0.028(3) -0.007(2) 0.003(2) -0.005(3) C132 0.040(3) 0.034(3) 0.037(3) -0.002(2) 0.002(3) 0.002(3) C133 0.043(3) 0.044(3) 0.044(3) -0.002(3) 0.007(3) -0.007(3) C134 0.051(4) 0.048(4) 0.063(4) 0.006(3) 0.004(3) 0.009(3) C141 0.039(3) 0.037(3) 0.033(3) 0.000(2) 0.009(2) -0.002(2) C142 0.037(3) 0.033(3) 0.056(4) -0.007(3) 0.004(3) -0.004(3) C143 0.049(4) 0.039(3) 0.064(4) -0.007(3) 0.016(3) -0.010(3) C144 0.054(5) 0.046(4) 0.138(8) -0.001(5) 0.017(5) -0.010(3) N2 0.027(3) 0.122(6) 0.070(4) -0.046(4) 0.011(3) -0.013(3) C211 0.028(4) 0.148(9) 0.088(6) -0.047(6) 0.013(4) -0.021(5) C212 0.041(4) 0.162(10) 0.096(7) -0.034(7) -0.002(5) -0.021(6) C213 0.061(6) 0.202(14) 0.120(9) 0.012(10) -0.023(7) -0.028(8) C214 0.103(10) 0.184(14) 0.170(14) -0.080(12) -0.007(9) -0.034(10) C221 0.042(4) 0.131(7) 0.080(5) -0.065(4) 0.026(4) -0.036(4) C222 0.049(4) 0.174(9) 0.055(4) -0.026(5) 0.011(3) -0.042(5) C223 0.129(9) 0.071(5) 0.193(11) -0.066(5) 0.103(8) -0.048(6) C224 0.146(10) 0.131(8) 0.084(7) -0.046(5) 0.046(6) -0.093(7) C231 0.037(4) 0.111(6) 0.066(5) -0.041(5) 0.011(3) -0.022(4) C232 0.056(5) 0.137(8) 0.077(5) -0.053(6) 0.010(4) -0.040(5) C233 0.067(5) 0.103(7) 0.068(5) -0.033(5) 0.011(4) -0.032(5) C234 0.117(8) 0.123(9) 0.064(5) -0.036(5) 0.007(5) -0.044(7) C241 0.027(3) 0.105(6) 0.072(5) -0.039(5) 0.017(3) -0.023(4) C242 0.032(4) 0.093(6) 0.080(5) -0.040(4) 0.013(3) -0.017(4) C243 0.057(4) 0.058(4) 0.052(4) -0.013(3) 0.005(3) 0.002(3) C244 0.081(5) 0.056(4) 0.054(4) -0.011(3) -0.003(4) 0.002(4) N3 0.061(4) 0.019(2) 0.106(5) -0.002(3) -0.017(4) -0.005(2) C311 0.121(8) 0.026(3) 0.190(11) -0.001(5) -0.056(8) -0.033(4) C312 0.121(8) 0.081(7) 0.195(12) 0.024(8) -0.058(7) -0.015(6) C313 0.112(8) 0.066(6) 0.173(10) -0.017(7) -0.036(7) -0.011(6) C314 0.137(9) 0.073(6) 0.147(9) -0.006(7) -0.058(7) -0.002(6) C321 0.076(5) 0.024(3) 0.101(6) 0.002(3) -0.026(5) -0.004(3) C322 0.096(6) 0.033(3) 0.105(7) -0.004(4) -0.020(5) -0.013(4) C323 0.095(7) 0.042(4) 0.116(8) -0.017(5) -0.016(6) -0.007(4) C324 0.105(8) 0.075(6) 0.116(8) -0.016(6) -0.002(7) -0.025(6) C331 0.042(4) 0.023(3) 0.128(7) -0.001(4) 0.006(4) -0.010(3) C332 0.056(4) 0.033(3) 0.129(7) 0.008(4) 0.011(5) 0.000(3) C333 0.043(4) 0.042(4) 0.158(9) -0.001(5) 0.023(5) 0.005(3) C334 0.070(6) 0.076(6) 0.156(10) 0.003(6) 0.052(7) 0.020(5) C341 0.079(5) 0.024(3) 0.096(6) 0.002(3) -0.008(5) 0.009(3) C342 0.082(6) 0.053(4) 0.076(5) 0.001(4) -0.017(4) 0.022(4) C343 0.064(5) 0.052(4) 0.111(7) -0.023(4) -0.012(5) -0.002(4) C344 0.055(6) 0.096(8) 0.236(16) -0.021(9) -0.011(8) 0.000(5) C1A 0.063(9) 0.023(6) 0.041(7) -0.017(5) -0.028(6) -0.001(6) C2A 0.049(8) 0.047(9) 0.023(8) -0.017(6) -0.014(5) 0.016(6) C3A 0.054(8) 0.054(8) 0.033(7) -0.009(7) 0.003(6) -0.010(7) C4A 0.046(7) 0.008(4) 0.046(7) 0.004(4) 0.023(6) 0.006(5) O4A 0.084(8) 0.026(4) 0.067(6) -0.012(4) 0.022(6) -0.003(5) C5A 0.040(7) 0.016(6) 0.050(8) -0.009(6) 0.010(6) -0.002(6) O5A 0.058(6) 0.034(4) 0.067(6) -0.005(4) 0.024(4) -0.012(4) C1B 0.039(7) 0.028(6) 0.054(8) -0.006(5) 0.001(7) -0.021(5) C2B 0.056(8) 0.059(9) 0.057(9) -0.018(8) 0.010(7) 0.004(7) C3B 0.055(9) 0.074(11) 0.069(10) -0.047(10) -0.023(8) 0.015(9) C4B 0.083(12) 0.026(6) 0.026(6) -0.007(5) -0.010(8) 0.028(8) O4B 0.195(18) 0.046(7) 0.076(9) -0.017(6) -0.019(11) -0.012(10) C5B 0.046(7) 0.032(10) 0.016(8) -0.016(7) 0.001(6) 0.008(8) O5B 0.037(5) 0.055(6) 0.049(5) 0.004(4) -0.009(4) -0.011(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C4B 1.965(14) . ? Mo1 C2A 1.975(16) . ? Mo1 C4A 1.979(11) . ? Mo1 C2B 2.016(16) . ? Mo1 C5A 2.038(13) . ? Mo1 C3B 2.144(19) . ? Mo1 C3A 2.162(14) . ? Mo1 C5B 2.17(2) . ? Mo1 C1A 2.181(13) . ? Mo1 O1P 2.181(4) . ? Mo1 O3P 2.200(5) . ? Mo1 O2P 2.216(4) . ? P1 O11 1.471(4) . ? P1 O1P 1.497(4) . ? P1 O13 1.595(4) . ? P1 O12 1.615(4) . ? P2 O21 1.436(4) . ? P2 O2P 1.499(4) . ? P2 O24 1.601(4) . ? P2 O12 1.603(4) . ? P3 O31 1.477(5) . ? P3 O3P 1.491(5) . ? P3 O34 1.575(4) . ? P3 O13 1.598(4) . ? P4 O41 1.468(4) . ? P4 O42 1.483(4) . ? P4 O24 1.606(4) . ? P4 O34 1.607(4) . ? C1S Cl2 1.734(7) . ? C1S Cl1 1.736(9) . ? N1 C111 1.499(7) . ? N1 C121 1.518(6) . ? N1 C141 1.526(7) . ? N1 C131 1.531(7) . ? C111 C112 1.524(9) . ? C112 C113 1.523(9) . ? C113 C114 1.517(11) . ? C121 C122 1.508(8) . ? C122 C123 1.522(8) . ? C123 C124 1.515(10) . ? C131 C132 1.521(8) . ? C132 C133 1.525(8) . ? C133 C134 1.496(9) . ? C141 C142 1.506(8) . ? C142 C143 1.526(9) . ? C143 C144 1.498(10) . ? N2 C231 1.516(9) . ? N2 C241 1.520(8) . ? N2 C221 1.532(11) . ? N2 C211 1.533(12) . ? C211 C212 1.501(13) . ? C212 C213 1.556(15) . ? C213 C214 1.510(18) . ? C221 C222 1.509(14) . ? C222 C223 1.472(13) . ? C223 C224 1.452(17) . ? C231 C232 1.506(9) . ? C232 C233 1.526(11) . ? C233 C234 1.459(12) . ? C241 C242 1.529(9) . ? C242 C243 1.510(9) . ? C243 C244 1.499(9) . ? N3 C341 1.499(9) . ? N3 C331 1.511(10) . ? N3 C321 1.517(10) . ? N3 C311 1.578(10) . ? C311 C312 1.593(14) . ? C312 C313 1.496(15) . ? C313 C314 1.479(17) . ? C321 C322 1.494(12) . ? C322 C323 1.506(12) . ? C323 C324 1.497(13) . ? C331 C332 1.517(11) . ? C332 C333 1.517(12) . ? C333 C334 1.525(13) . ? C341 C342 1.484(11) . ? C342 C343 1.549(10) . ? C343 C344 1.460(12) . ? C1A C2A 1.51(2) . ? C2A C3A 1.344(17) . ? C4A O4A 1.177(14) . ? C5A O5A 1.149(16) . ? C1B C2B 1.37(2) . ? C2B C3B 1.44(2) . ? C4B O4B 1.170(18) . ? C5B O5B 1.14(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4B Mo1 C2A 85.6(7) . . ? C4B Mo1 C4A 25.3(5) . . ? C2A Mo1 C4A 109.1(6) . . ? C4B Mo1 C2B 106.2(7) . . ? C2A Mo1 C2B 96.6(8) . . ? C4A Mo1 C2B 93.6(6) . . ? C4B Mo1 C5A 88.8(7) . . ? C2A Mo1 C5A 111.0(7) . . ? C4A Mo1 C5A 71.8(5) . . ? C2B Mo1 C5A 23.3(4) . . ? C4B Mo1 C3B 70.4(7) . . ? C2A Mo1 C3B 111.7(7) . . ? C4A Mo1 C3B 53.4(7) . . ? C2B Mo1 C3B 40.5(6) . . ? C5A Mo1 C3B 18.7(5) . . ? C4B Mo1 C3A 48.6(7) . . ? C2A Mo1 C3A 37.6(5) . . ? C4A Mo1 C3A 73.3(6) . . ? C2B Mo1 C3A 110.0(6) . . ? C5A Mo1 C3A 109.9(5) . . ? C3B Mo1 C3A 98.7(6) . . ? C4B Mo1 C5B 70.5(7) . . ? C2A Mo1 C5B 15.1(5) . . ? C4A Mo1 C5B 94.1(6) . . ? C2B Mo1 C5B 99.9(7) . . ? C5A Mo1 C5B 108.8(6) . . ? C3B Mo1 C5B 104.6(6) . . ? C3A Mo1 C5B 22.9(5) . . ? C4B Mo1 C1A 99.0(5) . . ? C2A Mo1 C1A 42.3(7) . . ? C4A Mo1 C1A 109.8(5) . . ? C2B Mo1 C1A 54.4(7) . . ? C5A Mo1 C1A 71.4(6) . . ? C3B Mo1 C1A 78.8(7) . . ? C3A Mo1 C1A 66.5(6) . . ? C5B Mo1 C1A 48.3(7) . . ? C4B Mo1 O1P 89.5(5) . . ? C2A Mo1 O1P 88.4(6) . . ? C4A Mo1 O1P 99.4(3) . . ? C2B Mo1 O1P 163.7(5) . . ? C5A Mo1 O1P 160.3(4) . . ? C3B Mo1 O1P 149.7(6) . . ? C3A Mo1 O1P 83.3(4) . . ? C5B Mo1 O1P 89.0(5) . . ? C1A Mo1 O1P 128.2(5) . . ? C4B Mo1 O3P 102.7(5) . . ? C2A Mo1 O3P 164.1(5) . . ? C4A Mo1 O3P 81.9(4) . . ? C2B Mo1 O3P 94.0(5) . . ? C5A Mo1 O3P 83.0(4) . . ? C3B Mo1 O3P 84.0(5) . . ? C3A Mo1 O3P 146.1(5) . . ? C5B Mo1 O3P 165.8(5) . . ? C1A Mo1 O3P 145.8(5) . . ? O1P Mo1 O3P 78.28(15) . . ? C4B Mo1 O2P 168.3(6) . . ? C2A Mo1 O2P 85.9(4) . . ? C4A Mo1 O2P 165.0(5) . . ? C2B Mo1 O2P 82.7(5) . . ? C5A Mo1 O2P 101.8(4) . . ? C3B Mo1 O2P 120.3(6) . . ? C3A Mo1 O2P 121.7(5) . . ? C5B Mo1 O2P 100.9(5) . . ? C1A Mo1 O2P 79.9(3) . . ? O1P Mo1 O2P 82.22(14) . . ? O3P Mo1 O2P 83.79(16) . . ? O11 P1 O1P 119.2(2) . . ? O11 P1 O13 108.9(2) . . ? O1P P1 O13 109.8(2) . . ? O11 P1 O12 107.3(2) . . ? O1P P1 O12 107.8(2) . . ? O13 P1 O12 102.5(2) . . ? O21 P2 O2P 123.1(3) . . ? O21 P2 O24 108.2(2) . . ? O2P P2 O24 107.8(2) . . ? O21 P2 O12 108.5(2) . . ? O2P P2 O12 107.1(2) . . ? O24 P2 O12 99.5(2) . . ? O31 P3 O3P 118.1(3) . . ? O31 P3 O34 110.0(3) . . ? O3P P3 O34 110.3(3) . . ? O31 P3 O13 105.8(3) . . ? O3P P3 O13 107.3(2) . . ? O34 P3 O13 104.3(2) . . ? O41 P4 O42 120.5(2) . . ? O41 P4 O24 111.5(2) . . ? O42 P4 O24 106.4(2) . . ? O41 P4 O34 106.4(2) . . ? O42 P4 O34 106.9(3) . . ? O24 P4 O34 103.9(2) . . ? P1 O1P Mo1 126.5(2) . . ? P2 O2P Mo1 140.3(3) . . ? P3 O3P Mo1 130.9(2) . . ? P2 O12 P1 125.4(3) . . ? P1 O13 P3 134.3(3) . . ? P2 O24 P4 137.3(3) . . ? P3 O34 P4 140.0(3) . . ? Cl2 C1S Cl1 111.0(5) . . ? C111 N1 C121 112.2(4) . . ? C111 N1 C141 111.9(4) . . ? C121 N1 C141 105.8(4) . . ? C111 N1 C131 106.0(4) . . ? C121 N1 C131 110.6(4) . . ? C141 N1 C131 110.3(4) . . ? N1 C111 C112 114.2(5) . . ? C113 C112 C111 113.7(6) . . ? C114 C113 C112 112.4(6) . . ? C122 C121 N1 116.1(4) . . ? C121 C122 C123 110.0(5) . . ? C124 C123 C122 114.8(6) . . ? C132 C131 N1 116.5(4) . . ? C131 C132 C133 109.8(5) . . ? C134 C133 C132 111.7(5) . . ? C142 C141 N1 114.9(5) . . ? C141 C142 C143 109.9(5) . . ? C144 C143 C142 113.8(7) . . ? C231 N2 C241 108.0(5) . . ? C231 N2 C221 110.2(6) . . ? C241 N2 C221 110.9(6) . . ? C231 N2 C211 111.2(7) . . ? C241 N2 C211 109.1(7) . . ? C221 N2 C211 107.4(6) . . ? C212 C211 N2 117.1(6) . . ? C211 C212 C213 109.7(8) . . ? C214 C213 C212 114.0(10) . . ? C222 C221 N2 115.4(6) . . ? C223 C222 C221 114.5(8) . . ? C224 C223 C222 116.8(10) . . ? C232 C231 N2 115.9(6) . . ? C231 C232 C233 111.9(6) . . ? C234 C233 C232 115.0(8) . . ? N2 C241 C242 116.0(5) . . ? C243 C242 C241 111.3(6) . . ? C244 C243 C242 112.6(6) . . ? C341 N3 C331 112.5(6) . . ? C341 N3 C321 111.6(6) . . ? C331 N3 C321 104.6(5) . . ? C341 N3 C311 108.3(5) . . ? C331 N3 C311 110.4(7) . . ? C321 N3 C311 109.3(6) . . ? N3 C311 C312 114.7(6) . . ? C313 C312 C311 114.1(9) . . ? C314 C313 C312 103.9(11) . . ? C322 C321 N3 115.8(5) . . ? C321 C322 C323 108.9(6) . . ? C324 C323 C322 112.5(7) . . ? N3 C331 C332 116.3(5) . . ? C331 C332 C333 110.0(6) . . ? C332 C333 C334 114.7(7) . . ? C342 C341 N3 114.2(5) . . ? C341 C342 C343 106.1(6) . . ? C344 C343 C342 108.6(7) . . ? C2A C1A Mo1 61.6(7) . . ? C3A C2A C1A 112.8(14) . . ? C3A C2A Mo1 78.8(9) . . ? C1A C2A Mo1 76.1(9) . . ? C2A C3A Mo1 63.7(9) . . ? O4A C4A Mo1 169.4(12) . . ? O5A C5A Mo1 169.3(12) . . ? C2B C1B Mo1 59.8(9) . . ? C1B C2B C3B 118.4(15) . . ? C1B C2B Mo1 84.1(9) . . ? C3B C2B Mo1 74.5(12) . . ? C2B C3B Mo1 65.0(9) . . ? O4B C4B Mo1 170.5(16) . . ? O5B C5B Mo1 171.1(16) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.248 _refine_diff_density_min -1.273 _refine_diff_density_rms 0.081 _database_code_depnum_ccdc_archive 'CCDC 898621' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_12063 #TrackingRef '13601_web_deposit_cif_file_4_DanielTofan_1346189895.VP3_12063.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H64 Cl4 F2 N2 O10 P7 V' _chemical_formula_weight 1588.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7925(12) _cell_length_b 13.5617(14) _cell_length_c 24.724(3) _cell_angle_alpha 83.503(2) _cell_angle_beta 84.906(2) _cell_angle_gamma 88.089(2) _cell_volume 3580.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9381 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 30.82 _exptl_crystal_description Plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.474 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 0.511 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8415 _exptl_absorpt_correction_T_max 0.9603 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; 'Siemens three-circle diffractometer, Bruker APEX CCD' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 103381 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0314 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 30.51 _reflns_number_total 21764 _reflns_number_gt 18176 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2011.4.0 (Bruker-AXS, 2011)' _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2011)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0611P)^2^+5.2781P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 21764 _refine_ls_number_parameters 924 _refine_ls_number_restraints 57 _refine_ls_R_factor_all 0.0592 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1344 _refine_ls_wR_factor_gt 0.1261 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.55790(4) 0.12702(3) 0.796709(16) 0.02695(9) Uani 1 1 d . . . O1 O 0.70330(17) 0.09881(15) 0.80416(7) 0.0342(4) Uani 1 1 d . . . F1 F 0.54498(15) 0.23203(12) 0.83319(6) 0.0343(3) Uani 1 1 d . . . F2 F 0.48910(16) 0.04709(12) 0.85078(6) 0.0360(3) Uani 1 1 d . . . O10 O 0.36843(14) 0.16406(11) 0.77715(6) 0.0216(3) Uani 1 1 d . . . O20 O 0.60062(14) 0.22174(11) 0.72794(7) 0.0229(3) Uani 1 1 d . . . O30 O 0.54613(14) 0.02688(11) 0.74571(6) 0.0199(3) Uani 1 1 d . . . P1 P 0.31640(5) 0.17183(4) 0.72250(2) 0.01789(10) Uani 1 1 d . . . P2 P 0.55121(5) 0.23113(4) 0.67196(2) 0.01836(10) Uani 1 1 d . . . P3 P 0.49730(5) 0.02930(3) 0.68980(2) 0.01457(9) Uani 1 1 d . . . O12 O 0.40215(14) 0.24817(10) 0.68078(6) 0.0205(3) Uani 1 1 d . . . O23 O 0.56178(13) 0.12114(10) 0.65180(6) 0.0168(3) Uani 1 1 d . . . O13 O 0.35522(13) 0.06928(10) 0.69579(6) 0.0179(3) Uani 1 1 d . . . O11 O 0.18465(15) 0.19393(13) 0.71727(8) 0.0298(4) Uani 1 1 d . . . O22 O 0.60286(16) 0.30394(11) 0.62853(7) 0.0279(3) Uani 1 1 d . . . O33 O 0.50783(15) -0.06092(10) 0.66274(6) 0.0209(3) Uani 1 1 d . . . P1C P -0.12046(4) -0.17918(3) 0.575657(19) 0.01149(9) Uani 1 1 d . . . P2C P -0.24639(4) -0.37262(3) 0.606947(19) 0.01172(9) Uani 1 1 d . . . P3C P 0.10880(4) -0.35670(3) 0.879845(19) 0.01196(9) Uani 1 1 d . . . P4C P -0.11973(4) -0.24527(3) 0.908925(18) 0.01078(8) Uani 1 1 d . . . N1C N -0.19084(15) -0.26782(11) 0.61165(7) 0.0147(3) Uani 1 1 d . . . N2C N -0.02858(15) -0.33957(11) 0.90595(7) 0.0147(3) Uani 1 1 d . . . C115 C 0.0346(2) 0.04238(14) 0.64348(8) 0.0194(4) Uani 1 1 d . . . H115 H 0.1044 0.0841 0.6359 0.023 Uiso 1 1 calc R . . C122 C 0.1044(2) -0.28095(16) 0.57163(9) 0.0216(4) Uani 1 1 d . . . H122 H 0.0837 -0.2984 0.6096 0.026 Uiso 1 1 calc R . . C153 C -0.3679(2) -0.39628(18) 0.45725(9) 0.0256(4) Uani 1 1 d . . . H153 H -0.4441 -0.3895 0.4405 0.031 Uiso 1 1 calc R . . C154 C -0.2568(2) -0.41125(19) 0.42617(9) 0.0279(5) Uani 1 1 d . . . H154 H -0.2568 -0.4127 0.3878 0.033 Uiso 1 1 calc R . . C152 C -0.36719(19) -0.39121(15) 0.51340(8) 0.0198(4) Uani 1 1 d . . . H152 H -0.4430 -0.3808 0.5349 0.024 Uiso 1 1 calc R . . C123 C 0.2145(2) -0.31719(17) 0.54665(10) 0.0254(4) Uani 1 1 d . . . H123 H 0.2687 -0.3594 0.5676 0.030 Uiso 1 1 calc R . . C116 C 0.01703(18) -0.03050(13) 0.60961(8) 0.0154(3) Uani 1 1 d . . . H116 H 0.0740 -0.0382 0.5787 0.018 Uiso 1 1 calc R . . C141 C -0.15320(18) -0.46839(13) 0.64132(8) 0.0156(3) Uani 1 1 d . . . C121 C 0.02401(17) -0.21882(13) 0.54103(8) 0.0145(3) Uani 1 1 d . . . C126 C 0.05694(19) -0.19190(15) 0.48556(8) 0.0188(4) Uani 1 1 d . . . H126 H 0.0041 -0.1483 0.4647 0.023 Uiso 1 1 calc R . . C124 C 0.2455(2) -0.29191(17) 0.49125(10) 0.0252(4) Uani 1 1 d . . . H124 H 0.3202 -0.3176 0.4742 0.030 Uiso 1 1 calc R . . C161 C -0.40265(17) -0.37647(13) 0.63881(7) 0.0128(3) Uani 1 1 d . . . C111 C -0.08555(17) -0.09242(12) 0.62152(7) 0.0123(3) Uani 1 1 d . . . C125 C 0.1672(2) -0.22890(17) 0.46078(9) 0.0246(4) Uani 1 1 d . . . H125 H 0.1889 -0.2110 0.4229 0.030 Uiso 1 1 calc R . . C166 C -0.46807(18) -0.28726(13) 0.64505(8) 0.0161(3) Uani 1 1 d . . . H166 H -0.4286 -0.2257 0.6343 0.019 Uiso 1 1 calc R . . C142 C -0.0711(2) -0.44243(15) 0.67791(9) 0.0209(4) Uani 1 1 d . . . H142 H -0.0660 -0.3752 0.6847 0.025 Uiso 1 1 calc R . . C162 C -0.46097(18) -0.46735(14) 0.65440(8) 0.0168(3) Uani 1 1 d . . . H162 H -0.4168 -0.5280 0.6499 0.020 Uiso 1 1 calc R . . C156 C -0.14412(19) -0.41923(15) 0.50626(9) 0.0202(4) Uani 1 1 d . . . H156 H -0.0679 -0.4279 0.5229 0.024 Uiso 1 1 calc R . . C144 C -0.0056(2) -0.61408(17) 0.69523(10) 0.0286(5) Uani 1 1 d . . . H144 H 0.0458 -0.6636 0.7129 0.034 Uiso 1 1 calc R . . C146 C -0.16278(19) -0.56775(14) 0.63256(9) 0.0191(4) Uani 1 1 d . . . H146 H -0.2188 -0.5858 0.6080 0.023 Uiso 1 1 calc R . . C155 C -0.1455(2) -0.42418(18) 0.45069(9) 0.0263(4) Uani 1 1 d . . . H155 H -0.0702 -0.4365 0.4293 0.032 Uiso 1 1 calc R . . C114 C -0.0493(2) 0.05421(14) 0.68826(8) 0.0201(4) Uani 1 1 d . . . H114 H -0.0374 0.1048 0.7108 0.024 Uiso 1 1 calc R . . C145 C -0.0895(2) -0.64015(15) 0.66010(10) 0.0249(4) Uani 1 1 d . . . H145 H -0.0971 -0.7079 0.6548 0.030 Uiso 1 1 calc R . . C165 C -0.59135(19) -0.28908(15) 0.66711(9) 0.0208(4) Uani 1 1 d . . . H165 H -0.6362 -0.2286 0.6714 0.025 Uiso 1 1 calc R . . C163 C -0.58411(19) -0.46799(15) 0.67653(9) 0.0205(4) Uani 1 1 d . . . H163 H -0.6241 -0.5293 0.6874 0.025 Uiso 1 1 calc R . . C164 C -0.64865(19) -0.37901(16) 0.68281(9) 0.0215(4) Uani 1 1 d . . . H164 H -0.7327 -0.3799 0.6980 0.026 Uiso 1 1 calc R . . C151 C -0.25500(18) -0.40137(13) 0.53802(8) 0.0148(3) Uani 1 1 d . . . C143 C 0.0030(2) -0.51543(17) 0.70437(10) 0.0277(5) Uani 1 1 d . . . H143 H 0.0597 -0.4977 0.7287 0.033 Uiso 1 1 calc R . . C112 C -0.16900(18) -0.08119(14) 0.66707(8) 0.0164(3) Uani 1 1 d . . . H112 H -0.2380 -0.1236 0.6753 0.020 Uiso 1 1 calc R . . C113 C -0.1508(2) -0.00770(15) 0.70040(8) 0.0200(4) Uani 1 1 d . . . H113 H -0.2074 0.0002 0.7314 0.024 Uiso 1 1 calc R . . C132 C -0.25864(19) -0.01690(15) 0.53256(9) 0.0207(4) Uani 1 1 d . . . H132 H -0.2394 0.0141 0.5633 0.025 Uiso 1 1 calc R . . C135 C -0.3185(2) -0.10808(17) 0.44310(9) 0.0249(4) Uani 1 1 d . . . H135 H -0.3396 -0.1393 0.4128 0.030 Uiso 1 1 calc R . . C136 C -0.2434(2) -0.15824(15) 0.48059(8) 0.0194(4) Uani 1 1 d . . . H136 H -0.2130 -0.2235 0.4758 0.023 Uiso 1 1 calc R . . C131 C -0.21259(17) -0.11251(14) 0.52556(8) 0.0151(3) Uani 1 1 d . . . C133 C -0.3331(2) 0.03295(17) 0.49429(10) 0.0281(5) Uani 1 1 d . . . H133 H -0.3634 0.0983 0.4988 0.034 Uiso 1 1 calc R . . C134 C -0.3629(2) -0.01264(18) 0.44976(10) 0.0281(5) Uani 1 1 d . . . H134 H -0.4136 0.0215 0.4239 0.034 Uiso 1 1 calc R . . C221 C 0.15601(17) -0.26732(13) 0.82324(8) 0.0140(3) Uani 1 1 d . . . C226 C 0.09987(18) -0.27035(14) 0.77448(8) 0.0171(3) Uani 1 1 d . . . H226 H 0.0484 -0.3241 0.7705 0.020 Uiso 1 1 calc R . . C261 C -0.04448(16) -0.12754(12) 0.89763(7) 0.0125(3) Uani 1 1 d . . . C211 C 0.22064(18) -0.35937(13) 0.92989(8) 0.0153(3) Uani 1 1 d . . . C262 C 0.03190(18) -0.10373(13) 0.93705(8) 0.0156(3) Uani 1 1 d . . . H262 H 0.0380 -0.1469 0.9698 0.019 Uiso 1 1 calc R . . C225 C 0.11935(19) -0.19510(15) 0.73201(8) 0.0191(4) Uani 1 1 d . . . H225 H 0.0801 -0.1967 0.6992 0.023 Uiso 1 1 calc R . . C222 C 0.23250(18) -0.18841(14) 0.82881(8) 0.0167(3) Uani 1 1 d . . . H222 H 0.2703 -0.1858 0.8619 0.020 Uiso 1 1 calc R . . C212 C 0.34900(19) -0.36327(15) 0.91435(9) 0.0208(4) Uani 1 1 d . . . H212 H 0.3782 -0.3592 0.8768 0.025 Uiso 1 1 calc R . . C251 C -0.23503(17) -0.24362(13) 0.86066(7) 0.0137(3) Uani 1 1 d . . . C242 C -0.22531(18) -0.34983(14) 1.00246(8) 0.0172(3) Uani 1 1 d . . . H242 H -0.1951 -0.4070 0.9861 0.021 Uiso 1 1 calc R . . C245 C -0.31360(18) -0.18218(15) 1.05088(8) 0.0180(4) Uani 1 1 d . . . H245 H -0.3431 -0.1253 1.0677 0.022 Uiso 1 1 calc R . . C263 C 0.09872(19) -0.01666(14) 0.92799(9) 0.0199(4) Uani 1 1 d . . . H263 H 0.1497 0.0002 0.9548 0.024 Uiso 1 1 calc R . . C231 C 0.11668(19) -0.47726(13) 0.85581(8) 0.0164(3) Uani 1 1 d . . . C246 C -0.24631(17) -0.17098(13) 0.99982(8) 0.0150(3) Uani 1 1 d . . . H246 H -0.2313 -0.1065 0.9815 0.018 Uiso 1 1 calc R . . C266 C -0.05317(19) -0.06391(14) 0.84943(8) 0.0170(3) Uani 1 1 d . . . H266 H -0.1054 -0.0796 0.8228 0.020 Uiso 1 1 calc R . . C224 C 0.19656(18) -0.11719(15) 0.73746(9) 0.0202(4) Uani 1 1 d . . . H224 H 0.2108 -0.0661 0.7081 0.024 Uiso 1 1 calc R . . C241 C -0.20093(16) -0.25507(13) 0.97570(7) 0.0125(3) Uani 1 1 d . . . C235 C 0.2246(2) -0.60111(15) 0.80520(9) 0.0249(4) Uani 1 1 d . . . H235 H 0.2925 -0.6200 0.7810 0.030 Uiso 1 1 calc R . . C223 C 0.25294(18) -0.11375(15) 0.78569(9) 0.0198(4) Uani 1 1 d . . . H223 H 0.3054 -0.0604 0.7892 0.024 Uiso 1 1 calc R . . C213 C 0.4331(2) -0.37314(16) 0.95424(11) 0.0269(5) Uani 1 1 d . . . H213 H 0.5200 -0.3751 0.9438 0.032 Uiso 1 1 calc R . . C233 C 0.0362(3) -0.64211(17) 0.86063(11) 0.0334(5) Uani 1 1 d . . . H233 H -0.0250 -0.6893 0.8746 0.040 Uiso 1 1 calc R . . C216 C 0.1787(2) -0.36463(15) 0.98515(8) 0.0192(4) Uani 1 1 d . . . H216 H 0.0920 -0.3611 0.9958 0.023 Uiso 1 1 calc R . . C236 C 0.2167(2) -0.50488(14) 0.82042(8) 0.0191(4) Uani 1 1 d . . . H236 H 0.2790 -0.4584 0.8068 0.023 Uiso 1 1 calc R . . C252 C -0.2248(2) -0.30813(15) 0.82047(9) 0.0204(4) Uani 1 1 d . . . H252 H -0.1592 -0.3565 0.8195 0.024 Uiso 1 1 calc R . . C254 C -0.4090(2) -0.23267(18) 0.78352(9) 0.0276(5) Uani 1 1 d . . . H254 H -0.4675 -0.2281 0.7567 0.033 Uiso 1 1 calc R . . C234 C 0.1347(3) -0.66884(15) 0.82500(9) 0.0291(5) Uani 1 1 d . . . H234 H 0.1403 -0.7340 0.8142 0.035 Uiso 1 1 calc R . . C214 C 0.3908(2) -0.38016(16) 1.00911(10) 0.0281(5) Uani 1 1 d . . . H214 H 0.4487 -0.3885 1.0362 0.034 Uiso 1 1 calc R . . C255 C -0.4215(2) -0.17072(17) 0.82456(9) 0.0241(4) Uani 1 1 d . . . H255 H -0.4901 -0.1251 0.8266 0.029 Uiso 1 1 calc R . . C256 C -0.33409(19) -0.17512(15) 0.86270(9) 0.0200(4) Uani 1 1 d . . . H256 H -0.3417 -0.1313 0.8903 0.024 Uiso 1 1 calc R . . C215 C 0.2641(2) -0.37499(17) 1.02465(9) 0.0262(4) Uani 1 1 d . . . H215 H 0.2356 -0.3785 1.0623 0.031 Uiso 1 1 calc R . . C243 C -0.2937(2) -0.36017(15) 1.05289(9) 0.0220(4) Uani 1 1 d . . . H243 H -0.3107 -0.4245 1.0709 0.026 Uiso 1 1 calc R . . C232 C 0.0266(2) -0.54605(15) 0.87603(10) 0.0255(4) Uani 1 1 d . . . H232 H -0.0414 -0.5277 0.9003 0.031 Uiso 1 1 calc R . . C253 C -0.3117(2) -0.30116(18) 0.78148(10) 0.0284(5) Uani 1 1 d . . . H253 H -0.3037 -0.3439 0.7534 0.034 Uiso 1 1 calc R . . C264 C 0.0911(2) 0.04576(15) 0.87973(9) 0.0235(4) Uani 1 1 d . . . H264 H 0.1381 0.1046 0.8734 0.028 Uiso 1 1 calc R . . C244 C -0.33750(19) -0.27640(16) 1.07717(8) 0.0212(4) Uani 1 1 d . . . H244 H -0.3839 -0.2838 1.1118 0.025 Uiso 1 1 calc R . . C265 C 0.0154(2) 0.02282(15) 0.84076(9) 0.0230(4) Uani 1 1 d . . . H265 H 0.0101 0.0662 0.8080 0.028 Uiso 1 1 calc R . . C1S C 0.6250(2) 0.12731(18) 0.95511(10) 0.0269(4) Uani 1 1 d D . . H1S1 H 0.5963 0.1959 0.9436 0.032 Uiso 1 1 calc R . . H1S2 H 0.5792 0.0816 0.9360 0.032 Uiso 1 1 calc R . . Cl1A Cl 0.59113(5) 0.10042(5) 1.02656(2) 0.03032(12) Uani 1 1 d D . . Cl1B Cl 0.78657(6) 0.11507(5) 0.93609(2) 0.03024(12) Uani 1 1 d D . . C2S C -0.3571(6) -0.5691(7) 0.7870(3) 0.0518(11) Uani 0.656(7) 1 d PDU A 1 H2S1 H -0.3891 -0.6297 0.7748 0.062 Uiso 0.656(7) 1 calc PR A 1 H2S2 H -0.3462 -0.5184 0.7549 0.062 Uiso 0.656(7) 1 calc PR A 1 Cl2A Cl -0.21941(12) -0.59512(15) 0.81303(10) 0.0605(6) Uani 0.656(7) 1 d PDU A 1 Cl2B Cl -0.46706(18) -0.52346(13) 0.83820(16) 0.0745(8) Uani 0.656(7) 1 d PDU A 1 C2P C -0.3982(10) -0.5682(14) 0.7908(6) 0.0518(11) Uani 0.344(7) 1 d PDU A 2 H2P1 H -0.4294 -0.6359 0.7904 0.062 Uiso 0.344(7) 1 calc PR A 2 H2P2 H -0.4331 -0.5249 0.7606 0.062 Uiso 0.344(7) 1 calc PR A 2 Cl2C Cl -0.2486(6) -0.5712(5) 0.7804(4) 0.107(3) Uani 0.344(7) 1 d PDU A 2 Cl2D Cl -0.4493(10) -0.5255(7) 0.8514(5) 0.157(4) Uani 0.344(7) 1 d PDU 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 V1 0.0354(2) 0.02969(19) 0.01738(17) -0.01024(14) -0.00452(15) 0.00772(15) O1 0.0299(9) 0.0508(11) 0.0256(9) -0.0170(8) -0.0114(7) 0.0119(8) F1 0.0392(8) 0.0385(8) 0.0276(7) -0.0179(6) 0.0020(6) -0.0008(6) F2 0.0531(10) 0.0365(8) 0.0178(6) -0.0042(5) 0.0001(6) 0.0037(7) O10 0.0209(7) 0.0231(7) 0.0205(7) -0.0067(5) 0.0041(6) 0.0013(5) O20 0.0199(7) 0.0248(7) 0.0258(8) -0.0107(6) -0.0002(6) -0.0028(5) O30 0.0236(7) 0.0212(7) 0.0151(6) -0.0032(5) -0.0039(5) 0.0047(5) P1 0.0148(2) 0.0153(2) 0.0236(3) -0.00462(17) 0.00115(18) 0.00051(16) P2 0.0200(2) 0.0143(2) 0.0210(2) -0.00449(17) 0.00131(19) -0.00328(17) P3 0.0177(2) 0.0123(2) 0.0141(2) -0.00326(15) -0.00213(17) 0.00251(16) O12 0.0217(7) 0.0139(6) 0.0256(7) -0.0020(5) -0.0011(6) 0.0004(5) O23 0.0198(7) 0.0138(6) 0.0169(6) -0.0028(5) -0.0006(5) -0.0012(5) O13 0.0167(6) 0.0144(6) 0.0230(7) -0.0044(5) -0.0013(5) 0.0008(5) O11 0.0171(7) 0.0277(8) 0.0462(10) -0.0121(7) -0.0028(7) 0.0056(6) O22 0.0349(9) 0.0173(7) 0.0302(9) -0.0025(6) 0.0066(7) -0.0076(6) O33 0.0282(8) 0.0120(6) 0.0232(7) -0.0045(5) -0.0044(6) 0.0035(5) P1C 0.0124(2) 0.01150(19) 0.0107(2) -0.00122(14) -0.00172(15) -0.00116(14) P2C 0.0127(2) 0.00983(18) 0.0130(2) -0.00234(14) -0.00190(16) 0.00022(14) P3C 0.0127(2) 0.01010(18) 0.0126(2) -0.00045(14) -0.00006(16) 0.00178(14) P4C 0.01095(19) 0.00994(18) 0.0116(2) -0.00129(14) -0.00212(15) 0.00065(14) N1C 0.0181(7) 0.0123(6) 0.0139(7) -0.0017(5) -0.0007(6) -0.0036(5) N2C 0.0136(7) 0.0117(6) 0.0181(7) -0.0003(5) 0.0003(6) 0.0013(5) C115 0.0253(10) 0.0160(8) 0.0176(9) 0.0014(6) -0.0072(7) -0.0062(7) C122 0.0197(9) 0.0282(10) 0.0169(9) -0.0024(7) -0.0026(7) 0.0043(7) C153 0.0235(10) 0.0353(11) 0.0207(10) -0.0105(8) -0.0079(8) 0.0008(8) C154 0.0301(12) 0.0379(12) 0.0179(10) -0.0128(8) -0.0053(8) 0.0061(9) C152 0.0169(9) 0.0245(9) 0.0192(9) -0.0067(7) -0.0034(7) 0.0001(7) C123 0.0198(10) 0.0297(11) 0.0271(11) -0.0061(8) -0.0046(8) 0.0074(8) C116 0.0184(9) 0.0150(8) 0.0129(8) 0.0005(6) -0.0032(7) -0.0038(6) C141 0.0160(8) 0.0122(7) 0.0187(9) -0.0018(6) -0.0031(7) 0.0016(6) C121 0.0149(8) 0.0154(8) 0.0138(8) -0.0041(6) -0.0009(6) -0.0007(6) C126 0.0203(9) 0.0209(9) 0.0150(9) -0.0017(7) 0.0004(7) -0.0009(7) C124 0.0204(10) 0.0309(11) 0.0260(11) -0.0143(8) 0.0023(8) 0.0033(8) C161 0.0129(8) 0.0121(7) 0.0135(8) -0.0021(6) -0.0020(6) -0.0003(6) C111 0.0138(8) 0.0109(7) 0.0125(8) -0.0010(6) -0.0036(6) 0.0008(6) C125 0.0252(11) 0.0322(11) 0.0165(9) -0.0078(8) 0.0040(8) -0.0007(8) C166 0.0162(8) 0.0128(8) 0.0200(9) -0.0042(6) -0.0017(7) 0.0004(6) C142 0.0238(10) 0.0157(8) 0.0246(10) -0.0016(7) -0.0103(8) 0.0004(7) C162 0.0177(9) 0.0136(8) 0.0188(9) -0.0007(6) -0.0012(7) -0.0017(6) C156 0.0188(9) 0.0223(9) 0.0206(9) -0.0077(7) -0.0034(7) 0.0050(7) C144 0.0305(12) 0.0233(10) 0.0321(12) 0.0003(8) -0.0107(9) 0.0107(8) C146 0.0201(9) 0.0146(8) 0.0236(10) -0.0047(7) -0.0051(7) 0.0027(7) C155 0.0247(11) 0.0357(12) 0.0198(10) -0.0123(8) 0.0001(8) 0.0065(8) C114 0.0281(10) 0.0154(8) 0.0191(9) -0.0057(7) -0.0105(8) 0.0024(7) C145 0.0303(11) 0.0143(8) 0.0302(11) -0.0033(7) -0.0054(9) 0.0070(7) C165 0.0171(9) 0.0213(9) 0.0248(10) -0.0084(7) -0.0001(7) 0.0035(7) C163 0.0196(9) 0.0218(9) 0.0198(9) -0.0001(7) -0.0012(7) -0.0072(7) C164 0.0142(9) 0.0295(10) 0.0212(10) -0.0052(8) 0.0007(7) -0.0024(7) C151 0.0165(8) 0.0140(8) 0.0148(8) -0.0049(6) -0.0030(7) 0.0009(6) C143 0.0278(11) 0.0248(10) 0.0319(12) -0.0006(8) -0.0155(9) 0.0035(8) C112 0.0146(8) 0.0195(8) 0.0159(8) -0.0048(6) -0.0010(7) 0.0007(6) C113 0.0218(9) 0.0228(9) 0.0165(9) -0.0072(7) -0.0033(7) 0.0047(7) C132 0.0199(9) 0.0209(9) 0.0222(10) -0.0029(7) -0.0080(8) 0.0030(7) C135 0.0266(11) 0.0320(11) 0.0166(9) 0.0029(8) -0.0095(8) -0.0074(8) C136 0.0226(10) 0.0208(9) 0.0151(9) 0.0007(7) -0.0053(7) -0.0042(7) C131 0.0137(8) 0.0174(8) 0.0140(8) 0.0005(6) -0.0035(6) -0.0017(6) C133 0.0264(11) 0.0259(10) 0.0325(12) 0.0000(9) -0.0128(9) 0.0069(8) C134 0.0233(11) 0.0353(12) 0.0253(11) 0.0054(9) -0.0121(9) -0.0014(9) C221 0.0127(8) 0.0131(7) 0.0150(8) 0.0005(6) 0.0011(6) 0.0025(6) C226 0.0177(9) 0.0168(8) 0.0162(9) -0.0011(6) -0.0004(7) 0.0016(6) C261 0.0127(8) 0.0104(7) 0.0145(8) -0.0012(6) -0.0021(6) 0.0010(6) C211 0.0160(8) 0.0109(7) 0.0186(9) 0.0004(6) -0.0027(7) 0.0008(6) C262 0.0166(8) 0.0147(8) 0.0156(8) 0.0004(6) -0.0046(7) -0.0011(6) C225 0.0187(9) 0.0223(9) 0.0152(9) 0.0022(7) -0.0017(7) 0.0029(7) C222 0.0146(8) 0.0168(8) 0.0179(9) 0.0020(6) -0.0018(7) 0.0002(6) C212 0.0158(9) 0.0198(9) 0.0261(10) -0.0008(7) -0.0022(7) 0.0032(7) C251 0.0134(8) 0.0150(8) 0.0127(8) -0.0002(6) -0.0025(6) -0.0013(6) C242 0.0183(9) 0.0135(8) 0.0187(9) 0.0008(6) -0.0009(7) 0.0025(6) C245 0.0150(8) 0.0225(9) 0.0172(9) -0.0050(7) -0.0008(7) 0.0012(7) C263 0.0206(9) 0.0171(8) 0.0230(10) -0.0013(7) -0.0068(8) -0.0047(7) C231 0.0220(9) 0.0122(7) 0.0149(8) -0.0017(6) -0.0009(7) 0.0029(6) C246 0.0163(8) 0.0129(7) 0.0161(8) -0.0025(6) -0.0017(7) -0.0004(6) C266 0.0211(9) 0.0148(8) 0.0155(8) 0.0001(6) -0.0054(7) -0.0015(6) C224 0.0158(9) 0.0208(9) 0.0209(9) 0.0076(7) 0.0015(7) 0.0019(7) C241 0.0110(7) 0.0136(7) 0.0133(8) -0.0010(6) -0.0029(6) 0.0007(6) C235 0.0416(13) 0.0174(9) 0.0147(9) -0.0034(7) 0.0005(8) 0.0107(8) C223 0.0152(9) 0.0181(8) 0.0243(10) 0.0055(7) -0.0008(7) -0.0020(6) C213 0.0167(9) 0.0226(10) 0.0417(13) 0.0003(9) -0.0101(9) 0.0023(7) C233 0.0466(15) 0.0159(9) 0.0370(13) -0.0051(9) 0.0060(11) -0.0068(9) C216 0.0205(9) 0.0184(8) 0.0185(9) 0.0012(7) -0.0040(7) -0.0005(7) C236 0.0263(10) 0.0166(8) 0.0137(8) -0.0012(6) 0.0003(7) 0.0046(7) C252 0.0215(10) 0.0215(9) 0.0200(9) -0.0074(7) -0.0050(7) 0.0000(7) C254 0.0247(11) 0.0367(12) 0.0227(10) 0.0005(9) -0.0123(9) -0.0054(9) C234 0.0529(15) 0.0129(8) 0.0213(10) -0.0042(7) -0.0016(10) 0.0043(9) C214 0.0283(11) 0.0221(10) 0.0353(12) 0.0022(8) -0.0180(10) -0.0021(8) C255 0.0190(10) 0.0280(10) 0.0249(10) 0.0027(8) -0.0084(8) 0.0024(8) C256 0.0182(9) 0.0228(9) 0.0198(9) -0.0040(7) -0.0060(7) 0.0039(7) C215 0.0316(12) 0.0269(10) 0.0207(10) 0.0018(8) -0.0097(9) -0.0034(8) C243 0.0209(10) 0.0209(9) 0.0213(10) 0.0074(7) 0.0016(8) 0.0015(7) C232 0.0306(11) 0.0164(9) 0.0287(11) -0.0059(8) 0.0077(9) -0.0037(8) C253 0.0320(12) 0.0341(12) 0.0225(11) -0.0113(9) -0.0090(9) -0.0040(9) C264 0.0274(11) 0.0152(8) 0.0275(11) 0.0032(7) -0.0050(8) -0.0072(7) C244 0.0176(9) 0.0293(10) 0.0152(9) 0.0015(7) 0.0009(7) 0.0023(7) C265 0.0307(11) 0.0159(8) 0.0216(10) 0.0054(7) -0.0053(8) -0.0046(7) C1S 0.0231(10) 0.0308(11) 0.0279(11) -0.0038(9) -0.0084(9) 0.0032(8) Cl1A 0.0267(3) 0.0363(3) 0.0285(3) -0.0065(2) -0.0034(2) 0.0034(2) Cl1B 0.0272(3) 0.0350(3) 0.0282(3) -0.0041(2) -0.0026(2) 0.0066(2) C2S 0.045(3) 0.055(2) 0.056(2) 0.0093(16) -0.022(3) -0.030(3) Cl2A 0.0239(6) 0.1062(13) 0.0533(11) -0.0201(9) -0.0027(5) 0.0067(6) Cl2B 0.0325(8) 0.0289(7) 0.149(2) 0.0097(9) 0.0369(9) 0.0061(5) C2P 0.045(3) 0.055(2) 0.056(2) 0.0093(16) -0.022(3) -0.030(3) Cl2C 0.086(3) 0.114(4) 0.128(6) -0.064(4) 0.016(4) 0.009(3) Cl2D 0.163(8) 0.124(6) 0.173(7) -0.043(5) 0.088(6) -0.019(5) _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 V1 O1 1.6243(18) . ? V1 F2 1.7501(16) . ? V1 F1 1.7651(15) . ? V1 O30 1.9693(15) . ? V1 O20 2.0394(17) . ? V1 O10 2.1725(16) . ? O10 P1 1.5001(17) . ? O20 P2 1.5175(17) . ? O30 P3 1.5191(15) . ? P1 O11 1.4574(17) . ? P1 O12 1.6264(16) . ? P1 O13 1.6327(15) . ? P2 O22 1.4592(16) . ? P2 O12 1.6166(16) . ? P2 O23 1.6227(14) . ? P3 O33 1.4559(14) . ? P3 O13 1.6092(15) . ? P3 O23 1.6110(14) . ? P1C N1C 1.5851(16) . ? P1C C111 1.7942(18) . ? P1C C131 1.8016(19) . ? P1C C121 1.8067(19) . ? P2C N1C 1.5811(16) . ? P2C C161 1.7966(19) . ? P2C C141 1.7988(19) . ? P2C C151 1.8016(19) . ? P3C N2C 1.5842(17) . ? P3C C221 1.7940(18) . ? P3C C231 1.7986(19) . ? P3C C211 1.800(2) . ? P4C N2C 1.5916(16) . ? P4C C241 1.7923(19) . ? P4C C251 1.7968(19) . ? P4C C261 1.7977(18) . ? C115 C114 1.387(3) . ? C115 C116 1.394(3) . ? C122 C123 1.391(3) . ? C122 C121 1.400(3) . ? C153 C154 1.388(3) . ? C153 C152 1.398(3) . ? C154 C155 1.390(3) . ? C152 C151 1.399(3) . ? C123 C124 1.388(3) . ? C116 C111 1.402(2) . ? C141 C146 1.397(3) . ? C141 C142 1.401(3) . ? C121 C126 1.396(3) . ? C126 C125 1.394(3) . ? C124 C125 1.390(3) . ? C161 C166 1.397(2) . ? C161 C162 1.402(2) . ? C111 C112 1.397(3) . ? C166 C165 1.392(3) . ? C142 C143 1.394(3) . ? C162 C163 1.392(3) . ? C156 C155 1.384(3) . ? C156 C151 1.401(3) . ? C144 C143 1.389(3) . ? C144 C145 1.390(3) . ? C146 C145 1.395(3) . ? C114 C113 1.393(3) . ? C165 C164 1.386(3) . ? C163 C164 1.390(3) . ? C112 C113 1.392(3) . ? C132 C131 1.397(3) . ? C132 C133 1.397(3) . ? C135 C134 1.387(3) . ? C135 C136 1.390(3) . ? C136 C131 1.402(3) . ? C133 C134 1.388(3) . ? C221 C222 1.399(3) . ? C221 C226 1.402(3) . ? C226 C225 1.386(3) . ? C261 C266 1.398(2) . ? C261 C262 1.402(3) . ? C211 C216 1.395(3) . ? C211 C212 1.405(3) . ? C262 C263 1.390(3) . ? C225 C224 1.393(3) . ? C222 C223 1.393(3) . ? C212 C213 1.391(3) . ? C251 C252 1.391(3) . ? C251 C256 1.394(3) . ? C242 C243 1.387(3) . ? C242 C241 1.399(2) . ? C245 C244 1.388(3) . ? C245 C246 1.395(3) . ? C263 C264 1.390(3) . ? C231 C232 1.391(3) . ? C231 C236 1.396(3) . ? C246 C241 1.400(2) . ? C266 C265 1.396(3) . ? C224 C223 1.392(3) . ? C235 C234 1.378(3) . ? C235 C236 1.396(3) . ? C213 C214 1.386(4) . ? C233 C234 1.385(4) . ? C233 C232 1.396(3) . ? C216 C215 1.395(3) . ? C252 C253 1.397(3) . ? C254 C253 1.381(3) . ? C254 C255 1.384(3) . ? C214 C215 1.389(3) . ? C255 C256 1.387(3) . ? C243 C244 1.394(3) . ? C264 C265 1.384(3) . ? C1S Cl1A 1.771(2) . ? C1S Cl1B 1.773(2) . ? C2S Cl2A 1.682(6) . ? C2S Cl2B 1.804(7) . ? C2P Cl2C 1.611(10) . ? C2P Cl2D 1.706(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 V1 F2 99.26(9) . . ? O1 V1 F1 98.16(9) . . ? F2 V1 F1 94.38(7) . . ? O1 V1 O30 92.38(8) . . ? F2 V1 O30 91.06(7) . . ? F1 V1 O30 167.19(7) . . ? O1 V1 O20 92.58(9) . . ? F2 V1 O20 167.63(8) . . ? F1 V1 O20 87.41(7) . . ? O30 V1 O20 84.86(6) . . ? O1 V1 O10 173.68(8) . . ? F2 V1 O10 85.27(7) . . ? F1 V1 O10 85.81(7) . . ? O30 V1 O10 83.09(6) . . ? O20 V1 O10 82.65(6) . . ? P1 O10 V1 128.41(9) . . ? P2 O20 V1 131.43(9) . . ? P3 O30 V1 133.82(9) . . ? O11 P1 O10 120.94(10) . . ? O11 P1 O12 110.82(10) . . ? O10 P1 O12 107.58(9) . . ? O11 P1 O13 109.15(9) . . ? O10 P1 O13 107.23(8) . . ? O12 P1 O13 98.82(8) . . ? O22 P2 O20 120.13(10) . . ? O22 P2 O12 109.59(9) . . ? O20 P2 O12 107.29(9) . . ? O22 P2 O23 109.95(9) . . ? O20 P2 O23 106.57(8) . . ? O12 P2 O23 101.71(8) . . ? O33 P3 O30 118.41(9) . . ? O33 P3 O13 111.04(8) . . ? O30 P3 O13 106.81(8) . . ? O33 P3 O23 111.38(8) . . ? O30 P3 O23 106.91(8) . . ? O13 P3 O23 100.71(8) . . ? P2 O12 P1 121.12(9) . . ? P3 O23 P2 119.62(9) . . ? P3 O13 P1 121.78(9) . . ? N1C P1C C111 106.73(8) . . ? N1C P1C C131 113.80(9) . . ? C111 P1C C131 106.78(8) . . ? N1C P1C C121 112.71(9) . . ? C111 P1C C121 108.26(9) . . ? C131 P1C C121 108.25(9) . . ? N1C P2C C161 108.99(8) . . ? N1C P2C C141 109.45(9) . . ? C161 P2C C141 109.25(9) . . ? N1C P2C C151 114.73(9) . . ? C161 P2C C151 106.50(9) . . ? C141 P2C C151 107.80(9) . . ? N2C P3C C221 114.26(8) . . ? N2C P3C C231 107.57(9) . . ? C221 P3C C231 107.89(9) . . ? N2C P3C C211 111.65(9) . . ? C221 P3C C211 108.61(9) . . ? C231 P3C C211 106.51(9) . . ? N2C P4C C241 107.72(8) . . ? N2C P4C C251 111.22(9) . . ? C241 P4C C251 107.06(8) . . ? N2C P4C C261 114.95(8) . . ? C241 P4C C261 107.93(8) . . ? C251 P4C C261 107.64(8) . . ? P2C N1C P1C 141.21(11) . . ? P3C N2C P4C 134.32(10) . . ? C114 C115 C116 120.29(18) . . ? C123 C122 C121 120.2(2) . . ? C154 C153 C152 119.6(2) . . ? C153 C154 C155 120.5(2) . . ? C153 C152 C151 120.10(19) . . ? C124 C123 C122 120.3(2) . . ? C115 C116 C111 119.43(18) . . ? C146 C141 C142 119.87(17) . . ? C146 C141 P2C 121.05(15) . . ? C142 C141 P2C 119.08(14) . . ? C126 C121 C122 119.30(18) . . ? C126 C121 P1C 123.05(15) . . ? C122 C121 P1C 117.64(15) . . ? C125 C126 C121 120.12(19) . . ? C123 C124 C125 119.9(2) . . ? C166 C161 C162 120.20(17) . . ? C166 C161 P2C 118.99(14) . . ? C162 C161 P2C 120.71(14) . . ? C112 C111 C116 120.15(17) . . ? C112 C111 P1C 118.60(14) . . ? C116 C111 P1C 121.00(14) . . ? C124 C125 C126 120.2(2) . . ? C165 C166 C161 119.66(17) . . ? C143 C142 C141 119.89(19) . . ? C163 C162 C161 119.49(18) . . ? C155 C156 C151 120.11(19) . . ? C143 C144 C145 119.8(2) . . ? C145 C146 C141 119.53(19) . . ? C156 C155 C154 120.1(2) . . ? C115 C114 C113 120.38(18) . . ? C144 C145 C146 120.60(19) . . ? C164 C165 C166 120.07(18) . . ? C164 C163 C162 120.07(18) . . ? C165 C164 C163 120.51(19) . . ? C152 C151 C156 119.48(18) . . ? C152 C151 P2C 121.06(15) . . ? C156 C151 P2C 118.72(15) . . ? C144 C143 C142 120.2(2) . . ? C113 C112 C111 119.86(18) . . ? C112 C113 C114 119.88(19) . . ? C131 C132 C133 119.8(2) . . ? C134 C135 C136 120.3(2) . . ? C135 C136 C131 120.0(2) . . ? C132 C131 C136 119.57(18) . . ? C132 C131 P1C 120.30(15) . . ? C136 C131 P1C 120.06(15) . . ? C134 C133 C132 120.3(2) . . ? C135 C134 C133 120.0(2) . . ? C222 C221 C226 119.82(17) . . ? C222 C221 P3C 121.99(15) . . ? C226 C221 P3C 117.60(14) . . ? C225 C226 C221 120.13(18) . . ? C266 C261 C262 120.03(16) . . ? C266 C261 P4C 121.85(14) . . ? C262 C261 P4C 117.95(13) . . ? C216 C211 C212 119.74(18) . . ? C216 C211 P3C 119.18(15) . . ? C212 C211 P3C 120.93(15) . . ? C263 C262 C261 119.70(17) . . ? C226 C225 C224 119.92(19) . . ? C223 C222 C221 119.71(18) . . ? C213 C212 C211 119.7(2) . . ? C252 C251 C256 119.70(18) . . ? C252 C251 P4C 120.76(15) . . ? C256 C251 P4C 119.52(14) . . ? C243 C242 C241 119.92(18) . . ? C244 C245 C246 120.07(18) . . ? C264 C263 C262 120.10(19) . . ? C232 C231 C236 119.76(18) . . ? C232 C231 P3C 119.21(15) . . ? C236 C231 P3C 120.85(15) . . ? C245 C246 C241 119.76(17) . . ? C265 C266 C261 119.54(18) . . ? C223 C224 C225 120.30(18) . . ? C242 C241 C246 119.86(17) . . ? C242 C241 P4C 118.38(14) . . ? C246 C241 P4C 121.65(14) . . ? C234 C235 C236 120.4(2) . . ? C224 C223 C222 120.10(19) . . ? C214 C213 C212 120.3(2) . . ? C234 C233 C232 120.2(2) . . ? C215 C216 C211 119.9(2) . . ? C235 C236 C231 119.7(2) . . ? C251 C252 C253 119.5(2) . . ? C253 C254 C255 120.0(2) . . ? C235 C234 C233 120.1(2) . . ? C213 C214 C215 120.2(2) . . ? C254 C255 C256 120.1(2) . . ? C255 C256 C251 120.18(19) . . ? C214 C215 C216 120.2(2) . . ? C242 C243 C244 120.18(18) . . ? C231 C232 C233 119.9(2) . . ? C254 C253 C252 120.5(2) . . ? C265 C264 C263 120.43(18) . . ? C245 C244 C243 120.20(19) . . ? C264 C265 C266 120.19(18) . . ? Cl1A C1S Cl1B 111.53(12) . . ? Cl2A C2S Cl2B 109.8(4) . . ? Cl2C C2P Cl2D 112.8(8) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.874 _refine_diff_density_min -1.671 _refine_diff_density_rms 0.088 _database_code_depnum_ccdc_archive 'CCDC 898623' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_12086 #TrackingRef '13602_web_deposit_cif_file_5_DanielTofan_1346189895.WP3_12086.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H60 Cl N2 O11 P7 W' _chemical_formula_weight 1565.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 23.8075(18) _cell_length_b 13.7219(11) _cell_length_c 22.0782(17) _cell_angle_alpha 90.00 _cell_angle_beta 113.0000(10) _cell_angle_gamma 90.00 _cell_volume 6639.2(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9330 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 30.96 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3160 _exptl_absorpt_coefficient_mu 2.013 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4998 _exptl_absorpt_correction_T_max 0.6330 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; 'Siemens three-circle diffractometer, Bruker APEX CCD' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 184026 _diffrn_reflns_av_R_equivalents 0.0455 _diffrn_reflns_av_sigmaI/netI 0.0242 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 30.51 _reflns_number_total 20238 _reflns_number_gt 18166 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2011.4.0 (Bruker-AXS, 2011)' _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2011)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0208P)^2^+5.0460P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20238 _refine_ls_number_parameters 884 _refine_ls_number_restraints 140 _refine_ls_R_factor_all 0.0270 _refine_ls_R_factor_gt 0.0221 _refine_ls_wR_factor_ref 0.0531 _refine_ls_wR_factor_gt 0.0511 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.254770(12) 0.656268(5) 0.188833(6) 0.01144(4) Uani 0.9543(11) 1 d PDU A 1 Cl1 Cl 0.17078(2) 0.54919(4) 0.15028(3) 0.01910(10) Uani 0.9543(11) 1 d PDU A 1 O1W O 0.31081(13) 0.56952(16) 0.2101(2) 0.0193(5) Uani 0.9543(11) 1 d PDU A 1 O3W O 0.25002(6) 0.68184(10) 0.26273(6) 0.0189(3) Uani 0.9543(11) 1 d PDU A 1 O2A O 0.31281(6) 0.76966(12) 0.19607(11) 0.0135(2) Uani 0.9543(11) 1 d PDU A 1 O3A O 0.18661(8) 0.76782(12) 0.14123(9) 0.0122(2) Uani 0.9543(11) 1 d PDU A 1 W2 W 0.2268(3) 0.65648(14) 0.1740(2) 0.0211(8) Uani 0.0457(11) 1 d PDU A 2 Cl2 Cl 0.3074(10) 0.5444(13) 0.2054(15) 0.023(4) Uani 0.0457(11) 1 d PDU A 2 O2W O 0.1661(12) 0.5799(19) 0.1382(17) 0.027(6) Uani 0.0457(11) 1 d PDU A 2 O4W O 0.2274(13) 0.677(2) 0.2499(9) 0.0189(3) Uani 0.0457(11) 1 d PDU A 2 O2B O 0.1784(17) 0.779(2) 0.133(2) 0.0122(2) Uani 0.0457(11) 1 d PDU A 2 O3B O 0.3013(14) 0.762(2) 0.195(3) 0.0135(2) Uani 0.0457(11) 1 d PDU A 2 O1 O 0.24967(5) 0.65422(8) 0.08761(5) 0.0139(2) Uani 1 1 d U . . P1 P 0.249793(17) 0.73479(3) 0.041190(18) 0.01183(7) Uani 1 1 d U A . P2 P 0.313482(17) 0.85369(3) 0.151254(19) 0.01246(7) Uani 1 1 d U . . P3 P 0.184594(17) 0.85213(3) 0.095951(18) 0.01096(7) Uani 1 1 d U . . O33 O 0.13426(5) 0.92154(9) 0.07607(5) 0.0174(2) Uani 1 1 d . A . O12 O 0.30682(5) 0.80520(8) 0.08254(5) 0.0137(2) Uani 1 1 d . A . O23 O 0.24926(5) 0.90902(8) 0.13086(5) 0.0123(2) Uani 1 1 d . A . O13 O 0.19315(5) 0.80642(8) 0.03269(5) 0.0126(2) Uani 1 1 d . A . O22 O 0.36440(5) 0.92189(9) 0.17551(6) 0.0208(2) Uani 1 1 d . A . O11 O 0.25033(6) 0.71156(9) -0.02304(5) 0.0196(2) Uani 1 1 d . . . P12 P 0.417899(17) 1.19324(3) -0.018917(18) 0.01053(7) Uani 1 1 d . . . P11 P 0.359213(16) 1.38006(3) 0.000363(18) 0.01006(7) Uani 1 1 d . . . P21 P 0.076844(16) 0.32280(3) 0.260378(18) 0.00974(7) Uani 1 1 d . . . P22 P 0.149169(16) 0.17077(3) 0.225283(18) 0.00935(7) Uani 1 1 d . . . N2 N 0.13160(6) 0.25434(9) 0.26428(6) 0.0122(2) Uani 1 1 d . . . N1 N 0.37664(6) 1.28628(10) -0.02924(6) 0.0146(2) Uani 1 1 d . . . C151 C 0.46243(7) 1.20332(11) -0.06844(7) 0.0135(3) Uani 1 1 d . . . C252 C 0.25402(7) 0.13080(12) 0.20285(8) 0.0163(3) Uani 1 1 d . . . H252 H 0.2404 0.0651 0.1971 0.020 Uiso 1 1 calc R . . C241 C 0.16140(6) 0.05602(10) 0.26777(7) 0.0106(3) Uani 1 1 d . . . C226 C 0.04458(7) 0.17500(12) 0.32593(8) 0.0166(3) Uani 1 1 d . . . H226 H 0.0724 0.1359 0.3153 0.020 Uiso 1 1 calc R . . C266 C 0.10767(7) 0.15736(11) 0.08871(7) 0.0149(3) Uani 1 1 d . . . H266 H 0.1479 0.1746 0.0936 0.018 Uiso 1 1 calc R . . C114 C 0.17565(8) 1.33346(13) 0.01790(9) 0.0214(3) Uani 1 1 d . . . H114 H 0.1374 1.3237 0.0212 0.026 Uiso 1 1 calc R . . C111 C 0.28684(6) 1.36231(11) 0.00653(7) 0.0114(3) Uani 1 1 d . . . C141 C 0.46889(7) 1.17342(11) 0.06544(7) 0.0122(3) Uani 1 1 d . . . C214 C 0.14909(7) 0.60698(12) 0.37294(8) 0.0194(3) Uani 1 1 d . . . H214 H 0.1632 0.6656 0.3969 0.023 Uiso 1 1 calc R . . C222 C -0.00708(7) 0.32842(12) 0.32020(8) 0.0162(3) Uani 1 1 d . . . H222 H -0.0138 0.3945 0.3063 0.019 Uiso 1 1 calc R . . C232 C 0.05029(7) 0.37556(11) 0.13138(7) 0.0141(3) Uani 1 1 d . . . H232 H 0.0933 0.3816 0.1451 0.017 Uiso 1 1 calc R . . C143 C 0.57012(7) 1.14964(12) 0.14916(8) 0.0187(3) Uani 1 1 d . . . H143 H 0.6126 1.1401 0.1612 0.022 Uiso 1 1 calc R . . C221 C 0.03413(6) 0.27101(11) 0.30434(7) 0.0122(3) Uani 1 1 d . . . C134 C 0.33758(7) 1.63421(13) -0.14132(9) 0.0202(3) Uani 1 1 d . . . H134 H 0.3320 1.6867 -0.1712 0.024 Uiso 1 1 calc R . . C122 C 0.39586(7) 1.43130(12) 0.13347(7) 0.0157(3) Uani 1 1 d . . . H122 H 0.3538 1.4315 0.1264 0.019 Uiso 1 1 calc R . . C261 C 0.09355(7) 0.14769(10) 0.14386(7) 0.0111(3) Uani 1 1 d . . . C121 C 0.41330(6) 1.41326(11) 0.08117(7) 0.0119(3) Uani 1 1 d . . . C164 C 0.29999(7) 0.92157(12) -0.09644(9) 0.0196(3) Uani 1 1 d . . . H164 H 0.2760 0.8650 -0.1135 0.024 Uiso 1 1 calc R . . C161 C 0.37147(7) 1.08649(11) -0.04705(7) 0.0128(3) Uani 1 1 d . . . C142 C 0.53168(7) 1.16001(11) 0.08311(8) 0.0151(3) Uani 1 1 d . . . H142 H 0.5480 1.1580 0.0501 0.018 Uiso 1 1 calc R . . C156 C 0.48264(8) 1.11971(12) -0.09011(8) 0.0184(3) Uani 1 1 d . . . H156 H 0.4727 1.0570 -0.0790 0.022 Uiso 1 1 calc R . . C152 C 0.47677(7) 1.29529(12) -0.08540(8) 0.0180(3) Uani 1 1 d . . . H152 H 0.4629 1.3522 -0.0710 0.022 Uiso 1 1 calc R . . C231 C 0.02524(7) 0.35054(11) 0.17701(7) 0.0119(3) Uani 1 1 d . . . C144 C 0.54647(8) 1.15318(12) 0.19744(8) 0.0200(3) Uani 1 1 d . . . H144 H 0.5730 1.1472 0.2424 0.024 Uiso 1 1 calc R . . C153 C 0.51147(8) 1.30343(14) -0.12339(9) 0.0229(3) Uani 1 1 d . . . H153 H 0.5213 1.3660 -0.1349 0.027 Uiso 1 1 calc R . . C251 C 0.21963(6) 0.20260(11) 0.21797(7) 0.0114(3) Uani 1 1 d . . . C132 C 0.36245(7) 1.57597(11) -0.03096(8) 0.0160(3) Uani 1 1 d . . . H132 H 0.3741 1.5888 0.0146 0.019 Uiso 1 1 calc R . . C242 C 0.15396(7) -0.03015(11) 0.23140(7) 0.0123(3) Uani 1 1 d . . . H242 H 0.1391 -0.0275 0.1848 0.015 Uiso 1 1 calc R . . C263 C -0.01031(7) 0.10658(12) 0.07406(8) 0.0192(3) Uani 1 1 d . . . H263 H -0.0506 0.0893 0.0689 0.023 Uiso 1 1 calc R . . C223 C -0.03796(7) 0.28853(14) 0.35620(8) 0.0199(3) Uani 1 1 d . . . H223 H -0.0665 0.3269 0.3661 0.024 Uiso 1 1 calc R . . C135 C 0.32865(7) 1.53904(13) -0.16437(8) 0.0189(3) Uani 1 1 d . . . H135 H 0.3173 1.5267 -0.2100 0.023 Uiso 1 1 calc R . . C211 C 0.10590(6) 0.43558(11) 0.30243(7) 0.0118(3) Uani 1 1 d . . . C154 C 0.53169(8) 1.22019(14) -0.14441(8) 0.0225(3) Uani 1 1 d . . . H154 H 0.5555 1.2259 -0.1702 0.027 Uiso 1 1 calc R . . C236 C -0.03825(7) 0.34258(12) 0.15627(8) 0.0158(3) Uani 1 1 d . . . H236 H -0.0557 0.3263 0.1870 0.019 Uiso 1 1 calc R . . C116 C 0.25604(7) 1.44097(11) 0.01980(7) 0.0137(3) Uani 1 1 d . . . H116 H 0.2732 1.5045 0.0252 0.016 Uiso 1 1 calc R . . C166 C 0.37644(7) 1.00663(12) -0.00639(8) 0.0157(3) Uani 1 1 d . . . H166 H 0.4043 1.0083 0.0383 0.019 Uiso 1 1 calc R . . C146 C 0.44521(7) 1.17563(12) 0.11425(8) 0.0161(3) Uani 1 1 d . . . H146 H 0.4026 1.1840 0.1024 0.019 Uiso 1 1 calc R . . C264 C 0.00396(8) 0.11687(12) 0.01909(8) 0.0198(3) Uani 1 1 d . . . H264 H -0.0267 0.1068 -0.0236 0.024 Uiso 1 1 calc R . . C225 C 0.01424(8) 0.13587(13) 0.36322(9) 0.0223(3) Uani 1 1 d . . . H225 H 0.0219 0.0706 0.3786 0.027 Uiso 1 1 calc R . . C235 C -0.07573(7) 0.35857(13) 0.09041(8) 0.0190(3) Uani 1 1 d . . . H235 H -0.1188 0.3531 0.0764 0.023 Uiso 1 1 calc R . . C255 C 0.29313(8) 0.32435(13) 0.21803(9) 0.0218(3) Uani 1 1 d . . . H255 H 0.3063 0.3903 0.2224 0.026 Uiso 1 1 calc R . . C265 C 0.06254(8) 0.14169(12) 0.02611(8) 0.0186(3) Uani 1 1 d . . . H265 H 0.0720 0.1481 -0.0117 0.022 Uiso 1 1 calc R . . C234 C -0.05060(8) 0.38234(13) 0.04535(8) 0.0197(3) Uani 1 1 d . . . H234 H -0.0763 0.3923 0.0004 0.024 Uiso 1 1 calc R . . C253 C 0.30792(8) 0.15544(13) 0.19623(9) 0.0209(3) Uani 1 1 d . . . H253 H 0.3313 0.1068 0.1862 0.025 Uiso 1 1 calc R . . C131 C 0.35309(6) 1.48028(11) -0.05395(7) 0.0119(3) Uani 1 1 d . . . C145 C 0.48384(8) 1.16557(12) 0.18014(8) 0.0192(3) Uani 1 1 d . . . H145 H 0.4677 1.1671 0.2133 0.023 Uiso 1 1 calc R . . C216 C 0.10097(8) 0.52342(12) 0.26952(8) 0.0183(3) Uani 1 1 d . . . H216 H 0.0826 0.5252 0.2228 0.022 Uiso 1 1 calc R . . C243 C 0.16834(7) -0.11949(11) 0.26358(7) 0.0131(3) Uani 1 1 d . . . H243 H 0.1643 -0.1778 0.2390 0.016 Uiso 1 1 calc R . . C126 C 0.47537(7) 1.41452(12) 0.09205(8) 0.0170(3) Uani 1 1 d . . . H126 H 0.4876 1.4041 0.0564 0.020 Uiso 1 1 calc R . . C125 C 0.51894(7) 1.43100(13) 0.15487(9) 0.0209(3) Uani 1 1 d . . . H125 H 0.5610 1.4307 0.1623 0.025 Uiso 1 1 calc R . . C244 C 0.18866(7) -0.12319(11) 0.33172(7) 0.0134(3) Uani 1 1 d . . . H244 H 0.1984 -0.1842 0.3537 0.016 Uiso 1 1 calc R . . C254 C 0.32740(8) 0.25224(14) 0.20445(9) 0.0238(4) Uani 1 1 d . . . H254 H 0.3646 0.2690 0.2007 0.029 Uiso 1 1 calc R . . C113 C 0.20636(8) 1.25485(13) 0.00590(8) 0.0208(3) Uani 1 1 d . . . H113 H 0.1896 1.1912 0.0021 0.025 Uiso 1 1 calc R . . C124 C 0.50127(7) 1.44793(13) 0.20686(8) 0.0197(3) Uani 1 1 d . . . H124 H 0.5313 1.4587 0.2498 0.024 Uiso 1 1 calc R . . C163 C 0.29429(8) 1.00160(13) -0.13703(9) 0.0245(4) Uani 1 1 d . . . H163 H 0.2662 0.9998 -0.1816 0.029 Uiso 1 1 calc R . . C115 C 0.20042(7) 1.42653(13) 0.02511(8) 0.0180(3) Uani 1 1 d . . . H115 H 0.1793 1.4801 0.0337 0.022 Uiso 1 1 calc R . . C165 C 0.34053(8) 0.92413(12) -0.03126(8) 0.0189(3) Uani 1 1 d . . . H165 H 0.3439 0.8697 -0.0035 0.023 Uiso 1 1 calc R . . C246 C 0.18199(6) 0.05181(11) 0.33651(7) 0.0123(3) Uani 1 1 d . . . H246 H 0.1872 0.1100 0.3615 0.015 Uiso 1 1 calc R . . C245 C 0.19472(7) -0.03819(12) 0.36773(7) 0.0140(3) Uani 1 1 d . . . H245 H 0.2077 -0.0416 0.4142 0.017 Uiso 1 1 calc R . . C233 C 0.01236(8) 0.39162(12) 0.06588(8) 0.0180(3) Uani 1 1 d . . . H233 H 0.0295 0.4090 0.0351 0.022 Uiso 1 1 calc R . . C136 C 0.33616(7) 1.46170(12) -0.12144(7) 0.0148(3) Uani 1 1 d . . . H136 H 0.3299 1.3967 -0.1375 0.018 Uiso 1 1 calc R . . C213 C 0.15476(8) 0.51935(13) 0.40612(8) 0.0236(4) Uani 1 1 d . . . H213 H 0.1732 0.5179 0.4528 0.028 Uiso 1 1 calc R . . C262 C 0.03422(7) 0.12160(12) 0.13650(8) 0.0153(3) Uani 1 1 d . . . H262 H 0.0246 0.1142 0.1742 0.018 Uiso 1 1 calc R . . C123 C 0.43997(7) 1.44910(13) 0.19626(8) 0.0191(3) Uani 1 1 d . . . H123 H 0.4280 1.4620 0.2318 0.023 Uiso 1 1 calc R . . C155 C 0.51725(8) 1.12857(14) -0.12790(8) 0.0225(3) Uani 1 1 d . . . H155 H 0.5311 1.0718 -0.1425 0.027 Uiso 1 1 calc R . . C224 C -0.02712(8) 0.19258(15) 0.37775(8) 0.0225(4) Uani 1 1 d . . . H224 H -0.0482 0.1656 0.4026 0.027 Uiso 1 1 calc R . . C133 C 0.35471(8) 1.65271(12) -0.07468(9) 0.0209(3) Uani 1 1 d . . . H133 H 0.3611 1.7179 -0.0589 0.025 Uiso 1 1 calc R . . C212 C 0.13348(8) 0.43394(13) 0.37123(8) 0.0218(3) Uani 1 1 d . . . H212 H 0.1376 0.3740 0.3941 0.026 Uiso 1 1 calc R . . C162 C 0.32956(8) 1.08410(12) -0.11262(8) 0.0213(3) Uani 1 1 d . . . H162 H 0.3253 1.1389 -0.1403 0.026 Uiso 1 1 calc R . . C256 C 0.23915(7) 0.29948(12) 0.22527(8) 0.0165(3) Uani 1 1 d . . . H256 H 0.2158 0.3484 0.2351 0.020 Uiso 1 1 calc R . . C112 C 0.26180(7) 1.26879(12) -0.00061(8) 0.0156(3) Uani 1 1 d . . . H112 H 0.2824 1.2151 -0.0098 0.019 Uiso 1 1 calc R . . C215 C 0.12293(8) 0.60906(12) 0.30497(9) 0.0224(3) Uani 1 1 d . . . H215 H 0.1199 0.6690 0.2823 0.027 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.01470(9) 0.00932(3) 0.00997(4) 0.00098(2) 0.00447(5) 0.00139(3) Cl1 0.02243(19) 0.0151(2) 0.0232(2) -0.00024(18) 0.01264(17) -0.00532(16) O1W 0.0213(7) 0.0117(12) 0.0221(9) 0.0022(11) 0.0054(6) 0.0040(8) O3W 0.0292(7) 0.0161(6) 0.0118(5) 0.0018(5) 0.0086(5) 0.0018(6) O2A 0.0122(7) 0.0126(6) 0.0118(5) -0.0012(4) 0.0006(6) 0.0004(5) O3A 0.0140(7) 0.0117(6) 0.0121(8) 0.0009(4) 0.0062(6) 0.0013(4) W2 0.023(2) 0.0223(9) 0.0211(11) 0.0035(6) 0.0120(14) 0.0021(8) Cl2 0.035(7) 0.010(7) 0.023(6) 0.001(6) 0.012(5) 0.011(6) O2W 0.036(9) 0.014(10) 0.035(15) 0.003(12) 0.018(11) -0.012(8) O4W 0.0292(7) 0.0161(6) 0.0118(5) 0.0018(5) 0.0086(5) 0.0018(6) O2B 0.0140(7) 0.0117(6) 0.0121(8) 0.0009(4) 0.0062(6) 0.0013(4) O3B 0.0122(7) 0.0126(6) 0.0118(5) -0.0012(4) 0.0006(6) 0.0004(5) O1 0.0191(5) 0.0099(5) 0.0147(5) -0.0025(4) 0.0089(4) -0.0006(4) P1 0.01475(16) 0.01158(17) 0.01044(16) -0.00202(13) 0.00632(14) -0.00043(13) P2 0.01045(16) 0.01098(17) 0.01411(17) -0.00249(13) 0.00280(14) -0.00059(13) P3 0.01051(15) 0.01205(17) 0.00977(15) -0.00048(13) 0.00337(13) 0.00149(13) O33 0.0144(5) 0.0189(6) 0.0174(5) 0.0006(4) 0.0045(4) 0.0060(4) O12 0.0136(5) 0.0131(5) 0.0165(5) -0.0024(4) 0.0080(4) -0.0018(4) O23 0.0125(5) 0.0102(5) 0.0130(5) -0.0015(4) 0.0039(4) 0.0006(4) O13 0.0130(5) 0.0149(5) 0.0088(4) -0.0015(4) 0.0031(4) 0.0011(4) O22 0.0144(5) 0.0170(6) 0.0276(6) -0.0053(5) 0.0046(5) -0.0047(4) O11 0.0280(6) 0.0207(6) 0.0138(5) -0.0042(4) 0.0121(5) 0.0003(5) P12 0.01278(16) 0.00853(16) 0.01064(16) -0.00010(12) 0.00495(13) 0.00125(13) P11 0.01074(15) 0.00889(16) 0.01070(15) -0.00044(12) 0.00437(13) 0.00061(12) P21 0.01064(15) 0.00881(16) 0.01036(15) 0.00029(12) 0.00473(13) 0.00054(12) P22 0.00999(15) 0.00859(16) 0.00957(15) -0.00026(12) 0.00391(13) 0.00021(12) N2 0.0129(5) 0.0119(6) 0.0119(5) -0.0011(4) 0.0049(5) 0.0020(4) N1 0.0179(6) 0.0116(6) 0.0137(6) -0.0002(5) 0.0056(5) 0.0045(5) C151 0.0156(6) 0.0135(7) 0.0119(6) 0.0008(5) 0.0060(5) 0.0019(5) C252 0.0173(7) 0.0121(7) 0.0227(7) 0.0005(6) 0.0112(6) 0.0004(5) C241 0.0111(6) 0.0104(6) 0.0110(6) 0.0002(5) 0.0051(5) -0.0001(5) C226 0.0161(7) 0.0158(7) 0.0177(7) 0.0014(6) 0.0064(6) -0.0006(5) C266 0.0143(6) 0.0169(7) 0.0128(6) 0.0001(5) 0.0047(5) 0.0001(5) C114 0.0162(7) 0.0276(9) 0.0226(8) 0.0008(7) 0.0100(6) -0.0037(6) C111 0.0114(6) 0.0126(7) 0.0095(6) 0.0004(5) 0.0034(5) 0.0000(5) C141 0.0143(6) 0.0096(6) 0.0118(6) 0.0002(5) 0.0040(5) 0.0005(5) C214 0.0207(7) 0.0154(8) 0.0227(8) -0.0072(6) 0.0091(6) -0.0047(6) C222 0.0151(7) 0.0198(8) 0.0142(7) 0.0000(6) 0.0062(6) 0.0021(6) C232 0.0151(6) 0.0124(7) 0.0152(7) 0.0007(5) 0.0065(6) 0.0021(5) C143 0.0146(7) 0.0170(8) 0.0209(8) -0.0011(6) 0.0032(6) 0.0012(6) C221 0.0120(6) 0.0137(7) 0.0114(6) 0.0005(5) 0.0051(5) -0.0015(5) C134 0.0177(7) 0.0196(8) 0.0258(8) 0.0112(6) 0.0112(7) 0.0031(6) C122 0.0134(6) 0.0190(8) 0.0138(7) -0.0002(6) 0.0045(6) -0.0011(5) C261 0.0128(6) 0.0087(6) 0.0107(6) -0.0001(5) 0.0033(5) 0.0005(5) C121 0.0107(6) 0.0103(6) 0.0134(6) -0.0008(5) 0.0032(5) 0.0005(5) C164 0.0178(7) 0.0159(8) 0.0270(8) -0.0076(6) 0.0108(7) -0.0048(6) C161 0.0143(6) 0.0102(7) 0.0141(6) -0.0014(5) 0.0059(5) 0.0002(5) C142 0.0157(7) 0.0135(7) 0.0167(7) -0.0010(5) 0.0069(6) 0.0006(5) C156 0.0268(8) 0.0144(7) 0.0168(7) 0.0024(6) 0.0116(6) 0.0056(6) C152 0.0222(7) 0.0146(7) 0.0202(7) -0.0002(6) 0.0116(6) -0.0002(6) C231 0.0132(6) 0.0101(6) 0.0119(6) -0.0006(5) 0.0044(5) 0.0010(5) C144 0.0218(8) 0.0179(8) 0.0143(7) 0.0007(6) 0.0006(6) 0.0020(6) C153 0.0242(8) 0.0224(9) 0.0261(8) 0.0059(7) 0.0142(7) -0.0001(7) C251 0.0109(6) 0.0126(7) 0.0109(6) 0.0001(5) 0.0044(5) -0.0002(5) C132 0.0182(7) 0.0128(7) 0.0189(7) -0.0003(6) 0.0092(6) 0.0004(5) C242 0.0148(6) 0.0122(7) 0.0109(6) 0.0000(5) 0.0059(5) -0.0004(5) C263 0.0138(7) 0.0200(8) 0.0207(8) -0.0024(6) 0.0034(6) -0.0032(6) C223 0.0126(7) 0.0332(10) 0.0148(7) -0.0022(6) 0.0063(6) 0.0002(6) C135 0.0153(7) 0.0247(9) 0.0168(7) 0.0063(6) 0.0066(6) 0.0011(6) C211 0.0124(6) 0.0103(7) 0.0132(6) -0.0017(5) 0.0056(5) -0.0003(5) C154 0.0214(8) 0.0318(10) 0.0188(7) 0.0077(7) 0.0128(7) 0.0077(7) C236 0.0148(7) 0.0187(8) 0.0142(7) -0.0008(6) 0.0059(6) 0.0015(6) C116 0.0138(6) 0.0139(7) 0.0128(6) 0.0000(5) 0.0045(5) 0.0005(5) C166 0.0195(7) 0.0144(7) 0.0137(6) 0.0000(5) 0.0071(6) -0.0015(6) C146 0.0155(7) 0.0179(8) 0.0152(7) 0.0007(6) 0.0063(6) 0.0021(5) C264 0.0195(7) 0.0186(8) 0.0154(7) -0.0020(6) 0.0004(6) 0.0001(6) C225 0.0225(8) 0.0218(8) 0.0226(8) 0.0057(6) 0.0089(7) -0.0049(6) C235 0.0149(7) 0.0231(8) 0.0161(7) -0.0016(6) 0.0028(6) 0.0044(6) C255 0.0222(8) 0.0157(8) 0.0327(9) -0.0023(7) 0.0162(7) -0.0052(6) C265 0.0211(7) 0.0224(8) 0.0108(6) -0.0001(6) 0.0045(6) 0.0012(6) C234 0.0212(8) 0.0228(8) 0.0121(7) 0.0005(6) 0.0031(6) 0.0076(6) C253 0.0192(7) 0.0181(8) 0.0313(9) 0.0018(7) 0.0165(7) 0.0024(6) C131 0.0119(6) 0.0116(7) 0.0143(6) 0.0020(5) 0.0074(5) 0.0014(5) C145 0.0233(8) 0.0215(8) 0.0129(7) 0.0011(6) 0.0072(6) 0.0031(6) C216 0.0268(8) 0.0128(7) 0.0151(7) 0.0001(6) 0.0079(6) -0.0017(6) C243 0.0147(6) 0.0097(6) 0.0157(7) -0.0006(5) 0.0068(6) -0.0001(5) C126 0.0149(7) 0.0173(8) 0.0201(7) -0.0040(6) 0.0083(6) -0.0011(5) C125 0.0111(6) 0.0219(8) 0.0266(8) -0.0033(7) 0.0041(6) -0.0004(6) C244 0.0127(6) 0.0123(7) 0.0153(7) 0.0033(5) 0.0058(5) 0.0001(5) C254 0.0189(8) 0.0227(9) 0.0351(10) 0.0006(7) 0.0162(7) -0.0033(6) C113 0.0208(7) 0.0205(8) 0.0219(8) -0.0025(6) 0.0093(6) -0.0090(6) C124 0.0164(7) 0.0205(8) 0.0160(7) -0.0006(6) -0.0003(6) -0.0021(6) C163 0.0266(8) 0.0196(8) 0.0192(8) -0.0042(6) 0.0001(7) -0.0014(7) C115 0.0154(7) 0.0222(8) 0.0181(7) 0.0003(6) 0.0085(6) 0.0034(6) C165 0.0255(8) 0.0149(7) 0.0206(7) -0.0003(6) 0.0137(7) -0.0044(6) C246 0.0126(6) 0.0128(7) 0.0113(6) -0.0016(5) 0.0042(5) -0.0005(5) C245 0.0140(6) 0.0176(7) 0.0100(6) 0.0017(5) 0.0041(5) -0.0007(5) C233 0.0235(8) 0.0184(8) 0.0144(7) 0.0018(6) 0.0097(6) 0.0050(6) C136 0.0140(6) 0.0153(7) 0.0153(7) 0.0011(5) 0.0058(6) 0.0001(5) C213 0.0322(9) 0.0189(8) 0.0147(7) -0.0041(6) 0.0038(7) -0.0043(7) C262 0.0143(7) 0.0162(7) 0.0159(7) -0.0008(6) 0.0064(6) -0.0020(5) C123 0.0191(7) 0.0243(8) 0.0124(7) -0.0017(6) 0.0044(6) -0.0028(6) C155 0.0289(9) 0.0252(9) 0.0175(7) 0.0036(6) 0.0136(7) 0.0121(7) C224 0.0176(7) 0.0361(10) 0.0150(7) 0.0028(7) 0.0077(6) -0.0086(7) C133 0.0249(8) 0.0115(7) 0.0307(9) 0.0027(6) 0.0156(7) 0.0016(6) C212 0.0309(9) 0.0151(8) 0.0143(7) 0.0011(6) 0.0033(7) -0.0018(6) C162 0.0279(8) 0.0143(8) 0.0155(7) 0.0003(6) 0.0017(6) -0.0014(6) C256 0.0169(7) 0.0130(7) 0.0216(7) -0.0023(6) 0.0096(6) -0.0012(5) C112 0.0189(7) 0.0133(7) 0.0162(7) -0.0022(5) 0.0084(6) -0.0028(5) C215 0.0324(9) 0.0106(7) 0.0233(8) -0.0005(6) 0.0100(7) -0.0037(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 O1W 1.711(2) . ? W1 O3W 1.7151(12) . ? W1 O2A 2.0453(13) . ? W1 O3A 2.1790(12) . ? W1 O1 2.1904(11) . ? W1 Cl1 2.3562(6) . ? O2A P2 1.5236(19) . ? O3A P3 1.5173(16) . ? W2 O4W 1.694(16) . ? W2 O2W 1.710(16) . ? W2 O2B 2.045(16) . ? W2 O1 2.179(2) . ? W2 O3B 2.195(16) . ? W2 Cl2 2.343(15) . ? O2B P3 1.33(4) . ? O3B P2 1.67(4) . ? O1 P1 1.5084(11) . ? P1 O11 1.4583(12) . ? P1 O13 1.6193(11) . ? P1 O12 1.6252(11) . ? P2 O22 1.4577(12) . ? P2 O23 1.6058(11) . ? P2 O12 1.6066(11) . ? P3 O33 1.4577(11) . ? P3 O13 1.6148(11) . ? P3 O23 1.6268(11) . ? P12 N1 1.5722(13) . ? P12 C161 1.7934(15) . ? P12 C151 1.8011(16) . ? P12 C141 1.8027(15) . ? P11 N1 1.5708(13) . ? P11 C131 1.7927(15) . ? P11 C111 1.7972(15) . ? P11 C121 1.8037(15) . ? P21 N2 1.5817(13) . ? P21 C211 1.7982(15) . ? P21 C221 1.8034(15) . ? P21 C231 1.8097(15) . ? P22 N2 1.5851(13) . ? P22 C261 1.7959(14) . ? P22 C241 1.7974(15) . ? P22 C251 1.8007(15) . ? C151 C152 1.396(2) . ? C151 C156 1.399(2) . ? C252 C253 1.389(2) . ? C252 C251 1.402(2) . ? C241 C242 1.401(2) . ? C241 C246 1.4019(19) . ? C226 C221 1.390(2) . ? C226 C225 1.398(2) . ? C266 C261 1.390(2) . ? C266 C265 1.396(2) . ? C114 C113 1.386(3) . ? C114 C115 1.390(2) . ? C111 C112 1.398(2) . ? C111 C116 1.399(2) . ? C141 C146 1.398(2) . ? C141 C142 1.402(2) . ? C214 C215 1.382(2) . ? C214 C213 1.387(2) . ? C222 C223 1.389(2) . ? C222 C221 1.405(2) . ? C232 C233 1.391(2) . ? C232 C231 1.399(2) . ? C143 C144 1.387(2) . ? C143 C142 1.393(2) . ? C134 C135 1.387(3) . ? C134 C133 1.388(3) . ? C122 C121 1.394(2) . ? C122 C123 1.395(2) . ? C261 C262 1.404(2) . ? C121 C126 1.401(2) . ? C164 C165 1.385(2) . ? C164 C163 1.390(3) . ? C161 C166 1.392(2) . ? C161 C162 1.401(2) . ? C156 C155 1.388(2) . ? C152 C153 1.393(2) . ? C231 C236 1.402(2) . ? C144 C145 1.398(2) . ? C153 C154 1.388(3) . ? C251 C256 1.397(2) . ? C132 C133 1.391(2) . ? C132 C131 1.394(2) . ? C242 C243 1.391(2) . ? C263 C262 1.387(2) . ? C263 C264 1.390(2) . ? C223 C224 1.390(3) . ? C135 C136 1.387(2) . ? C211 C216 1.389(2) . ? C211 C212 1.400(2) . ? C154 C155 1.389(3) . ? C236 C235 1.395(2) . ? C116 C115 1.389(2) . ? C166 C165 1.395(2) . ? C146 C145 1.391(2) . ? C264 C265 1.384(2) . ? C225 C224 1.387(3) . ? C235 C234 1.385(2) . ? C255 C254 1.388(2) . ? C255 C256 1.398(2) . ? C234 C233 1.392(2) . ? C253 C254 1.395(2) . ? C131 C136 1.407(2) . ? C216 C215 1.395(2) . ? C243 C244 1.390(2) . ? C126 C125 1.388(2) . ? C125 C124 1.388(2) . ? C244 C245 1.387(2) . ? C113 C112 1.396(2) . ? C124 C123 1.385(2) . ? C163 C162 1.387(2) . ? C246 C245 1.389(2) . ? C213 C212 1.385(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1W W1 O3W 102.41(15) . . ? O1W W1 O2A 94.44(10) . . ? O3W W1 O2A 93.65(8) . . ? O1W W1 O3A 167.17(15) . . ? O3W W1 O3A 90.10(7) . . ? O2A W1 O3A 81.74(6) . . ? O1W W1 O1 89.89(14) . . ? O3W W1 O1 167.20(5) . . ? O2A W1 O1 81.72(7) . . ? O3A W1 O1 77.46(7) . . ? O1W W1 Cl1 97.23(9) . . ? O3W W1 Cl1 96.27(5) . . ? O2A W1 Cl1 162.68(6) . . ? O3A W1 Cl1 84.08(5) . . ? O1 W1 Cl1 85.55(3) . . ? P2 O2A W1 134.68(11) . . ? P3 O3A W1 132.79(12) . . ? O4W W2 O2W 103.7(14) . . ? O4W W2 O2B 95.4(15) . . ? O2W W2 O2B 94.2(13) . . ? O4W W2 O1 163.9(10) . . ? O2W W2 O1 92.4(13) . . ? O2B W2 O1 84.9(15) . . ? O4W W2 O3B 89.7(14) . . ? O2W W2 O3B 165.7(18) . . ? O2B W2 O3B 79.5(12) . . ? O1 W2 O3B 74.4(14) . . ? O4W W2 Cl2 97.2(11) . . ? O2W W2 Cl2 100.3(11) . . ? O2B W2 Cl2 157.9(15) . . ? O1 W2 Cl2 78.0(8) . . ? O3B W2 Cl2 82.5(11) . . ? P3 O2B W2 136(3) . . ? P2 O3B W2 133(3) . . ? P1 O1 W2 130.68(9) . . ? P1 O1 W1 132.05(6) . . ? W2 O1 W1 16.24(17) . . ? O11 P1 O1 120.23(7) . . ? O11 P1 O13 110.08(6) . . ? O1 P1 O13 107.52(6) . . ? O11 P1 O12 110.70(7) . . ? O1 P1 O12 106.08(6) . . ? O13 P1 O12 100.33(6) . . ? O22 P2 O2A 117.75(8) . . ? O22 P2 O23 111.32(7) . . ? O2A P2 O23 106.83(7) . . ? O22 P2 O12 111.95(7) . . ? O2A P2 O12 106.11(9) . . ? O23 P2 O12 101.48(6) . . ? O22 P2 O3B 125.3(13) . . ? O2A P2 O3B 8.6(12) . . ? O23 P2 O3B 99.1(13) . . ? O12 P2 O3B 104.6(17) . . ? O2B P3 O33 113.6(16) . . ? O2B P3 O3A 7.6(16) . . ? O33 P3 O3A 120.48(9) . . ? O2B P3 O13 108(2) . . ? O33 P3 O13 111.10(6) . . ? O3A P3 O13 106.94(9) . . ? O2B P3 O23 112.4(17) . . ? O33 P3 O23 110.09(6) . . ? O3A P3 O23 105.86(8) . . ? O13 P3 O23 100.38(6) . . ? P2 O12 P1 121.96(7) . . ? P2 O23 P3 121.81(7) . . ? P3 O13 P1 121.09(6) . . ? N1 P12 C161 110.33(7) . . ? N1 P12 C151 109.40(7) . . ? C161 P12 C151 106.37(7) . . ? N1 P12 C141 113.74(7) . . ? C161 P12 C141 108.04(7) . . ? C151 P12 C141 108.68(7) . . ? N1 P11 C131 108.41(7) . . ? N1 P11 C111 109.72(7) . . ? C131 P11 C111 108.96(7) . . ? N1 P11 C121 114.58(7) . . ? C131 P11 C121 107.93(7) . . ? C111 P11 C121 107.12(7) . . ? N2 P21 C211 109.90(7) . . ? N2 P21 C221 111.26(7) . . ? C211 P21 C221 104.20(7) . . ? N2 P21 C231 113.44(7) . . ? C211 P21 C231 108.39(7) . . ? C221 P21 C231 109.20(7) . . ? N2 P22 C261 115.05(7) . . ? N2 P22 C241 111.94(7) . . ? C261 P22 C241 105.88(7) . . ? N2 P22 C251 109.03(7) . . ? C261 P22 C251 107.54(7) . . ? C241 P22 C251 107.02(7) . . ? P21 N2 P22 141.90(8) . . ? P11 N1 P12 148.94(9) . . ? C152 C151 C156 119.78(15) . . ? C152 C151 P12 119.73(12) . . ? C156 C151 P12 120.49(12) . . ? C253 C252 C251 120.23(15) . . ? C242 C241 C246 119.88(13) . . ? C242 C241 P22 118.80(11) . . ? C246 C241 P22 121.19(11) . . ? C221 C226 C225 120.12(16) . . ? C261 C266 C265 119.75(15) . . ? C113 C114 C115 120.37(15) . . ? C112 C111 C116 119.79(14) . . ? C112 C111 P11 119.68(12) . . ? C116 C111 P11 120.52(11) . . ? C146 C141 C142 119.72(14) . . ? C146 C141 P12 118.78(11) . . ? C142 C141 P12 121.45(12) . . ? C215 C214 C213 120.07(15) . . ? C223 C222 C221 119.93(15) . . ? C233 C232 C231 120.08(14) . . ? C144 C143 C142 120.19(15) . . ? C226 C221 C222 119.66(14) . . ? C226 C221 P21 119.67(12) . . ? C222 C221 P21 120.57(12) . . ? C135 C134 C133 120.03(15) . . ? C121 C122 C123 120.14(14) . . ? C266 C261 C262 119.98(13) . . ? C266 C261 P22 121.59(11) . . ? C262 C261 P22 118.41(11) . . ? C122 C121 C126 119.43(13) . . ? C122 C121 P11 122.39(11) . . ? C126 C121 P11 118.05(12) . . ? C165 C164 C163 120.17(15) . . ? C166 C161 C162 119.64(14) . . ? C166 C161 P12 122.28(11) . . ? C162 C161 P12 118.08(12) . . ? C143 C142 C141 119.83(15) . . ? C155 C156 C151 119.88(16) . . ? C153 C152 C151 119.92(16) . . ? C232 C231 C236 119.50(14) . . ? C232 C231 P21 118.23(11) . . ? C236 C231 P21 122.18(12) . . ? C143 C144 C145 120.29(15) . . ? C154 C153 C152 120.01(16) . . ? C256 C251 C252 119.82(14) . . ? C256 C251 P22 120.01(11) . . ? C252 C251 P22 120.14(12) . . ? C133 C132 C131 120.09(15) . . ? C243 C242 C241 120.02(13) . . ? C262 C263 C264 120.00(15) . . ? C222 C223 C224 120.02(16) . . ? C136 C135 C134 120.60(15) . . ? C216 C211 C212 119.32(14) . . ? C216 C211 P21 122.69(11) . . ? C212 C211 P21 117.98(12) . . ? C153 C154 C155 120.22(16) . . ? C235 C236 C231 119.82(15) . . ? C115 C116 C111 120.19(15) . . ? C161 C166 C165 120.03(14) . . ? C145 C146 C141 120.19(15) . . ? C265 C264 C263 120.44(14) . . ? C224 C225 C226 119.84(16) . . ? C234 C235 C236 120.38(15) . . ? C254 C255 C256 119.67(16) . . ? C264 C265 C266 120.04(15) . . ? C235 C234 C233 120.00(14) . . ? C252 C253 C254 119.47(16) . . ? C132 C131 C136 119.70(14) . . ? C132 C131 P11 121.29(12) . . ? C136 C131 P11 118.97(12) . . ? C146 C145 C144 119.78(15) . . ? C211 C216 C215 120.07(15) . . ? C244 C243 C242 119.81(14) . . ? C125 C126 C121 119.97(15) . . ? C124 C125 C126 120.27(15) . . ? C245 C244 C243 120.27(14) . . ? C255 C254 C253 120.89(15) . . ? C114 C113 C112 120.26(15) . . ? C123 C124 C125 120.15(14) . . ? C162 C163 C164 120.17(15) . . ? C116 C115 C114 119.83(15) . . ? C164 C165 C166 120.03(15) . . ? C245 C246 C241 119.34(14) . . ? C244 C245 C246 120.64(13) . . ? C232 C233 C234 120.21(15) . . ? C135 C136 C131 119.49(15) . . ? C212 C213 C214 120.05(15) . . ? C263 C262 C261 119.78(15) . . ? C124 C123 C122 120.01(15) . . ? C156 C155 C154 120.18(16) . . ? C225 C224 C223 120.40(16) . . ? C134 C133 C132 120.10(16) . . ? C213 C212 C211 120.30(15) . . ? C163 C162 C161 119.95(16) . . ? C251 C256 C255 119.90(15) . . ? C113 C112 C111 119.55(15) . . ? C214 C215 C216 120.18(16) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.884 _refine_diff_density_min -0.738 _refine_diff_density_rms 0.076 _database_code_depnum_ccdc_archive 'CCDC 898624' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_11209 #TrackingRef '18537_web_deposit_cif_file_0_DanielTofan_1363226975.MoP3_11209.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C77 H65 Mo N2 O11 P7' _chemical_formula_weight 1507.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 29.871(5) _cell_length_b 13.004(2) _cell_length_c 20.900(3) _cell_angle_alpha 90.00 _cell_angle_beta 122.557(2) _cell_angle_gamma 90.00 _cell_volume 6842.9(19) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9673 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 30.80 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3104 _exptl_absorpt_coefficient_mu 0.420 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7433 _exptl_absorpt_correction_T_max 0.9435 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; 'Siemens three-circle diffractometer, Bruker APEX CCD' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 78082 _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 30.51 _reflns_number_total 20083 _reflns_number_gt 19526 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2011.4.0 (Bruker-AXS, 2011)' _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2011)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0371P)^2^+1.8831P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.474(9) _refine_ls_number_reflns 20083 _refine_ls_number_parameters 884 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0237 _refine_ls_R_factor_gt 0.0225 _refine_ls_wR_factor_ref 0.0598 _refine_ls_wR_factor_gt 0.0588 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.267365(4) 0.217472(9) 0.318117(5) 0.01851(3) Uani 1 1 d . . . P7 P 0.064338(12) 0.32873(2) 0.726672(16) 0.01139(6) Uani 1 1 d . . . P6 P 0.133022(13) 0.36399(2) 0.895546(17) 0.01236(6) Uani 1 1 d . . . P1 P 0.289081(13) 0.36017(2) 0.204664(18) 0.01242(6) Uani 1 1 d . . . P2 P 0.284343(14) 0.14617(3) 0.17761(2) 0.01760(7) Uani 1 1 d . . . P3 P 0.375860(14) 0.23350(3) 0.30629(2) 0.01707(6) Uani 1 1 d . . . P4 P 0.925587(13) 0.13718(2) 0.205399(17) 0.01209(6) Uani 1 1 d . . . P5 P 0.988371(13) 0.16562(2) 0.375175(17) 0.01198(6) Uani 1 1 d . . . C42 C 0.15075(5) 0.49586(10) 0.92286(7) 0.0148(2) Uani 1 1 d . . . C44 C 0.13057(7) 0.67661(12) 0.89789(9) 0.0235(3) Uani 1 1 d . . . H44 H 0.1078 0.7301 0.8661 0.028 Uiso 1 1 calc R . . C46 C 0.21136(6) 0.62271(12) 1.01180(8) 0.0225(3) Uani 1 1 d . . . H46 H 0.2433 0.6394 1.0582 0.027 Uiso 1 1 calc R . . C47 C 0.19846(6) 0.52071(11) 0.99042(7) 0.0179(2) Uani 1 1 d . . . H47 H 0.2220 0.4676 1.0216 0.021 Uiso 1 1 calc R . . C45 C 0.17757(7) 0.70046(11) 0.96529(9) 0.0240(3) Uani 1 1 d . . . H45 H 0.1867 0.7703 0.9797 0.029 Uiso 1 1 calc R . . C43 C 0.11680(6) 0.57445(11) 0.87681(8) 0.0185(2) Uani 1 1 d . . . H43 H 0.0843 0.5581 0.8311 0.022 Uiso 1 1 calc R . . O4 O 0.27254(4) 0.26350(7) 0.14769(5) 0.01453(17) Uani 1 1 d . . . O6 O 0.35196(4) 0.34022(7) 0.26027(5) 0.01475(17) Uani 1 1 d . . . O1 O 0.26363(4) 0.34427(7) 0.24960(5) 0.01558(17) Uani 1 1 d . . . O5 O 0.34815(4) 0.15141(7) 0.23697(6) 0.01953(19) Uani 1 1 d . . . O9 O 0.43357(4) 0.23139(9) 0.34234(7) 0.0256(2) Uani 1 1 d . . . C48 C 0.19205(5) 0.30052(10) 0.91188(7) 0.0154(2) Uani 1 1 d . . . C72 C 0.10744(5) 0.36905(10) 0.69616(7) 0.0135(2) Uani 1 1 d . . . C6 C 0.90523(5) 0.00872(10) 0.17092(7) 0.0142(2) Uani 1 1 d . . . C30 C 0.94359(5) 0.12282(10) 0.40231(7) 0.0136(2) Uani 1 1 d . . . C36 C 1.05149(5) 0.10552(10) 0.43804(7) 0.0142(2) Uani 1 1 d . . . C24 C 0.99526(6) 0.30230(10) 0.39228(7) 0.0151(2) Uani 1 1 d . . . C66 C 0.00108(5) 0.39021(10) 0.66672(7) 0.0130(2) Uani 1 1 d . . . N2 N 0.08426(5) 0.35832(9) 0.81067(6) 0.0162(2) Uani 1 1 d . . . N1 N 0.97102(5) 0.13464(9) 0.29228(6) 0.0161(2) Uani 1 1 d . . . O3 O 0.35247(4) 0.21843(8) 0.35354(6) 0.0202(2) Uani 1 1 d . . . O2 O 0.25890(4) 0.12779(8) 0.22179(6) 0.0204(2) Uani 1 1 d . . . O7 O 0.27889(4) 0.45639(7) 0.16280(5) 0.01762(18) Uani 1 1 d . . . O8 O 0.27187(5) 0.07840(8) 0.11414(6) 0.0260(2) Uani 1 1 d . . . C2 C 0.19267(7) 0.23131(13) 0.28258(9) 0.0241(3) Uani 1 1 d . . . C27 C 1.00001(7) 0.51428(11) 0.41737(9) 0.0233(3) Uani 1 1 d . . . H27 H 1.0017 0.5863 0.4260 0.028 Uiso 1 1 calc R . . C31 C 0.92716(6) 0.18832(11) 0.43884(7) 0.0170(2) Uani 1 1 d . . . H31 H 0.9404 0.2567 0.4509 0.020 Uiso 1 1 calc R . . C32 C 0.89167(6) 0.15416(11) 0.45755(8) 0.0202(3) Uani 1 1 d . . . H32 H 0.8807 0.1990 0.4825 0.024 Uiso 1 1 calc R . . C33 C 0.87217(6) 0.05444(12) 0.43993(8) 0.0208(3) Uani 1 1 d . . . H33 H 0.8477 0.0313 0.4526 0.025 Uiso 1 1 calc R . . C29 C 1.04083(6) 0.34637(11) 0.45320(8) 0.0183(2) Uani 1 1 d . . . H29 H 1.0705 0.3043 0.4864 0.022 Uiso 1 1 calc R . . C28 C 1.04305(6) 0.45220(11) 0.46566(9) 0.0241(3) Uani 1 1 d . . . H28 H 1.0742 0.4819 0.5074 0.029 Uiso 1 1 calc R . . C26 C 0.95441(7) 0.47045(11) 0.35627(9) 0.0266(3) Uani 1 1 d . . . H26 H 0.9249 0.5127 0.3230 0.032 Uiso 1 1 calc R . . O11 O 0.14855(5) 0.24038(12) 0.26354(7) 0.0340(3) Uani 1 1 d . . . C17 C 0.99405(6) 0.26672(11) 0.19475(8) 0.0208(3) Uani 1 1 d . . . H17 H 1.0094 0.2773 0.2476 0.025 Uiso 1 1 calc R . . C41 C 1.08155(6) 0.07026(11) 0.40953(8) 0.0195(3) Uani 1 1 d . . . H41 H 1.0683 0.0761 0.3569 0.023 Uiso 1 1 calc R . . C18 C 0.86710(5) 0.20618(10) 0.18424(7) 0.0146(2) Uani 1 1 d . . . C12 C 0.95130(5) 0.19960(10) 0.15495(7) 0.0145(2) Uani 1 1 d . . . C19 C 0.85288(6) 0.29886(11) 0.14434(9) 0.0210(3) Uani 1 1 d . . . H19 H 0.8715 0.3222 0.1219 0.025 Uiso 1 1 calc R . . C13 C 0.92879(6) 0.18393(11) 0.07738(8) 0.0192(3) Uani 1 1 d . . . H13 H 0.8999 0.1377 0.0502 0.023 Uiso 1 1 calc R . . C37 C 1.07132(6) 0.09544(11) 0.51556(8) 0.0200(3) Uani 1 1 d . . . H37 H 1.0508 0.1185 0.5352 0.024 Uiso 1 1 calc R . . C40 C 1.13111(6) 0.02654(12) 0.45871(10) 0.0254(3) Uani 1 1 d . . . H40 H 1.1515 0.0023 0.4393 0.030 Uiso 1 1 calc R . . C23 C 0.83867(6) 0.17041(11) 0.21531(8) 0.0178(2) Uani 1 1 d . . . H23 H 0.8470 0.1057 0.2403 0.021 Uiso 1 1 calc R . . C25 C 0.95198(7) 0.36539(11) 0.34381(8) 0.0242(3) Uani 1 1 d . . . H25 H 0.9207 0.3359 0.3021 0.029 Uiso 1 1 calc R . . C35 C 0.92400(6) 0.02187(10) 0.38508(8) 0.0180(2) Uani 1 1 d . . . H35 H 0.9352 -0.0235 0.3607 0.022 Uiso 1 1 calc R . . C34 C 0.88821(6) -0.01174(11) 0.40377(8) 0.0208(3) Uani 1 1 d . . . H34 H 0.8747 -0.0799 0.3918 0.025 Uiso 1 1 calc R . . C49 C 0.21584(5) 0.34013(12) 0.87496(8) 0.0198(3) Uani 1 1 d . . . H49 H 0.2042 0.4038 0.8487 0.024 Uiso 1 1 calc R . . C76 C 0.16280(6) 0.50189(11) 0.69306(8) 0.0210(3) Uani 1 1 d . . . H76 H 0.1761 0.5702 0.7039 0.025 Uiso 1 1 calc R . . C60 C 0.05554(5) 0.19214(10) 0.70885(7) 0.0135(2) Uani 1 1 d . . . C77 C 0.12657(6) 0.47045(10) 0.71098(8) 0.0177(2) Uani 1 1 d . . . H77 H 0.1146 0.5176 0.7334 0.021 Uiso 1 1 calc R . . C54 C 0.11406(5) 0.30452(10) 0.95490(7) 0.0143(2) Uani 1 1 d . . . C59 C 0.06637(6) 0.25020(11) 0.92235(8) 0.0186(2) Uani 1 1 d . . . H59 H 0.0434 0.2465 0.8687 0.022 Uiso 1 1 calc R . . C52 C 0.25272(6) 0.15690(12) 0.95636(10) 0.0250(3) Uani 1 1 d . . . H52 H 0.2660 0.0953 0.9850 0.030 Uiso 1 1 calc R . . C73 C 0.12437(6) 0.30090(11) 0.66188(8) 0.0178(2) Uani 1 1 d . . . H73 H 0.1114 0.2323 0.6514 0.021 Uiso 1 1 calc R . . C55 C 0.14797(6) 0.30906(12) 1.03374(8) 0.0200(3) Uani 1 1 d . . . H55 H 0.1802 0.3469 1.0561 0.024 Uiso 1 1 calc R . . C50 C 0.25653(6) 0.28602(13) 0.87678(9) 0.0249(3) Uani 1 1 d . . . H50 H 0.2721 0.3117 0.8505 0.030 Uiso 1 1 calc R . . C53 C 0.21120(6) 0.20990(11) 0.95393(8) 0.0196(3) Uani 1 1 d . . . H53 H 0.1960 0.1844 0.9808 0.024 Uiso 1 1 calc R . . C65 C 0.01306(6) 0.15279(10) 0.64112(7) 0.0169(2) Uani 1 1 d . . . H65 H -0.0138 0.1978 0.6052 0.020 Uiso 1 1 calc R . . C70 C -0.06960(6) 0.44925(11) 0.54384(8) 0.0219(3) Uani 1 1 d . . . H70 H -0.0834 0.4618 0.4916 0.026 Uiso 1 1 calc R . . C58 C 0.05264(6) 0.20155(12) 0.96861(9) 0.0227(3) Uani 1 1 d . . . H58 H 0.0198 0.1660 0.9466 0.027 Uiso 1 1 calc R . . C57 C 0.08695(7) 0.20482(11) 1.04706(9) 0.0228(3) Uani 1 1 d . . . H57 H 0.0778 0.1704 1.0785 0.027 Uiso 1 1 calc R . . C71 C -0.01899(5) 0.40797(10) 0.58991(7) 0.0172(2) Uani 1 1 d . . . H71 H 0.0018 0.3919 0.5693 0.021 Uiso 1 1 calc R . . C67 C -0.02894(5) 0.41641(10) 0.69744(8) 0.0162(2) Uani 1 1 d . . . H67 H -0.0147 0.4066 0.7500 0.019 Uiso 1 1 calc R . . C62 C 0.09085(6) 0.02024(11) 0.74593(9) 0.0235(3) Uani 1 1 d . . . H62 H 0.1174 -0.0252 0.7819 0.028 Uiso 1 1 calc R . . C64 C 0.00970(6) 0.04796(11) 0.62577(8) 0.0204(3) Uani 1 1 d . . . H64 H -0.0194 0.0217 0.5795 0.024 Uiso 1 1 calc R . . C63 C 0.04888(6) -0.01835(11) 0.67815(9) 0.0206(3) Uani 1 1 d . . . H63 H 0.0469 -0.0898 0.6675 0.025 Uiso 1 1 calc R . . C68 C -0.07968(6) 0.45689(11) 0.65100(8) 0.0211(3) Uani 1 1 d . . . H68 H -0.1003 0.4740 0.6716 0.025 Uiso 1 1 calc R . . C61 C 0.09455(6) 0.12479(11) 0.76179(8) 0.0217(3) Uani 1 1 d . . . H61 H 0.1235 0.1505 0.8084 0.026 Uiso 1 1 calc R . . C74 C 0.16028(6) 0.33357(12) 0.64302(9) 0.0218(3) Uani 1 1 d . . . H74 H 0.1715 0.2874 0.6191 0.026 Uiso 1 1 calc R . . C56 C 0.13447(7) 0.25808(13) 1.07951(8) 0.0232(3) Uani 1 1 d . . . H56 H 0.1579 0.2598 1.1332 0.028 Uiso 1 1 calc R . . C1 C 0.27359(7) 0.31914(15) 0.39042(9) 0.0297(3) Uani 1 1 d . . . C4 C 0.29015(7) 0.07265(15) 0.38047(10) 0.0355(4) Uani 1 1 d . . . H4 H 0.3137 0.0304 0.3747 0.043 Uiso 1 1 calc R . . C3 C 0.23451(7) 0.06412(14) 0.33250(10) 0.0349(4) Uani 1 1 d . . . H3A H 0.2122 0.1077 0.3399 0.042 Uiso 1 1 calc R . . H3B H 0.2194 0.0148 0.2927 0.042 Uiso 1 1 calc R . . C5 C 0.30857(8) 0.14859(16) 0.43787(10) 0.0377(4) Uani 1 1 d . . . H5A H 0.2839 0.1895 0.4419 0.045 Uiso 1 1 calc R . . H5B H 0.3456 0.1586 0.4723 0.045 Uiso 1 1 calc R . . O10 O 0.27694(6) 0.38208(13) 0.43185(8) 0.0444(4) Uani 1 1 d . . . C39 C 1.15106(6) 0.01793(12) 0.53541(10) 0.0275(3) Uani 1 1 d . . . H39 H 1.1852 -0.0110 0.5686 0.033 Uiso 1 1 calc R . . C8 C 0.92199(7) -0.17351(11) 0.18818(9) 0.0223(3) Uani 1 1 d . . . H8 H 0.9439 -0.2297 0.2171 0.027 Uiso 1 1 calc R . . C10 C 0.84134(6) -0.11012(11) 0.07841(8) 0.0208(3) Uani 1 1 d . . . H10 H 0.8086 -0.1231 0.0321 0.025 Uiso 1 1 calc R . . C14 C 0.94897(7) 0.23646(12) 0.03992(8) 0.0229(3) Uani 1 1 d . . . H14 H 0.9336 0.2265 -0.0130 0.027 Uiso 1 1 calc R . . C11 C 0.85654(6) -0.00966(10) 0.10346(7) 0.0171(2) Uani 1 1 d . . . H11 H 0.8340 0.0461 0.0750 0.021 Uiso 1 1 calc R . . C7 C 0.93812(6) -0.07324(10) 0.21348(8) 0.0178(2) Uani 1 1 d . . . H7 H 0.9712 -0.0607 0.2593 0.021 Uiso 1 1 calc R . . C9 C 0.87395(7) -0.19143(11) 0.12091(9) 0.0232(3) Uani 1 1 d . . . H9 H 0.8632 -0.2600 0.1037 0.028 Uiso 1 1 calc R . . C38 C 1.12093(6) 0.05173(12) 0.56380(8) 0.0249(3) Uani 1 1 d . . . H38 H 1.1343 0.0449 0.6164 0.030 Uiso 1 1 calc R . . C22 C 0.79798(6) 0.23039(13) 0.20925(9) 0.0235(3) Uani 1 1 d . . . H22 H 0.7790 0.2073 0.2312 0.028 Uiso 1 1 calc R . . C51 C 0.27459(6) 0.19418(13) 0.91695(10) 0.0271(3) Uani 1 1 d . . . H51 H 0.3021 0.1568 0.9174 0.033 Uiso 1 1 calc R . . C75 C 0.17978(6) 0.43337(12) 0.65909(8) 0.0229(3) Uani 1 1 d . . . H75 H 0.2047 0.4550 0.6469 0.027 Uiso 1 1 calc R . . C21 C 0.78508(7) 0.32366(13) 0.17130(10) 0.0270(3) Uani 1 1 d . . . H21 H 0.7579 0.3651 0.1685 0.032 Uiso 1 1 calc R . . C20 C 0.81158(7) 0.35685(12) 0.13740(10) 0.0274(3) Uani 1 1 d . . . H20 H 0.8015 0.4193 0.1094 0.033 Uiso 1 1 calc R . . C69 C -0.10008(6) 0.47225(12) 0.57411(9) 0.0227(3) Uani 1 1 d . . . H69 H -0.1350 0.4986 0.5421 0.027 Uiso 1 1 calc R . . C15 C 0.99151(7) 0.30316(12) 0.07993(9) 0.0240(3) Uani 1 1 d . . . H15 H 1.0052 0.3387 0.0543 0.029 Uiso 1 1 calc R . . C16 C 1.01424(7) 0.31824(12) 0.15723(9) 0.0250(3) Uani 1 1 d . . . H16 H 1.0435 0.3637 0.1844 0.030 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 0.01471(5) 0.02298(5) 0.01358(4) 0.00553(4) 0.00480(4) -0.00409(5) P7 0.01086(14) 0.01261(13) 0.00955(12) -0.00042(10) 0.00474(10) -0.00015(11) P6 0.01096(14) 0.01515(14) 0.00954(12) -0.00061(10) 0.00458(11) 0.00081(11) P1 0.01258(14) 0.01187(13) 0.01286(13) 0.00160(10) 0.00689(11) 0.00160(11) P2 0.01382(16) 0.01240(14) 0.01934(15) -0.00165(11) 0.00413(12) 0.00018(12) P3 0.01132(15) 0.01590(15) 0.01657(15) 0.00195(11) 0.00260(12) 0.00047(12) P4 0.01317(14) 0.01188(13) 0.01123(13) -0.00087(10) 0.00657(11) 0.00037(11) P5 0.01288(15) 0.01188(13) 0.01070(13) -0.00080(10) 0.00602(11) 0.00128(11) C42 0.0166(6) 0.0157(5) 0.0124(5) -0.0004(4) 0.0079(4) 0.0004(5) C44 0.0285(8) 0.0186(6) 0.0258(7) 0.0029(5) 0.0161(6) 0.0052(6) C46 0.0236(7) 0.0233(7) 0.0208(6) -0.0064(5) 0.0122(5) -0.0052(6) C47 0.0171(6) 0.0204(6) 0.0148(5) -0.0015(4) 0.0077(5) -0.0007(5) C45 0.0307(8) 0.0178(6) 0.0288(7) -0.0053(5) 0.0194(6) -0.0040(6) C43 0.0190(6) 0.0197(6) 0.0163(5) 0.0004(5) 0.0092(5) 0.0023(5) O4 0.0131(4) 0.0129(4) 0.0139(4) -0.0001(3) 0.0049(3) 0.0012(3) O6 0.0126(4) 0.0134(4) 0.0159(4) 0.0004(3) 0.0061(3) -0.0006(3) O1 0.0154(5) 0.0182(4) 0.0148(4) 0.0031(3) 0.0092(3) 0.0019(4) O5 0.0135(5) 0.0139(4) 0.0228(5) -0.0010(3) 0.0042(4) 0.0028(3) O9 0.0131(5) 0.0268(5) 0.0264(5) 0.0027(4) 0.0037(4) 0.0014(4) C48 0.0122(6) 0.0179(6) 0.0136(5) -0.0037(4) 0.0053(4) -0.0002(5) C72 0.0111(5) 0.0162(6) 0.0114(5) 0.0002(4) 0.0049(4) -0.0008(4) C6 0.0168(6) 0.0130(5) 0.0161(5) -0.0024(4) 0.0110(5) -0.0010(5) C30 0.0123(5) 0.0159(5) 0.0118(5) 0.0002(4) 0.0059(4) 0.0012(4) C36 0.0122(6) 0.0119(5) 0.0157(5) -0.0003(4) 0.0056(4) 0.0003(4) C24 0.0186(6) 0.0135(5) 0.0143(5) -0.0006(4) 0.0096(5) 0.0004(5) C66 0.0119(5) 0.0124(5) 0.0118(5) 0.0006(4) 0.0045(4) -0.0007(4) N2 0.0143(5) 0.0222(5) 0.0091(4) -0.0007(4) 0.0043(4) 0.0023(4) N1 0.0166(5) 0.0187(5) 0.0122(5) -0.0019(4) 0.0072(4) 0.0017(4) O3 0.0160(5) 0.0219(5) 0.0153(4) 0.0053(3) 0.0035(4) -0.0019(4) O2 0.0164(5) 0.0170(5) 0.0208(5) 0.0022(3) 0.0053(4) -0.0028(4) O7 0.0218(5) 0.0147(4) 0.0194(4) 0.0046(3) 0.0131(4) 0.0035(4) O8 0.0221(5) 0.0193(5) 0.0275(5) -0.0080(4) 0.0072(4) 0.0000(4) C2 0.0233(8) 0.0321(8) 0.0167(6) 0.0046(5) 0.0107(6) -0.0029(6) C27 0.0350(8) 0.0129(6) 0.0281(7) -0.0015(5) 0.0211(6) -0.0016(5) C31 0.0179(6) 0.0158(6) 0.0171(6) -0.0027(4) 0.0093(5) 0.0011(5) C32 0.0192(7) 0.0241(7) 0.0196(6) -0.0027(5) 0.0120(5) 0.0021(5) C33 0.0195(7) 0.0264(7) 0.0185(6) 0.0012(5) 0.0114(5) -0.0005(5) C29 0.0168(6) 0.0170(6) 0.0213(6) -0.0027(5) 0.0104(5) -0.0019(5) C28 0.0235(7) 0.0178(6) 0.0314(7) -0.0066(5) 0.0152(6) -0.0056(5) C26 0.0357(9) 0.0164(6) 0.0216(6) 0.0023(5) 0.0115(6) 0.0082(6) O11 0.0219(6) 0.0539(8) 0.0281(6) 0.0048(5) 0.0147(5) -0.0009(6) C17 0.0221(7) 0.0206(6) 0.0196(6) -0.0029(5) 0.0113(5) -0.0038(5) C41 0.0181(6) 0.0184(6) 0.0234(6) 0.0013(5) 0.0122(5) 0.0025(5) C18 0.0144(6) 0.0135(5) 0.0140(5) -0.0030(4) 0.0064(4) 0.0006(4) C12 0.0149(6) 0.0148(5) 0.0136(5) 0.0009(4) 0.0076(4) 0.0021(4) C19 0.0234(7) 0.0162(6) 0.0241(6) 0.0025(5) 0.0132(5) 0.0032(5) C13 0.0196(7) 0.0230(6) 0.0146(6) -0.0008(5) 0.0090(5) -0.0018(5) C37 0.0202(7) 0.0199(6) 0.0158(6) -0.0006(5) 0.0069(5) 0.0007(5) C40 0.0188(7) 0.0197(7) 0.0378(8) 0.0015(6) 0.0153(6) 0.0036(5) C23 0.0151(6) 0.0192(6) 0.0172(6) -0.0021(5) 0.0075(5) -0.0013(5) C25 0.0275(8) 0.0169(6) 0.0181(6) -0.0012(5) 0.0056(5) 0.0063(5) C35 0.0222(7) 0.0164(6) 0.0178(6) -0.0021(4) 0.0124(5) -0.0012(5) C34 0.0264(7) 0.0190(6) 0.0190(6) -0.0013(5) 0.0135(5) -0.0037(5) C49 0.0125(6) 0.0293(7) 0.0151(6) -0.0008(5) 0.0058(5) -0.0004(5) C76 0.0195(7) 0.0181(6) 0.0241(6) 0.0015(5) 0.0109(5) -0.0045(5) C60 0.0144(6) 0.0132(5) 0.0146(5) 0.0003(4) 0.0089(4) -0.0006(4) C77 0.0176(6) 0.0151(6) 0.0195(6) -0.0003(4) 0.0094(5) -0.0012(5) C54 0.0133(6) 0.0158(5) 0.0130(5) 0.0021(4) 0.0066(4) 0.0033(5) C59 0.0144(6) 0.0206(6) 0.0168(6) 0.0022(5) 0.0057(5) 0.0001(5) C52 0.0193(7) 0.0189(7) 0.0329(8) -0.0033(5) 0.0115(6) 0.0038(5) C73 0.0162(6) 0.0198(6) 0.0182(6) -0.0047(5) 0.0096(5) -0.0040(5) C55 0.0179(6) 0.0260(7) 0.0138(6) -0.0002(5) 0.0069(5) -0.0032(5) C50 0.0168(7) 0.0390(9) 0.0207(7) -0.0068(6) 0.0112(5) -0.0029(6) C53 0.0168(6) 0.0179(6) 0.0215(6) -0.0019(5) 0.0084(5) 0.0007(5) C65 0.0164(6) 0.0163(6) 0.0164(6) -0.0006(4) 0.0078(5) -0.0017(5) C70 0.0197(7) 0.0215(6) 0.0143(6) 0.0027(5) 0.0024(5) 0.0016(5) C58 0.0167(7) 0.0233(7) 0.0278(7) 0.0047(5) 0.0117(6) 0.0002(5) C57 0.0261(8) 0.0227(7) 0.0272(7) 0.0085(5) 0.0194(6) 0.0059(6) C71 0.0163(6) 0.0187(6) 0.0135(5) 0.0005(4) 0.0060(5) -0.0005(5) C67 0.0152(6) 0.0153(6) 0.0179(6) 0.0016(4) 0.0088(5) 0.0016(5) C62 0.0239(7) 0.0163(6) 0.0272(7) 0.0037(5) 0.0116(6) 0.0038(5) C64 0.0227(7) 0.0182(6) 0.0198(6) -0.0049(5) 0.0111(5) -0.0050(5) C63 0.0257(7) 0.0145(6) 0.0286(7) -0.0017(5) 0.0193(6) -0.0029(5) C68 0.0174(7) 0.0197(6) 0.0257(7) 0.0015(5) 0.0112(5) 0.0027(5) C61 0.0195(7) 0.0173(6) 0.0196(6) 0.0011(5) 0.0046(5) 0.0021(5) C74 0.0201(7) 0.0276(7) 0.0234(6) -0.0048(5) 0.0154(5) -0.0035(6) C56 0.0271(8) 0.0287(7) 0.0150(6) 0.0027(5) 0.0121(6) 0.0014(6) C1 0.0254(8) 0.0454(10) 0.0221(7) 0.0002(6) 0.0153(6) -0.0120(7) C4 0.0257(8) 0.0336(9) 0.0338(8) 0.0210(7) 0.0072(6) -0.0040(7) C3 0.0271(8) 0.0321(8) 0.0338(8) 0.0151(7) 0.0086(7) -0.0075(7) C5 0.0264(8) 0.0529(11) 0.0206(7) 0.0184(7) 0.0039(6) -0.0072(8) O10 0.0480(9) 0.0639(9) 0.0358(7) -0.0201(7) 0.0321(7) -0.0222(7) C39 0.0158(7) 0.0164(6) 0.0359(8) 0.0038(5) 0.0044(6) 0.0027(5) C8 0.0298(8) 0.0146(6) 0.0302(7) 0.0008(5) 0.0211(6) 0.0031(5) C10 0.0228(7) 0.0228(7) 0.0211(6) -0.0086(5) 0.0147(5) -0.0079(5) C14 0.0276(8) 0.0270(7) 0.0175(6) 0.0031(5) 0.0144(6) 0.0025(6) C11 0.0185(6) 0.0177(6) 0.0168(6) -0.0029(4) 0.0106(5) -0.0016(5) C7 0.0198(6) 0.0157(6) 0.0205(6) -0.0003(5) 0.0125(5) 0.0014(5) C9 0.0333(8) 0.0165(6) 0.0314(7) -0.0081(5) 0.0250(7) -0.0068(6) C38 0.0217(7) 0.0204(7) 0.0187(6) 0.0019(5) 0.0016(5) 0.0022(5) C22 0.0169(7) 0.0305(7) 0.0244(7) -0.0045(5) 0.0118(5) -0.0002(5) C51 0.0186(7) 0.0292(8) 0.0325(8) -0.0107(6) 0.0130(6) 0.0014(6) C75 0.0176(6) 0.0297(7) 0.0239(6) 0.0002(5) 0.0128(5) -0.0047(6) C21 0.0202(7) 0.0269(7) 0.0317(8) -0.0051(6) 0.0126(6) 0.0056(6) C20 0.0283(8) 0.0192(7) 0.0328(8) 0.0020(5) 0.0153(6) 0.0075(6) C69 0.0146(6) 0.0201(6) 0.0241(7) 0.0042(5) 0.0042(5) 0.0034(5) C15 0.0280(8) 0.0207(6) 0.0332(8) 0.0062(5) 0.0230(7) 0.0030(6) C16 0.0261(8) 0.0204(7) 0.0326(8) -0.0027(6) 0.0184(6) -0.0069(6) _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 1.9400(19) . ? Mo1 C2 1.9440(17) . ? Mo1 O1 2.1471(10) . ? Mo1 C4 2.1803(16) . ? Mo1 O2 2.2201(11) . ? Mo1 O3 2.2327(12) . ? Mo1 C5 2.2947(16) . ? Mo1 C3 2.3125(16) . ? P7 N2 1.5684(12) . ? P7 C72 1.7952(13) . ? P7 C66 1.7976(13) . ? P7 C60 1.8048(14) . ? P6 N2 1.5789(12) . ? P6 C54 1.7928(13) . ? P6 C42 1.7950(14) . ? P6 C48 1.8051(14) . ? P1 O7 1.4619(10) . ? P1 O1 1.5072(10) . ? P1 O6 1.6113(11) . ? P1 O4 1.6154(10) . ? P2 O8 1.4638(11) . ? P2 O2 1.4977(12) . ? P2 O4 1.6143(10) . ? P2 O5 1.6223(11) . ? P3 O9 1.4636(12) . ? P3 O3 1.4982(12) . ? P3 O6 1.6191(10) . ? P3 O5 1.6226(11) . ? P4 N1 1.5773(12) . ? P4 C6 1.7911(13) . ? P4 C18 1.7948(14) . ? P4 C12 1.7978(13) . ? P5 N1 1.5704(11) . ? P5 C36 1.7961(14) . ? P5 C30 1.7993(13) . ? P5 C24 1.8028(14) . ? C42 C43 1.3959(19) . ? C42 C47 1.4013(18) . ? C44 C45 1.387(2) . ? C44 C43 1.390(2) . ? C46 C47 1.386(2) . ? C46 C45 1.389(2) . ? C48 C53 1.3955(19) . ? C48 C49 1.3987(19) . ? C72 C73 1.3945(18) . ? C72 C77 1.4039(18) . ? C6 C7 1.3971(19) . ? C6 C11 1.3977(18) . ? C30 C31 1.3974(17) . ? C30 C35 1.4031(19) . ? C36 C41 1.3955(19) . ? C36 C37 1.4000(18) . ? C24 C29 1.3919(19) . ? C24 C25 1.400(2) . ? C66 C67 1.3972(18) . ? C66 C71 1.3978(17) . ? C2 O11 1.160(2) . ? C27 C28 1.388(2) . ? C27 C26 1.392(2) . ? C31 C32 1.386(2) . ? C32 C33 1.388(2) . ? C33 C34 1.390(2) . ? C29 C28 1.396(2) . ? C26 C25 1.385(2) . ? C17 C16 1.392(2) . ? C17 C12 1.393(2) . ? C41 C40 1.391(2) . ? C18 C19 1.3954(19) . ? C18 C23 1.3975(19) . ? C12 C13 1.3959(18) . ? C19 C20 1.385(2) . ? C13 C14 1.397(2) . ? C37 C38 1.388(2) . ? C40 C39 1.382(2) . ? C23 C22 1.391(2) . ? C35 C34 1.391(2) . ? C49 C50 1.387(2) . ? C76 C77 1.384(2) . ? C76 C75 1.394(2) . ? C60 C65 1.3937(18) . ? C60 C61 1.4005(18) . ? C54 C59 1.396(2) . ? C54 C55 1.3958(18) . ? C59 C58 1.389(2) . ? C52 C51 1.385(2) . ? C52 C53 1.396(2) . ? C73 C74 1.393(2) . ? C55 C56 1.390(2) . ? C50 C51 1.391(2) . ? C65 C64 1.3917(19) . ? C70 C71 1.391(2) . ? C70 C69 1.392(2) . ? C58 C57 1.390(2) . ? C57 C56 1.385(2) . ? C67 C68 1.3905(19) . ? C62 C63 1.385(2) . ? C62 C61 1.390(2) . ? C64 C63 1.390(2) . ? C68 C69 1.393(2) . ? C74 C75 1.388(2) . ? C1 O10 1.156(2) . ? C4 C3 1.409(2) . ? C4 C5 1.417(3) . ? C39 C38 1.389(3) . ? C8 C9 1.385(2) . ? C8 C7 1.3921(19) . ? C10 C9 1.387(2) . ? C10 C11 1.3896(19) . ? C14 C15 1.387(2) . ? C22 C21 1.386(2) . ? C21 C20 1.385(2) . ? C15 C16 1.389(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Mo1 C2 81.01(7) . . ? C1 Mo1 O1 86.84(6) . . ? C2 Mo1 O1 92.12(5) . . ? C1 Mo1 C4 104.77(8) . . ? C2 Mo1 C4 103.49(7) . . ? O1 Mo1 C4 161.71(6) . . ? C1 Mo1 O2 168.73(6) . . ? C2 Mo1 O2 98.91(6) . . ? O1 Mo1 O2 81.90(4) . . ? C4 Mo1 O2 86.27(7) . . ? C1 Mo1 O3 97.07(6) . . ? C2 Mo1 O3 173.78(5) . . ? O1 Mo1 O3 81.84(4) . . ? C4 Mo1 O3 82.71(6) . . ? O2 Mo1 O3 81.80(4) . . ? C1 Mo1 C5 69.28(8) . . ? C2 Mo1 C5 106.53(7) . . ? O1 Mo1 C5 146.31(6) . . ? C4 Mo1 C5 36.79(8) . . ? O2 Mo1 C5 121.10(7) . . ? O3 Mo1 C5 78.10(6) . . ? C1 Mo1 C3 110.86(7) . . ? C2 Mo1 C3 69.47(7) . . ? O1 Mo1 C3 151.11(5) . . ? C4 Mo1 C3 36.41(6) . . ? O2 Mo1 C3 79.37(6) . . ? O3 Mo1 C3 116.67(6) . . ? C5 Mo1 C3 62.46(7) . . ? N2 P7 C72 114.41(6) . . ? N2 P7 C66 107.13(6) . . ? C72 P7 C66 107.95(6) . . ? N2 P7 C60 113.44(6) . . ? C72 P7 C60 105.47(6) . . ? C66 P7 C60 108.19(6) . . ? N2 P6 C54 108.26(6) . . ? N2 P6 C42 109.74(6) . . ? C54 P6 C42 109.94(6) . . ? N2 P6 C48 114.06(6) . . ? C54 P6 C48 108.19(6) . . ? C42 P6 C48 106.61(6) . . ? O7 P1 O1 118.55(6) . . ? O7 P1 O6 110.85(6) . . ? O1 P1 O6 108.16(6) . . ? O7 P1 O4 110.02(6) . . ? O1 P1 O4 107.21(6) . . ? O6 P1 O4 100.47(5) . . ? O8 P2 O2 119.76(7) . . ? O8 P2 O4 108.78(6) . . ? O2 P2 O4 108.19(6) . . ? O8 P2 O5 109.86(6) . . ? O2 P2 O5 108.20(6) . . ? O4 P2 O5 100.27(5) . . ? O9 P3 O3 119.74(7) . . ? O9 P3 O6 110.03(6) . . ? O3 P3 O6 106.90(6) . . ? O9 P3 O5 109.93(6) . . ? O3 P3 O5 107.92(6) . . ? O6 P3 O5 100.58(5) . . ? N1 P4 C6 109.83(6) . . ? N1 P4 C18 114.49(6) . . ? C6 P4 C18 107.01(6) . . ? N1 P4 C12 108.07(6) . . ? C6 P4 C12 110.17(6) . . ? C18 P4 C12 107.22(6) . . ? N1 P5 C36 106.78(6) . . ? N1 P5 C30 114.11(6) . . ? C36 P5 C30 107.50(6) . . ? N1 P5 C24 113.98(6) . . ? C36 P5 C24 108.73(6) . . ? C30 P5 C24 105.51(6) . . ? C43 C42 C47 119.57(13) . . ? C43 C42 P6 119.98(10) . . ? C47 C42 P6 120.45(10) . . ? C45 C44 C43 120.05(14) . . ? C47 C46 C45 119.97(14) . . ? C46 C47 C42 120.06(13) . . ? C44 C45 C46 120.34(14) . . ? C44 C43 C42 119.99(13) . . ? P2 O4 P1 122.25(6) . . ? P1 O6 P3 122.46(6) . . ? P1 O1 Mo1 131.17(6) . . ? P2 O5 P3 122.37(7) . . ? C53 C48 C49 120.05(13) . . ? C53 C48 P6 122.19(11) . . ? C49 C48 P6 117.51(11) . . ? C73 C72 C77 119.54(12) . . ? C73 C72 P7 121.65(10) . . ? C77 C72 P7 118.72(10) . . ? C7 C6 C11 120.35(12) . . ? C7 C6 P4 119.03(10) . . ? C11 C6 P4 120.60(10) . . ? C31 C30 C35 119.34(12) . . ? C31 C30 P5 121.53(10) . . ? C35 C30 P5 119.12(10) . . ? C41 C36 C37 119.65(13) . . ? C41 C36 P5 119.60(10) . . ? C37 C36 P5 120.74(11) . . ? C29 C24 C25 119.22(12) . . ? C29 C24 P5 122.58(10) . . ? C25 C24 P5 118.15(10) . . ? C67 C66 C71 120.19(12) . . ? C67 C66 P7 118.81(9) . . ? C71 C66 P7 120.95(10) . . ? P7 N2 P6 146.52(8) . . ? P5 N1 P4 146.44(8) . . ? P3 O3 Mo1 129.33(6) . . ? P2 O2 Mo1 128.85(6) . . ? O11 C2 Mo1 177.98(14) . . ? C28 C27 C26 119.66(13) . . ? C32 C31 C30 120.38(13) . . ? C31 C32 C33 120.01(13) . . ? C32 C33 C34 120.32(13) . . ? C24 C29 C28 120.11(14) . . ? C27 C28 C29 120.36(14) . . ? C25 C26 C27 120.17(14) . . ? C16 C17 C12 120.07(13) . . ? C40 C41 C36 119.51(13) . . ? C19 C18 C23 119.96(13) . . ? C19 C18 P4 121.48(11) . . ? C23 C18 P4 118.26(10) . . ? C17 C12 C13 119.91(13) . . ? C17 C12 P4 118.44(10) . . ? C13 C12 P4 121.64(11) . . ? C20 C19 C18 120.04(14) . . ? C12 C13 C14 119.75(13) . . ? C38 C37 C36 120.00(14) . . ? C39 C40 C41 120.89(15) . . ? C22 C23 C18 119.39(13) . . ? C26 C25 C24 120.48(14) . . ? C34 C35 C30 119.95(12) . . ? C33 C34 C35 119.99(13) . . ? C50 C49 C48 119.73(14) . . ? C77 C76 C75 120.06(13) . . ? C65 C60 C61 119.23(12) . . ? C65 C60 P7 121.52(10) . . ? C61 C60 P7 119.05(10) . . ? C76 C77 C72 120.17(13) . . ? C59 C54 C55 119.92(12) . . ? C59 C54 P6 120.04(10) . . ? C55 C54 P6 119.99(11) . . ? C58 C59 C54 119.83(13) . . ? C51 C52 C53 119.98(15) . . ? C74 C73 C72 119.93(13) . . ? C56 C55 C54 119.82(14) . . ? C49 C50 C51 120.10(15) . . ? C48 C53 C52 119.66(14) . . ? C64 C65 C60 120.47(13) . . ? C71 C70 C69 120.08(13) . . ? C59 C58 C57 120.04(14) . . ? C56 C57 C58 120.25(13) . . ? C70 C71 C66 119.57(13) . . ? C68 C67 C66 119.97(12) . . ? C63 C62 C61 120.69(14) . . ? C63 C64 C65 120.02(13) . . ? C62 C63 C64 119.72(13) . . ? C67 C68 C69 119.70(14) . . ? C62 C61 C60 119.86(13) . . ? C75 C74 C73 120.23(13) . . ? C57 C56 C55 120.12(13) . . ? O10 C1 Mo1 177.88(16) . . ? C3 C4 C5 115.4(2) . . ? C3 C4 Mo1 76.90(10) . . ? C5 C4 Mo1 76.00(10) . . ? C4 C3 Mo1 66.68(9) . . ? C4 C5 Mo1 67.21(9) . . ? C40 C39 C38 119.73(14) . . ? C9 C8 C7 120.06(14) . . ? C9 C10 C11 120.06(14) . . ? C15 C14 C13 119.98(13) . . ? C10 C11 C6 119.51(13) . . ? C8 C7 C6 119.46(13) . . ? C8 C9 C10 120.57(13) . . ? C37 C38 C39 120.20(14) . . ? C21 C22 C23 120.20(14) . . ? C52 C51 C50 120.37(14) . . ? C74 C75 C76 120.05(13) . . ? C20 C21 C22 120.41(15) . . ? C19 C20 C21 119.91(15) . . ? C70 C69 C68 120.44(13) . . ? C14 C15 C16 120.38(13) . . ? C15 C16 C17 119.90(14) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.471 _refine_diff_density_min -0.301 _refine_diff_density_rms 0.048 _database_code_depnum_ccdc_archive 'CCDC 928307' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_12053-final #TrackingRef '18538_web_deposit_cif_file_1_DanielTofan_1363226975.MoP4_12053-final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H110 Cl3 Mo N3 O14 P4' _chemical_formula_weight 1291.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.722(2) _cell_length_b 23.246(4) _cell_length_c 23.461(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.933(3) _cell_angle_gamma 90.00 _cell_volume 6834(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9949 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 30.43 _exptl_crystal_description Plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.255 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2760 _exptl_absorpt_coefficient_mu 0.458 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8749 _exptl_absorpt_correction_T_max 0.9775 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; 'Siemens three-circle diffractometer, Bruker APEX CCD' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 160859 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_av_sigmaI/netI 0.0305 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 30.51 _reflns_number_total 20812 _reflns_number_gt 15427 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2011.4.0 (Bruker-AXS, 2011)' _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2011)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0853P)^2^+9.7483P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20812 _refine_ls_number_parameters 966 _refine_ls_number_restraints 1129 _refine_ls_R_factor_all 0.0921 _refine_ls_R_factor_gt 0.0668 _refine_ls_wR_factor_ref 0.1939 _refine_ls_wR_factor_gt 0.1730 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.57386(6) 0.24053(3) 0.31142(3) 0.03364(15) Uani 1 1 d U . . P2 P 0.58788(6) 0.36580(3) 0.30086(3) 0.03306(15) Uani 1 1 d U . . P3 P 0.49142(8) 0.33580(3) 0.18427(3) 0.04269(19) Uani 1 1 d U . . Mo1 Mo 0.34487(3) 0.308754(18) 0.29564(2) 0.03369(12) Uani 0.8469(18) 1 d PU A 1 O1M O 0.3115(5) 0.3186(3) 0.3656(3) 0.0526(15) Uani 0.8469(18) 1 d PU A 1 O2M O 0.2539(2) 0.25970(12) 0.26501(14) 0.0454(6) Uani 0.8469(18) 1 d PU A 1 Cl1 Cl 0.25091(8) 0.39242(4) 0.25627(5) 0.0486(3) Uani 0.8469(18) 1 d PU A 1 P4 P 0.62632(14) 0.23038(7) 0.19409(9) 0.0379(3) Uani 0.8469(18) 1 d PU A 1 O1 O 0.46127(18) 0.25063(9) 0.32279(10) 0.0322(4) Uani 0.8469(18) 1 d PU A 1 O2 O 0.4789(5) 0.3667(3) 0.3182(2) 0.0299(10) Uani 0.8469(18) 1 d PU A 1 O3 O 0.4106(2) 0.30847(9) 0.21679(10) 0.0352(4) Uani 0.8469(18) 1 d PU A 1 O12 O 0.6334(7) 0.3016(3) 0.3114(3) 0.0334(11) Uani 0.8469(18) 1 d PU A 1 O23 O 0.5717(4) 0.3715(2) 0.2302(2) 0.0379(10) Uani 0.8469(18) 1 d PU A 1 O14 O 0.5613(2) 0.21756(9) 0.24862(10) 0.0301(4) Uani 0.8469(18) 1 d PU A 1 O34 O 0.5646(3) 0.28622(11) 0.16680(14) 0.0412(7) Uani 0.8469(18) 1 d PU A 1 O11 O 0.6392(3) 0.20135(15) 0.35400(14) 0.0428(7) Uani 0.8469(18) 1 d PU A 1 O22 O 0.6704(5) 0.4080(2) 0.3279(3) 0.0414(10) Uani 0.8469(18) 1 d PU A 1 O33 O 0.4518(3) 0.37064(12) 0.13362(13) 0.0511(7) Uani 0.8469(18) 1 d PU A 1 O43 O 0.5984(4) 0.1822(2) 0.1537(3) 0.0461(12) Uani 0.8469(18) 1 d PU A 1 O44 O 0.7365(2) 0.24242(15) 0.21765(16) 0.0602(8) Uani 0.8469(18) 1 d PU A 1 Mo1A Mo 0.33358(14) 0.32946(12) 0.26624(16) 0.0458(9) Uani 0.1531(18) 1 d PU A 2 Cl1A Cl 0.2975(9) 0.3070(6) 0.3540(6) 0.047(2) Uani 0.1531(18) 1 d PU A 2 O1N O 0.2284(16) 0.3837(8) 0.2740(9) 0.0486(3) Uani 0.1531(18) 1 d PU A 2 O2N O 0.2486(13) 0.2835(10) 0.2264(10) 0.067(4) Uani 0.1531(18) 1 d PU A 2 P4A P 0.6044(9) 0.2221(5) 0.1884(6) 0.0379(3) Uani 0.1531(18) 1 d PU A 2 O1A O 0.4516(10) 0.2609(5) 0.2776(7) 0.042(3) Uani 0.1531(18) 1 d PU A 2 O2A O 0.473(3) 0.3755(17) 0.3062(16) 0.031(4) Uani 0.1531(18) 1 d PU A 2 O3A O 0.4002(13) 0.3525(8) 0.1960(7) 0.056(3) Uani 0.1531(18) 1 d PU A 2 O12A O 0.624(4) 0.3011(18) 0.3245(14) 0.026(4) Uani 0.1531(18) 1 d PU A 2 O23A O 0.592(2) 0.3618(11) 0.2403(13) 0.029(3) Uani 0.1531(18) 1 d PU A 2 O14A O 0.6221(14) 0.2245(6) 0.2511(6) 0.037(3) Uani 0.1531(18) 1 d PU A 2 O34A O 0.5163(13) 0.2792(8) 0.1705(8) 0.042(3) Uani 0.1531(18) 1 d PU A 2 O11A O 0.5855(17) 0.2018(8) 0.3483(9) 0.048(4) Uani 0.1531(18) 1 d PU A 2 O22A O 0.658(3) 0.3981(16) 0.3185(18) 0.052(6) Uani 0.1531(18) 1 d PU A 2 O33A O 0.524(2) 0.3798(7) 0.1311(8) 0.074(6) Uani 0.1531(18) 1 d PU A 2 O43A O 0.558(2) 0.1792(13) 0.1508(14) 0.037(5) Uani 0.1531(18) 1 d PU A 2 O44A O 0.7202(13) 0.2683(7) 0.1786(9) 0.058(4) Uani 0.1531(18) 1 d PU A 2 C1S C 0.1925(5) 0.3639(3) 0.1081(3) 0.0995(17) Uani 1 1 d DU . . H1S1 H 0.2701 0.3662 0.1077 0.119 Uiso 1 1 calc R B 1 H1S2 H 0.1822 0.3546 0.1479 0.119 Uiso 1 1 calc R B 1 Cl1S Cl 0.1313(12) 0.4300(6) 0.0862(14) 0.323(10) Uani 0.439(17) 1 d PDU C 1 Cl2S Cl 0.1377(14) 0.3132(7) 0.0628(7) 0.276(9) Uani 0.439(17) 1 d PDU C 1 Cl1P Cl 0.1299(4) 0.4298(2) 0.10638(19) 0.115(2) Uani 0.561(17) 1 d PDU C 2 Cl2P Cl 0.1340(3) 0.31537(19) 0.05455(15) 0.0944(18) Uani 0.561(17) 1 d PDU C 2 N1 N 0.5639(3) 0.04722(11) 0.25279(14) 0.0547(7) Uani 1 1 d U . . C111 C 0.5448(3) 0.00866(14) 0.19934(17) 0.0553(9) Uani 1 1 d U . . H11A H 0.6032 -0.0200 0.2027 0.066 Uiso 1 1 calc R . . H11B H 0.4773 -0.0127 0.1989 0.066 Uiso 1 1 calc R . . C112 C 0.5385(5) 0.04004(17) 0.14198(19) 0.0811(15) Uani 1 1 d U . . H11C H 0.6063 0.0608 0.1415 0.097 Uiso 1 1 calc R . . H11D H 0.4804 0.0688 0.1381 0.097 Uiso 1 1 calc R . . C113 C 0.5179(4) -0.00139(19) 0.0910(2) 0.0755(13) Uani 1 1 d U . . H11E H 0.4568 -0.0263 0.0954 0.091 Uiso 1 1 calc R . . H11F H 0.4973 0.0212 0.0550 0.091 Uiso 1 1 calc R . . C114 C 0.6117(4) -0.0391(2) 0.0845(2) 0.0779(13) Uani 1 1 d U . . H11G H 0.6751 -0.0151 0.0846 0.117 Uiso 1 1 calc R . . H11H H 0.5959 -0.0602 0.0478 0.117 Uiso 1 1 calc R . . H11I H 0.6251 -0.0664 0.1167 0.117 Uiso 1 1 calc R . . C121 C 0.5694(4) 0.00783(15) 0.30607(17) 0.0615(10) Uani 1 1 d U . . H12A H 0.4996 -0.0116 0.3041 0.074 Uiso 1 1 calc R . . H12B H 0.6236 -0.0224 0.3041 0.074 Uiso 1 1 calc R . . C122 C 0.5970(5) 0.03842(18) 0.36491(19) 0.0845(16) Uani 1 1 d U . . H12C H 0.6712 0.0530 0.3698 0.101 Uiso 1 1 calc R . . H12D H 0.5491 0.0719 0.3654 0.101 Uiso 1 1 calc R . . C123 C 0.5863(5) -0.00082(19) 0.41512(19) 0.0841(15) Uani 1 1 d U . . H12E H 0.6215 0.0173 0.4517 0.101 Uiso 1 1 calc R . . H12F H 0.6232 -0.0376 0.4106 0.101 Uiso 1 1 calc R . . C124 C 0.4681(6) -0.0130(3) 0.4186(3) 0.1037(18) Uani 1 1 d U . . H12G H 0.4316 0.0233 0.4236 0.155 Uiso 1 1 calc R . . H12H H 0.4642 -0.0383 0.4516 0.155 Uiso 1 1 calc R . . H12I H 0.4335 -0.0318 0.3828 0.155 Uiso 1 1 calc R . . C131 C 0.4765(4) 0.09150(15) 0.2503(2) 0.0631(10) Uani 1 1 d U . . H13A H 0.4766 0.1158 0.2156 0.076 Uiso 1 1 calc R . . H13B H 0.4935 0.1167 0.2847 0.076 Uiso 1 1 calc R . . C132 C 0.3656(4) 0.06760(19) 0.2481(3) 0.0852(15) Uani 1 1 d U . . H13C H 0.3613 0.0467 0.2844 0.102 Uiso 1 1 calc R . . H13D H 0.3484 0.0404 0.2154 0.102 Uiso 1 1 calc R . . C133 C 0.2856(5) 0.1180(3) 0.2404(4) 0.108(2) Uani 1 1 d U . . H13E H 0.3021 0.1441 0.2741 0.130 Uiso 1 1 calc R . . H13F H 0.2942 0.1401 0.2054 0.130 Uiso 1 1 calc R . . C134 C 0.1743(6) 0.0985(5) 0.2348(5) 0.176(4) Uani 1 1 d U . . H13G H 0.1521 0.0807 0.1968 0.264 Uiso 1 1 calc R . . H13H H 0.1281 0.1315 0.2388 0.264 Uiso 1 1 calc R . . H13I H 0.1685 0.0703 0.2651 0.264 Uiso 1 1 calc R . . C141 C 0.6664(4) 0.08164(15) 0.25591(17) 0.0594(9) Uani 1 1 d U . . H14A H 0.6594 0.1070 0.2216 0.071 Uiso 1 1 calc R . . H14B H 0.6748 0.1066 0.2906 0.071 Uiso 1 1 calc R . . C142 C 0.7657(4) 0.04591(18) 0.2586(2) 0.0752(13) Uani 1 1 d U E . H14C H 0.7585 0.0205 0.2243 0.090 Uiso 1 1 calc R . . H14D H 0.7755 0.0214 0.2936 0.090 Uiso 1 1 calc R . . C143 C 0.8624(5) 0.0850(3) 0.2602(4) 0.113(2) Uani 1 1 d U . . H14E H 0.8562 0.1054 0.2228 0.136 Uiso 1 1 calc R D 1 H14F H 0.8621 0.1142 0.2908 0.136 Uiso 1 1 calc R D 1 C144 C 0.9486(9) 0.0591(8) 0.2694(10) 0.218(11) Uani 0.592(13) 1 d PU E 1 H14G H 1.0071 0.0866 0.2702 0.327 Uiso 0.592(13) 1 calc PR E 1 H14H H 0.9507 0.0308 0.2387 0.327 Uiso 0.592(13) 1 calc PR E 1 H14I H 0.9562 0.0393 0.3068 0.327 Uiso 0.592(13) 1 calc PR E 1 C148 C 0.9021(10) 0.1104(6) 0.3197(8) 0.115(6) Uani 0.408(13) 1 d PU E 2 H14J H 0.9177 0.0793 0.3481 0.172 Uiso 0.408(13) 1 calc PR E 2 H14K H 0.8471 0.1356 0.3306 0.172 Uiso 0.408(13) 1 calc PR E 2 H14L H 0.9672 0.1327 0.3188 0.172 Uiso 0.408(13) 1 calc PR E 2 N2 N 0.5030(3) 0.26536(13) -0.00224(12) 0.0575(8) Uani 1 1 d U . . C211 C 0.5564(4) 0.21769(16) -0.03259(15) 0.0569(9) Uani 1 1 d U G . H21A H 0.4999 0.1926 -0.0537 0.068 Uiso 1 1 calc R . . H21B H 0.5940 0.2357 -0.0616 0.068 Uiso 1 1 calc R . . C212 C 0.6346(5) 0.18073(19) 0.00690(19) 0.0717(12) Uani 1 1 d U . . H21C H 0.6960 0.2043 0.0253 0.086 Uiso 1 1 calc R G . H21D H 0.5998 0.1642 0.0378 0.086 Uiso 1 1 calc R . . C213 C 0.6729(4) 0.1331(2) -0.0280(2) 0.0752(12) Uani 1 1 d U G . H21E H 0.7034 0.1503 -0.0602 0.090 Uiso 1 1 calc R . . H21F H 0.6111 0.1092 -0.0451 0.090 Uiso 1 1 calc R . . C214 C 0.7560(5) 0.0950(3) 0.0071(3) 0.1045(19) Uani 1 1 d U . . H21G H 0.8194 0.1178 0.0223 0.157 Uiso 1 1 calc R G . H21H H 0.7756 0.0641 -0.0175 0.157 Uiso 1 1 calc R . . H21I H 0.7268 0.0782 0.0394 0.157 Uiso 1 1 calc R . . C221 C 0.4400(4) 0.23992(19) 0.04157(17) 0.0678(11) Uani 1 1 d U G . H22A H 0.4901 0.2186 0.0712 0.081 Uiso 1 1 calc R . . H22B H 0.4099 0.2720 0.0614 0.081 Uiso 1 1 calc R . . C222 C 0.3499(5) 0.1999(2) 0.0168(2) 0.0843(15) Uani 1 1 d U . . H22C H 0.3770 0.1692 -0.0061 0.101 Uiso 1 1 calc R G . H22D H 0.2940 0.2215 -0.0092 0.101 Uiso 1 1 calc R . . C223 C 0.3031(6) 0.1733(3) 0.0668(3) 0.116(2) Uani 1 1 d U G . H22E H 0.3601 0.1524 0.0928 0.139 Uiso 1 1 calc R . . H22F H 0.2770 0.2045 0.0896 0.139 Uiso 1 1 calc R . . C224 C 0.2135(8) 0.1328(4) 0.0464(5) 0.187(5) Uani 1 1 d U . . H22G H 0.1770 0.1231 0.0787 0.280 Uiso 1 1 calc R G . H22H H 0.2417 0.0976 0.0316 0.280 Uiso 1 1 calc R . . H22I H 0.1628 0.1510 0.0155 0.280 Uiso 1 1 calc R . . C231 C 0.5858(4) 0.30500(17) 0.03124(15) 0.0636(10) Uani 1 1 d U G . H23A H 0.6340 0.2818 0.0600 0.076 Uiso 1 1 calc R . . H23B H 0.5488 0.3328 0.0529 0.076 Uiso 1 1 calc R . . C232 C 0.6540(4) 0.33877(18) -0.00525(17) 0.0689(11) Uani 1 1 d U . . H23C H 0.6833 0.3120 -0.0314 0.083 Uiso 1 1 calc R G . H23D H 0.6087 0.3673 -0.0294 0.083 Uiso 1 1 calc R . . C233 C 0.7448(5) 0.3695(2) 0.0330(2) 0.0843(14) Uani 1 1 d U G . H23E H 0.7867 0.3916 0.0087 0.101 Uiso 1 1 calc R F 1 H23F H 0.7155 0.3969 0.0586 0.101 Uiso 1 1 calc R F 1 C234 C 0.8074(12) 0.3323(6) 0.0648(6) 0.122(5) Uani 0.505(8) 1 d PU G 1 H23G H 0.7751 0.3208 0.0981 0.183 Uiso 0.505(8) 1 calc PR G 1 H23H H 0.8771 0.3500 0.0785 0.183 Uiso 0.505(8) 1 calc PR G 1 H23I H 0.8168 0.2983 0.0415 0.183 Uiso 0.505(8) 1 calc PR G 1 C241 C 0.439(3) 0.2975(19) -0.051(2) 0.056(4) Uani 0.505(8) 1 d PU G 1 H24A H 0.3860 0.2713 -0.0733 0.067 Uiso 0.505(8) 1 calc PR G 1 H24B H 0.4869 0.3112 -0.0773 0.067 Uiso 0.505(8) 1 calc PR G 1 C242 C 0.3819(13) 0.3485(9) -0.0304(11) 0.053(3) Uani 0.505(8) 1 d PU G 1 H24C H 0.4347 0.3776 -0.0131 0.064 Uiso 0.505(8) 1 calc PR G 1 H24D H 0.3411 0.3358 -0.0004 0.064 Uiso 0.505(8) 1 calc PR G 1 C243 C 0.3063(9) 0.3750(5) -0.0810(7) 0.057(3) Uani 0.505(8) 1 d PU G 1 H24E H 0.3476 0.3847 -0.1118 0.068 Uiso 0.505(8) 1 calc PR G 1 H24F H 0.2778 0.4113 -0.0679 0.068 Uiso 0.505(8) 1 calc PR G 1 C244 C 0.2112(6) 0.3360(3) -0.1073(3) 0.0504(17) Uani 0.505(8) 1 d PU G 1 H24G H 0.2382 0.3009 -0.1228 0.076 Uiso 0.505(8) 1 calc PR G 1 H24H H 0.1653 0.3567 -0.1385 0.076 Uiso 0.505(8) 1 calc PR G 1 H24I H 0.1699 0.3258 -0.0772 0.076 Uiso 0.505(8) 1 calc PR G 1 C238 C 0.8260(7) 0.4042(4) -0.0027(4) 0.065(2) Uani 0.495(8) 1 d PU G 2 H23J H 0.8810 0.4239 0.0248 0.097 Uiso 0.495(8) 1 calc PR G 2 H23K H 0.7854 0.4325 -0.0285 0.097 Uiso 0.495(8) 1 calc PR G 2 H23L H 0.8600 0.3767 -0.0255 0.097 Uiso 0.495(8) 1 calc PR G 2 C245 C 0.422(3) 0.297(2) -0.048(2) 0.056(4) Uani 0.495(8) 1 d PU G 2 H24J H 0.4611 0.3139 -0.0771 0.067 Uiso 0.495(8) 1 calc PR G 2 H24K H 0.3721 0.2679 -0.0688 0.067 Uiso 0.495(8) 1 calc PR G 2 C246 C 0.3536(16) 0.3452(10) -0.0276(11) 0.070(5) Uani 0.495(8) 1 d PU G 2 H24L H 0.4003 0.3776 -0.0120 0.084 Uiso 0.495(8) 1 calc PR G 2 H24M H 0.3178 0.3304 0.0037 0.084 Uiso 0.495(8) 1 calc PR G 2 C247 C 0.2662(14) 0.3673(8) -0.0801(8) 0.093(5) Uani 0.495(8) 1 d PU G 2 H24N H 0.3015 0.3828 -0.1113 0.112 Uiso 0.495(8) 1 calc PR G 2 H24O H 0.2193 0.3351 -0.0961 0.112 Uiso 0.495(8) 1 calc PR G 2 C248 C 0.1987(17) 0.4156(8) -0.0565(7) 0.199(11) Uani 0.495(8) 1 d PU G 2 H24P H 0.1781 0.4028 -0.0202 0.298 Uiso 0.495(8) 1 calc PR G 2 H24Q H 0.1344 0.4234 -0.0850 0.298 Uiso 0.495(8) 1 calc PR G 2 H24R H 0.2414 0.4508 -0.0496 0.298 Uiso 0.495(8) 1 calc PR G 2 N3 N -0.0435(3) 0.3340(2) 0.2992(2) 0.0918(13) Uani 1 1 d U . . C311 C -0.1316(3) 0.3623(2) 0.2584(2) 0.0698(11) Uani 1 1 d U H . H31A H -0.1717 0.3323 0.2337 0.084 Uiso 1 1 calc R . . H31B H -0.1814 0.3803 0.2812 0.084 Uiso 1 1 calc R . . C312 C -0.0959(5) 0.4066(2) 0.2206(3) 0.1006(17) Uani 1 1 d U . . H31C H -0.0509 0.3887 0.1950 0.121 Uiso 1 1 calc R H . H31D H -0.0527 0.4361 0.2445 0.121 Uiso 1 1 calc R . . C313 C -0.1916(6) 0.4343(3) 0.1846(3) 0.1083(19) Uani 1 1 d U H . H31E H -0.2355 0.4042 0.1622 0.130 Uiso 1 1 calc R . . H31F H -0.2353 0.4525 0.2107 0.130 Uiso 1 1 calc R . . C314 C -0.1638(9) 0.4783(3) 0.1441(4) 0.157(3) Uani 1 1 d U . . H31G H -0.1241 0.5096 0.1661 0.236 Uiso 1 1 calc R H . H31H H -0.2293 0.4937 0.1210 0.236 Uiso 1 1 calc R . . H31I H -0.1196 0.4608 0.1185 0.236 Uiso 1 1 calc R . . C321 C 0.0260(4) 0.3788(3) 0.3363(3) 0.107(2) Uani 1 1 d U H . H32A H 0.0812 0.3582 0.3637 0.128 Uiso 1 1 calc R . . H32B H 0.0632 0.4021 0.3106 0.128 Uiso 1 1 calc R . . C322 C -0.0324(5) 0.4192(4) 0.3705(4) 0.134(3) Uani 1 1 d U . . H32C H -0.0566 0.3978 0.4024 0.161 Uiso 1 1 calc R H . H32D H -0.0962 0.4348 0.3451 0.161 Uiso 1 1 calc R . . C323 C 0.0418(6) 0.4697(4) 0.3961(4) 0.145(3) Uani 1 1 d U H . H32E H 0.1027 0.4542 0.4239 0.174 Uiso 1 1 calc R . . H32F H 0.0707 0.4890 0.3645 0.174 Uiso 1 1 calc R . . C324 C -0.0181(11) 0.5125(6) 0.4261(7) 0.253(8) Uani 1 1 d U . . H32G H 0.0296 0.5443 0.4409 0.380 Uiso 1 1 calc R H . H32H H -0.0441 0.4937 0.4584 0.380 Uiso 1 1 calc R . . H32I H -0.0787 0.5275 0.3987 0.380 Uiso 1 1 calc R . . C331 C -0.0994(11) 0.3013(6) 0.3417(8) 0.077(3) Uani 0.515(10) 1 d PU H 1 H33A H -0.1503 0.2740 0.3194 0.092 Uiso 0.515(10) 1 calc PR H 1 H33B H -0.1418 0.3293 0.3602 0.092 Uiso 0.515(10) 1 calc PR H 1 C332 C -0.0282(15) 0.2677(9) 0.3897(9) 0.134(6) Uani 0.515(10) 1 d PU H 1 H33C H 0.0195 0.2949 0.4143 0.160 Uiso 0.515(10) 1 calc PR H 1 H33D H 0.0172 0.2408 0.3719 0.160 Uiso 0.515(10) 1 calc PR H 1 C333 C -0.093(2) 0.2330(13) 0.4284(12) 0.159(9) Uani 0.515(10) 1 d PU H 1 H33E H -0.1607 0.2529 0.4305 0.191 Uiso 0.515(10) 1 calc PR H 1 H33F H -0.0514 0.2299 0.4681 0.191 Uiso 0.515(10) 1 calc PR H 1 C334 C -0.1166(19) 0.1685(12) 0.4002(12) 0.242(12) Uani 0.515(10) 1 d PU H 1 H33G H -0.1612 0.1469 0.4229 0.363 Uiso 0.515(10) 1 calc PR H 1 H33H H -0.0490 0.1481 0.4008 0.363 Uiso 0.515(10) 1 calc PR H 1 H33I H -0.1539 0.1721 0.3602 0.363 Uiso 0.515(10) 1 calc PR H 1 C341 C 0.0395(8) 0.3010(5) 0.2790(6) 0.083(3) Uani 0.515(10) 1 d PU H 1 H34A H 0.0905 0.2863 0.3126 0.099 Uiso 0.515(10) 1 calc PR H 1 H34B H 0.0792 0.3261 0.2560 0.099 Uiso 0.515(10) 1 calc PR H 1 C342 C -0.0087(8) 0.2508(5) 0.2420(6) 0.071(3) Uani 0.515(10) 1 d PU H 1 H34C H 0.0382 0.2169 0.2511 0.085 Uiso 0.515(10) 1 calc PR H 1 H34D H -0.0786 0.2413 0.2527 0.085 Uiso 0.515(10) 1 calc PR H 1 C343 C -0.0242(11) 0.2617(6) 0.1787(6) 0.092(4) Uani 0.515(10) 1 d PU H 1 H34E H 0.0443 0.2750 0.1688 0.111 Uiso 0.515(10) 1 calc PR H 1 H34F H -0.0765 0.2933 0.1693 0.111 Uiso 0.515(10) 1 calc PR H 1 C344 C -0.0638(10) 0.2086(6) 0.1398(5) 0.087(3) Uani 0.515(10) 1 d PU H 1 H34G H -0.0176 0.1755 0.1519 0.131 Uiso 0.515(10) 1 calc PR H 1 H34H H -0.0613 0.2178 0.0993 0.131 Uiso 0.515(10) 1 calc PR H 1 H34I H -0.1373 0.1993 0.1439 0.131 Uiso 0.515(10) 1 calc PR H 1 C335 C -0.0936(17) 0.2864(9) 0.3263(11) 0.098(4) Uani 0.485(10) 1 d PU H 2 H33J H -0.1329 0.2616 0.2955 0.117 Uiso 0.485(10) 1 calc PR H 2 H33K H -0.1461 0.3026 0.3485 0.117 Uiso 0.485(10) 1 calc PR H 2 C336 C -0.0154(15) 0.2501(7) 0.3659(9) 0.121(5) Uani 0.485(10) 1 d PU H 2 H33L H 0.0146 0.2206 0.3428 0.145 Uiso 0.485(10) 1 calc PR H 2 H33M H 0.0442 0.2747 0.3848 0.145 Uiso 0.485(10) 1 calc PR H 2 C337 C -0.0624(19) 0.2227(10) 0.4088(11) 0.120(5) Uani 0.485(10) 1 d PU H 2 H33N H -0.0137 0.1917 0.4260 0.144 Uiso 0.485(10) 1 calc PR H 2 H33O H -0.1291 0.2041 0.3895 0.144 Uiso 0.485(10) 1 calc PR H 2 C338 C -0.0912(13) 0.2629(7) 0.4621(7) 0.105(4) Uani 0.485(10) 1 d PU H 2 H33P H -0.1254 0.2391 0.4882 0.157 Uiso 0.485(10) 1 calc PR H 2 H33Q H -0.1398 0.2938 0.4462 0.157 Uiso 0.485(10) 1 calc PR H 2 H33R H -0.0254 0.2796 0.4837 0.157 Uiso 0.485(10) 1 calc PR H 2 C345 C 0.0186(9) 0.2959(7) 0.2534(7) 0.104(4) Uani 0.485(10) 1 d PU H 2 H34J H 0.0505 0.3245 0.2301 0.125 Uiso 0.485(10) 1 calc PR H 2 H34K H 0.0790 0.2760 0.2777 0.125 Uiso 0.485(10) 1 calc PR H 2 C346 C -0.0362(11) 0.2510(6) 0.2105(7) 0.077(3) Uani 0.485(10) 1 d PU H 2 H34L H -0.0457 0.2151 0.2318 0.092 Uiso 0.485(10) 1 calc PR H 2 H34M H -0.1080 0.2653 0.1932 0.092 Uiso 0.485(10) 1 calc PR H 2 C347 C 0.0241(8) 0.2377(5) 0.1635(5) 0.076(3) Uani 0.485(10) 1 d PU H 2 H34N H 0.0967 0.2246 0.1807 0.091 Uiso 0.485(10) 1 calc PR H 2 H34O H 0.0314 0.2733 0.1413 0.091 Uiso 0.485(10) 1 calc PR H 2 C348 C -0.0299(11) 0.1917(6) 0.1227(7) 0.098(4) Uani 0.485(10) 1 d PU H 2 H34P H -0.0758 0.1681 0.1427 0.147 Uiso 0.485(10) 1 calc PR H 2 H34Q H 0.0245 0.1674 0.1099 0.147 Uiso 0.485(10) 1 calc PR H 2 H34R H -0.0731 0.2101 0.0889 0.147 Uiso 0.485(10) 1 calc PR H 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 P1 0.0396(4) 0.0286(3) 0.0348(3) -0.0045(2) 0.0124(3) 0.0030(3) P2 0.0302(3) 0.0261(3) 0.0451(4) -0.0087(3) 0.0125(3) -0.0018(2) P3 0.0614(5) 0.0315(3) 0.0368(4) -0.0004(3) 0.0128(3) 0.0128(3) Mo1 0.02746(14) 0.03221(17) 0.0433(2) -0.00653(15) 0.01151(13) -0.00058(11) O1M 0.054(3) 0.054(3) 0.050(3) 0.002(2) 0.011(2) -0.0096(18) O2M 0.0330(12) 0.0410(13) 0.0633(18) -0.0132(12) 0.0116(12) -0.0053(10) Cl1 0.0395(5) 0.0403(5) 0.0650(7) -0.0065(4) 0.0066(4) 0.0083(4) P4 0.0503(9) 0.0251(6) 0.0433(6) -0.0081(4) 0.0218(6) 0.0010(4) O1 0.0375(11) 0.0279(10) 0.0339(12) 0.0005(8) 0.0140(9) 0.0007(8) O2 0.0288(14) 0.026(2) 0.036(3) -0.0073(16) 0.0094(17) 0.0016(13) O3 0.0438(12) 0.0268(10) 0.0337(11) -0.0041(8) 0.0032(9) 0.0022(8) O12 0.0299(19) 0.0304(12) 0.041(3) -0.007(2) 0.010(2) 0.0016(11) O23 0.050(3) 0.026(2) 0.041(2) 0.0042(13) 0.0188(16) 0.0009(15) O14 0.0397(13) 0.0226(9) 0.0305(11) -0.0006(7) 0.0133(10) 0.0011(9) O34 0.068(2) 0.0238(11) 0.0386(13) 0.0039(9) 0.0274(16) 0.0102(13) O11 0.0501(18) 0.0443(14) 0.0339(13) 0.0052(10) 0.0073(14) 0.0160(15) O22 0.0356(18) 0.030(2) 0.060(3) -0.0226(16) 0.0126(16) -0.0121(13) O33 0.078(2) 0.0362(13) 0.0414(14) 0.0111(11) 0.0150(15) 0.0148(14) O43 0.077(3) 0.0274(15) 0.0395(18) -0.0064(12) 0.025(3) 0.002(2) O44 0.0449(12) 0.068(2) 0.076(2) 0.0027(17) 0.0324(13) 0.0035(13) Mo1A 0.0257(8) 0.0415(12) 0.069(2) -0.0169(13) 0.0057(8) 0.0047(7) Cl1A 0.032(3) 0.062(5) 0.051(4) -0.014(3) 0.017(3) 0.003(3) O1N 0.0395(5) 0.0403(5) 0.0650(7) -0.0065(4) 0.0066(4) 0.0083(4) O2N 0.038(7) 0.076(11) 0.086(10) -0.045(9) 0.006(7) 0.001(6) P4A 0.0503(9) 0.0251(6) 0.0433(6) -0.0081(4) 0.0218(6) 0.0010(4) O1A 0.033(5) 0.026(5) 0.069(9) -0.017(5) 0.017(5) -0.004(4) O2A 0.035(5) 0.023(8) 0.035(10) 0.001(7) 0.004(6) 0.005(5) O3A 0.049(6) 0.072(9) 0.044(6) -0.016(6) -0.002(5) 0.014(6) O12A 0.024(8) 0.033(5) 0.023(9) 0.000(6) 0.009(8) 0.003(5) O23A 0.035(8) 0.009(7) 0.044(6) 0.007(5) 0.007(5) -0.002(6) O14A 0.047(7) 0.034(6) 0.033(5) -0.002(4) 0.017(5) 0.011(6) O34A 0.038(7) 0.042(6) 0.045(8) -0.011(5) 0.005(7) 0.002(5) O11A 0.068(12) 0.036(7) 0.043(8) 0.010(5) 0.020(9) 0.011(9) O22A 0.049(9) 0.037(9) 0.075(13) -0.041(9) 0.020(10) -0.013(8) O33A 0.124(18) 0.058(9) 0.043(8) 0.018(7) 0.022(10) 0.035(12) O43A 0.058(14) 0.030(6) 0.027(7) 0.001(5) 0.015(10) -0.007(8) O44A 0.049(7) 0.042(8) 0.090(12) -0.005(8) 0.032(8) -0.008(6) C1S 0.070(3) 0.147(5) 0.079(3) -0.016(3) 0.006(3) -0.012(3) Cl1S 0.157(9) 0.253(10) 0.50(2) -0.005(13) -0.101(13) 0.059(9) Cl2S 0.333(19) 0.276(12) 0.207(12) -0.055(9) 0.013(10) -0.102(12) Cl1P 0.078(2) 0.151(3) 0.104(3) -0.043(2) -0.0198(16) 0.039(2) Cl2P 0.093(3) 0.129(3) 0.0574(18) -0.0274(15) 0.0032(13) -0.0307(19) N1 0.0750(19) 0.0260(11) 0.0642(17) -0.0045(11) 0.0154(15) -0.0150(12) C111 0.070(2) 0.0301(14) 0.065(2) -0.0088(13) 0.0080(18) -0.0096(14) C112 0.136(4) 0.0368(18) 0.060(2) -0.0106(16) -0.013(3) 0.010(2) C113 0.103(4) 0.049(2) 0.068(3) -0.0169(19) -0.002(2) 0.009(2) C114 0.108(4) 0.062(2) 0.071(3) 0.020(2) 0.036(3) 0.013(2) C121 0.090(3) 0.0330(15) 0.063(2) 0.0012(14) 0.018(2) -0.0204(16) C122 0.148(5) 0.045(2) 0.060(2) 0.0001(18) 0.016(3) -0.031(3) C123 0.154(5) 0.044(2) 0.055(2) 0.0006(17) 0.019(3) -0.025(3) C124 0.152(5) 0.075(3) 0.090(4) 0.009(3) 0.038(4) 0.006(4) C131 0.080(3) 0.0314(15) 0.080(3) -0.0080(16) 0.020(2) -0.0105(15) C132 0.080(3) 0.046(2) 0.131(5) -0.008(2) 0.019(3) -0.003(2) C133 0.099(4) 0.070(3) 0.165(6) 0.013(4) 0.052(4) 0.019(3) C134 0.105(5) 0.195(10) 0.241(11) 0.098(9) 0.065(6) 0.051(6) C141 0.086(3) 0.0360(15) 0.056(2) 0.0017(14) 0.0119(19) -0.0241(16) C142 0.078(3) 0.050(2) 0.090(3) 0.017(2) -0.004(2) -0.0216(19) C143 0.095(4) 0.091(4) 0.148(6) 0.020(4) 0.008(4) -0.040(3) C144 0.097(7) 0.164(17) 0.39(3) 0.018(19) 0.023(16) -0.012(8) C148 0.058(7) 0.078(9) 0.192(14) -0.032(9) -0.025(9) -0.026(6) N2 0.093(2) 0.0493(15) 0.0323(13) 0.0023(11) 0.0158(14) 0.0027(14) C211 0.086(3) 0.0478(18) 0.0396(17) -0.0002(13) 0.0177(17) -0.0013(17) C212 0.104(4) 0.059(2) 0.056(2) 0.0097(18) 0.024(2) 0.013(2) C213 0.074(3) 0.059(2) 0.091(3) -0.014(2) 0.010(2) -0.003(2) C214 0.107(5) 0.077(3) 0.134(5) 0.016(3) 0.033(4) 0.022(3) C221 0.106(3) 0.060(2) 0.0440(19) 0.0081(16) 0.029(2) 0.008(2) C222 0.114(4) 0.069(3) 0.082(3) 0.006(2) 0.049(3) -0.003(3) C223 0.128(5) 0.100(4) 0.137(6) 0.031(4) 0.074(5) -0.003(4) C224 0.181(9) 0.149(8) 0.258(12) 0.019(8) 0.118(9) -0.056(7) C231 0.104(3) 0.056(2) 0.0302(15) -0.0040(14) 0.0095(17) 0.0000(19) C232 0.109(3) 0.053(2) 0.045(2) -0.0010(16) 0.013(2) -0.006(2) C233 0.116(4) 0.068(3) 0.067(3) -0.009(2) 0.010(3) -0.011(3) C234 0.135(12) 0.096(9) 0.121(11) 0.001(8) -0.015(8) -0.004(8) C241 0.083(9) 0.053(2) 0.034(3) 0.002(2) 0.015(6) 0.002(5) C242 0.060(6) 0.050(4) 0.052(6) 0.000(4) 0.016(5) -0.006(4) C243 0.065(6) 0.035(3) 0.072(6) 0.010(3) 0.015(5) -0.003(3) C244 0.053(4) 0.047(4) 0.049(4) 0.005(3) 0.003(3) 0.005(3) C238 0.076(5) 0.058(5) 0.060(5) -0.007(4) 0.010(4) -0.020(4) C245 0.083(9) 0.053(2) 0.034(3) 0.002(2) 0.015(6) 0.002(5) C246 0.108(12) 0.062(7) 0.044(5) 0.009(5) 0.022(9) 0.019(8) C247 0.115(13) 0.104(11) 0.063(7) 0.032(8) 0.022(9) 0.036(9) C248 0.23(2) 0.26(2) 0.110(12) 0.036(13) 0.025(13) 0.164(18) N3 0.0344(17) 0.100(3) 0.143(4) -0.016(2) 0.021(2) 0.0022(18) C311 0.0456(19) 0.078(3) 0.090(3) -0.030(2) 0.0240(19) -0.0017(18) C312 0.092(4) 0.079(3) 0.143(5) -0.032(3) 0.053(3) -0.018(3) C313 0.127(5) 0.078(4) 0.121(5) -0.019(3) 0.025(4) -0.031(3) C314 0.215(10) 0.072(4) 0.195(8) -0.009(4) 0.065(7) -0.046(5) C321 0.040(2) 0.117(4) 0.158(6) -0.026(4) 0.002(3) -0.009(2) C322 0.064(3) 0.186(7) 0.154(6) -0.068(5) 0.023(4) -0.041(4) C323 0.085(4) 0.190(8) 0.154(7) -0.088(6) 0.002(4) -0.037(5) C324 0.210(12) 0.267(14) 0.299(16) -0.171(13) 0.090(11) -0.084(10) C331 0.037(4) 0.065(7) 0.122(9) -0.008(5) -0.003(4) -0.004(4) C332 0.082(9) 0.146(12) 0.156(13) 0.027(9) -0.026(8) -0.015(9) C333 0.131(17) 0.180(16) 0.159(19) 0.059(12) 0.005(14) 0.003(16) C334 0.19(2) 0.27(2) 0.28(3) -0.040(19) 0.089(19) -0.144(19) C341 0.024(4) 0.087(6) 0.133(9) -0.036(6) 0.004(5) -0.002(3) C342 0.038(4) 0.075(5) 0.102(7) -0.017(5) 0.020(5) 0.013(4) C343 0.082(7) 0.104(8) 0.101(7) -0.036(6) 0.041(6) -0.039(6) C344 0.082(7) 0.093(8) 0.096(7) -0.028(6) 0.041(6) -0.002(6) C335 0.067(7) 0.101(9) 0.120(11) -0.008(7) 0.002(7) 0.023(6) C336 0.082(8) 0.160(12) 0.120(11) 0.012(8) 0.016(8) 0.059(8) C337 0.090(11) 0.117(11) 0.149(12) 0.018(7) 0.006(9) 0.023(8) C338 0.078(8) 0.115(11) 0.121(11) 0.019(8) 0.016(8) 0.006(8) C345 0.021(5) 0.161(11) 0.130(10) -0.055(8) 0.009(5) 0.008(5) C346 0.053(6) 0.092(7) 0.090(9) -0.005(6) 0.021(6) 0.007(5) C347 0.057(5) 0.087(7) 0.087(7) -0.013(5) 0.019(5) 0.002(5) C348 0.077(8) 0.093(8) 0.118(10) -0.039(7) 0.001(7) 0.021(6) _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 P1 O11A 1.240(17) . ? P1 O11 1.494(3) . ? P1 O1 1.520(2) . ? P1 O14 1.549(2) . ? P1 O12A 1.56(5) . ? P1 O12 1.609(8) . ? P1 O14A 1.679(13) . ? P1 O1A 1.688(14) . ? P2 O22A 1.18(3) . ? P2 O23A 1.43(3) . ? P2 O22 1.496(3) . ? P2 O2A 1.51(4) . ? P2 O2 1.511(6) . ? P2 O12 1.605(7) . ? P2 O23 1.639(5) . ? P2 O12A 1.64(4) . ? P3 O3A 1.297(16) . ? P3 O34A 1.405(18) . ? P3 O33 1.454(3) . ? P3 O3 1.521(3) . ? P3 O34 1.579(3) . ? P3 O23 1.586(6) . ? P3 O33A 1.721(17) . ? P3 O23A 1.77(3) . ? Mo1 O2M 1.694(3) . ? Mo1 O1M 1.780(6) . ? Mo1 O1 2.025(2) . ? Mo1 O3 2.157(2) . ? Mo1 O2 2.166(7) . ? Mo1 Cl1 2.3841(12) . ? P4 O44 1.442(4) . ? P4 O43 1.470(5) . ? P4 O34 1.593(3) . ? P4 O14 1.666(3) . ? Mo1A O2N 1.685(17) . ? Mo1A O1N 1.870(19) . ? Mo1A O3A 2.051(19) . ? Mo1A O2A 2.14(4) . ? Mo1A O1A 2.174(13) . ? Mo1A Cl1A 2.247(15) . ? P4A O43A 1.39(3) . ? P4A O14A 1.451(19) . ? P4A O34A 1.74(2) . ? P4A O44A 1.869(18) . ? C1S Cl2S 1.657(12) . ? C1S Cl1P 1.724(8) . ? C1S Cl2P 1.755(7) . ? C1S Cl1S 1.759(13) . ? N1 C131 1.509(5) . ? N1 C141 1.520(5) . ? N1 C111 1.526(4) . ? N1 C121 1.541(5) . ? C111 C112 1.521(6) . ? C112 C113 1.523(5) . ? C113 C114 1.509(7) . ? C121 C122 1.539(6) . ? C122 C123 1.515(6) . ? C123 C124 1.547(9) . ? C131 C132 1.509(6) . ? C132 C133 1.542(7) . ? C133 C134 1.472(10) . ? C141 C142 1.504(7) . ? C142 C143 1.525(7) . ? C143 C144 1.236(12) . ? C143 C148 1.520(17) . ? N2 C241 1.49(4) . ? N2 C231 1.513(5) . ? N2 C221 1.528(5) . ? N2 C211 1.537(5) . ? N2 C245 1.55(4) . ? C211 C212 1.507(6) . ? C212 C213 1.506(6) . ? C213 C214 1.511(7) . ? C221 C222 1.512(7) . ? C222 C223 1.537(7) . ? C223 C224 1.492(11) . ? C231 C232 1.536(6) . ? C232 C233 1.514(7) . ? C233 C234 1.317(10) . ? C233 C238 1.649(10) . ? C241 C242 1.51(4) . ? C242 C243 1.52(2) . ? C243 C244 1.553(13) . ? C245 C246 1.54(4) . ? C246 C247 1.59(3) . ? C247 C248 1.57(2) . ? N3 C341 1.450(11) . ? N3 C335 1.47(2) . ? N3 C311 1.495(6) . ? N3 C331 1.522(17) . ? N3 C321 1.535(7) . ? N3 C345 1.691(15) . ? C311 C312 1.483(8) . ? C312 C313 1.501(9) . ? C313 C314 1.480(9) . ? C321 C322 1.511(9) . ? C322 C323 1.560(9) . ? C323 C324 1.502(13) . ? C331 C332 1.53(3) . ? C332 C333 1.55(3) . ? C333 C334 1.65(4) . ? C341 C342 1.519(14) . ? C342 C343 1.486(18) . ? C343 C344 1.565(15) . ? C335 C336 1.50(3) . ? C336 C337 1.41(3) . ? C337 C338 1.65(3) . ? C345 C346 1.531(18) . ? C346 C347 1.481(16) . ? C347 C348 1.519(16) . ? 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 O11A P1 O11 26.5(10) . . ? O11A P1 O1 89.5(10) . . ? O11 P1 O1 114.17(16) . . ? O11A P1 O14 113.2(10) . . ? O11 P1 O14 112.33(16) . . ? O1 P1 O14 105.92(14) . . ? O11A P1 O12A 121.6(17) . . ? O11 P1 O12A 104.8(16) . . ? O1 P1 O12A 101.3(15) . . ? O14 P1 O12A 118.1(11) . . ? O11A P1 O12 129.9(11) . . ? O11 P1 O12 109.3(3) . . ? O1 P1 O12 108.8(3) . . ? O14 P1 O12 106.0(2) . . ? O12A P1 O12 12.5(11) . . ? O11A P1 O14A 114.2(10) . . ? O11 P1 O14A 100.7(5) . . ? O1 P1 O14A 132.5(6) . . ? O14 P1 O14A 27.7(6) . . ? O12A P1 O14A 99.7(12) . . ? O12 P1 O14A 87.4(6) . . ? O11A P1 O1A 121.4(11) . . ? O11 P1 O1A 147.9(5) . . ? O1 P1 O1A 38.7(5) . . ? O14 P1 O1A 73.3(5) . . ? O12A P1 O1A 98.9(18) . . ? O12 P1 O1A 98.5(5) . . ? O14A P1 O1A 96.1(7) . . ? O22A P2 O23A 103(3) . . ? O22A P2 O22 6(2) . . ? O23A P2 O22 108.7(12) . . ? O22A P2 O2A 124(3) . . ? O23A P2 O2A 107.1(18) . . ? O22 P2 O2A 119.1(17) . . ? O22A P2 O2 125(2) . . ? O23A P2 O2 117.4(12) . . ? O22 P2 O2 119.1(4) . . ? O2A P2 O2 13.2(13) . . ? O22A P2 O12 108(2) . . ? O23A P2 O12 91.0(10) . . ? O22 P2 O12 109.7(4) . . ? O2A P2 O12 117.2(14) . . ? O2 P2 O12 107.2(3) . . ? O22A P2 O23 105(2) . . ? O23A P2 O23 12.4(11) . . ? O22 P2 O23 109.4(3) . . ? O2A P2 O23 96.7(13) . . ? O2 P2 O23 108.1(3) . . ? O12 P2 O23 102.1(3) . . ? O22A P2 O12A 108(3) . . ? O23A P2 O12A 102.6(14) . . ? O22 P2 O12A 108.7(18) . . ? O2A P2 O12A 109(2) . . ? O2 P2 O12A 98.1(15) . . ? O12 P2 O12A 12.2(11) . . ? O23 P2 O12A 113.3(11) . . ? O3A P3 O34A 125.1(11) . . ? O3A P3 O33 79.0(8) . . ? O34A P3 O33 113.2(8) . . ? O3A P3 O3 46.5(9) . . ? O34A P3 O3 85.6(8) . . ? O33 P3 O3 118.27(18) . . ? O3A P3 O34 149.6(9) . . ? O34A P3 O34 24.5(7) . . ? O33 P3 O34 109.31(17) . . ? O3 P3 O34 107.77(14) . . ? O3A P3 O23 101.2(7) . . ? O34A P3 O23 120.2(7) . . ? O33 P3 O23 110.8(2) . . ? O3 P3 O23 106.8(2) . . ? O34 P3 O23 102.7(2) . . ? O3A P3 O33A 108.4(12) . . ? O34A P3 O33A 107.2(10) . . ? O33 P3 O33A 33.9(9) . . ? O3 P3 O33A 152.0(9) . . ? O34 P3 O33A 90.9(7) . . ? O23 P3 O33A 88.5(9) . . ? O3A P3 O23A 107.3(13) . . ? O34A P3 O23A 109.1(11) . . ? O33 P3 O23A 121.3(8) . . ? O3 P3 O23A 103.5(10) . . ? O34 P3 O23A 93.4(10) . . ? O23 P3 O23A 11.7(8) . . ? O33A P3 O23A 95.8(13) . . ? O2M Mo1 O1M 102.9(2) . . ? O2M Mo1 O1 95.36(12) . . ? O1M Mo1 O1 94.3(3) . . ? O2M Mo1 O3 88.37(12) . . ? O1M Mo1 O3 168.7(2) . . ? O1 Mo1 O3 84.10(9) . . ? O2M Mo1 O2 166.89(19) . . ? O1M Mo1 O2 89.8(2) . . ? O1 Mo1 O2 80.55(16) . . ? O3 Mo1 O2 78.85(16) . . ? O2M Mo1 Cl1 97.16(11) . . ? O1M Mo1 Cl1 93.9(2) . . ? O1 Mo1 Cl1 163.13(7) . . ? O3 Mo1 Cl1 84.99(7) . . ? O2 Mo1 Cl1 84.75(15) . . ? O44 P4 O43 120.3(3) . . ? O44 P4 O34 112.0(2) . . ? O43 P4 O34 108.3(3) . . ? O44 P4 O14 108.6(2) . . ? O43 P4 O14 105.2(2) . . ? O34 P4 O14 100.30(16) . . ? P1 O1 Mo1 135.09(14) . . ? P2 O2 Mo1 130.2(4) . . ? P3 O3 Mo1 145.51(14) . . ? P2 O12 P1 131.5(6) . . ? P3 O23 P2 126.8(4) . . ? P1 O14 P4 133.26(17) . . ? P3 O34 P4 139.6(2) . . ? O2N Mo1A O1N 94.6(9) . . ? O2N Mo1A O3A 92.0(10) . . ? O1N Mo1A O3A 107.8(8) . . ? O2N Mo1A O2A 164.5(13) . . ? O1N Mo1A O2A 99.9(13) . . ? O3A Mo1A O2A 78.3(11) . . ? O2N Mo1A O1A 88.1(7) . . ? O1N Mo1A O1A 166.6(8) . . ? O3A Mo1A O1A 85.2(6) . . ? O2A Mo1A O1A 79.2(11) . . ? O2N Mo1A Cl1A 98.5(9) . . ? O1N Mo1A Cl1A 78.7(8) . . ? O3A Mo1A Cl1A 167.3(5) . . ? O2A Mo1A Cl1A 89.9(10) . . ? O1A Mo1A Cl1A 87.9(6) . . ? O43A P4A O14A 130.1(17) . . ? O43A P4A O34A 102.1(17) . . ? O14A P4A O34A 101.3(11) . . ? O43A P4A O44A 126.1(15) . . ? O14A P4A O44A 96.6(11) . . ? O34A P4A O44A 91.2(10) . . ? P1 O1A Mo1A 145.5(7) . . ? P2 O2A Mo1A 129(3) . . ? P3 O3A Mo1A 126.9(11) . . ? P1 O12A P2 133(3) . . ? P2 O23A P3 128(2) . . ? P4A O14A P1 148.0(12) . . ? P3 O34A P4A 145.1(13) . . ? Cl2S C1S Cl1P 118.4(8) . . ? Cl2S C1S Cl2P 5.7(8) . . ? Cl1P C1S Cl2P 114.7(4) . . ? Cl2S C1S Cl1S 108.5(8) . . ? Cl1P C1S Cl1S 15.7(11) . . ? Cl2P C1S Cl1S 103.9(8) . . ? C131 N1 C141 105.2(3) . . ? C131 N1 C111 110.9(3) . . ? C141 N1 C111 111.2(3) . . ? C131 N1 C121 111.5(3) . . ? C141 N1 C121 110.8(3) . . ? C111 N1 C121 107.2(2) . . ? C112 C111 N1 115.0(3) . . ? C111 C112 C113 111.6(3) . . ? C114 C113 C112 114.5(4) . . ? C122 C121 N1 115.1(3) . . ? C123 C122 C121 112.5(3) . . ? C122 C123 C124 111.7(5) . . ? N1 C131 C132 115.4(3) . . ? C131 C132 C133 108.5(4) . . ? C134 C133 C132 112.4(6) . . ? C142 C141 N1 114.7(3) . . ? C141 C142 C143 109.9(4) . . ? C144 C143 C148 83.4(13) . . ? C144 C143 C142 113.7(9) . . ? C148 C143 C142 113.2(8) . . ? C241 N2 C231 109(2) . . ? C241 N2 C221 115.6(17) . . ? C231 N2 C221 106.6(3) . . ? C241 N2 C211 103.4(17) . . ? C231 N2 C211 110.9(3) . . ? C221 N2 C211 111.0(3) . . ? C241 N2 C245 9(3) . . ? C231 N2 C245 113.3(19) . . ? C221 N2 C245 106.7(17) . . ? C211 N2 C245 108.4(17) . . ? C212 C211 N2 115.1(3) . . ? C213 C212 C211 109.0(4) . . ? C212 C213 C214 113.3(5) . . ? C222 C221 N2 115.5(3) . . ? C221 C222 C223 108.7(5) . . ? C224 C223 C222 112.6(7) . . ? N2 C231 C232 115.5(3) . . ? C233 C232 C231 110.9(4) . . ? C234 C233 C232 110.6(7) . . ? C234 C233 C238 103.7(9) . . ? C232 C233 C238 114.2(5) . . ? N2 C241 C242 112(3) . . ? C241 C242 C243 110(2) . . ? C242 C243 C244 114.7(10) . . ? C246 C245 N2 118(3) . . ? C245 C246 C247 110(2) . . ? C248 C247 C246 107.9(16) . . ? C341 N3 C335 97.9(10) . . ? C341 N3 C311 122.1(7) . . ? C335 N3 C311 105.9(10) . . ? C341 N3 C331 113.5(9) . . ? C335 N3 C331 19.7(9) . . ? C311 N3 C331 104.8(7) . . ? C341 N3 C321 99.4(5) . . ? C335 N3 C321 121.0(10) . . ? C311 N3 C321 111.0(4) . . ? C331 N3 C321 104.8(6) . . ? C341 N3 C345 21.3(6) . . ? C335 N3 C345 99.5(10) . . ? C311 N3 C345 101.8(6) . . ? C331 N3 C345 118.6(9) . . ? C321 N3 C345 115.4(6) . . ? C312 C311 N3 114.6(4) . . ? C311 C312 C313 109.4(5) . . ? C314 C313 C312 113.4(7) . . ? C322 C321 N3 115.8(4) . . ? C321 C322 C323 110.6(5) . . ? C324 C323 C322 110.9(7) . . ? N3 C331 C332 116.8(11) . . ? C331 C332 C333 112.9(16) . . ? C332 C333 C334 109(2) . . ? N3 C341 C342 110.3(7) . . ? C343 C342 C341 114.3(11) . . ? C342 C343 C344 115.0(12) . . ? N3 C335 C336 113.6(15) . . ? C337 C336 C335 112.3(16) . . ? C336 C337 C338 117.5(17) . . ? C346 C345 N3 124.3(9) . . ? C347 C346 C345 113.3(11) . . ? C346 C347 C348 112.4(11) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.199 _refine_diff_density_min -0.643 _refine_diff_density_rms 0.086 _database_code_depnum_ccdc_archive 'CCDC 928308'