Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _audit_creation_date 10-05-05 _publ_contact_author_name 'Pierre Braunstein' _publ_contact_author_address ; Laboratoire de Chimie de Coordn. UMR 7177 CNRS Universite Louis Pasteur 4 Rue Blaise Pascal Strasbourg Cedex 67070 FRANCE ; _publ_contact_author_phone 0390241308 _publ_contact_author_fax 0390241322 _publ_contact_author_email braunst@chimie.u-strasbg.fr _publ_contact_letter ; ; _publ_requested_category FM _publ_section_title ; Organometallic Building Blocks with Amino-Substituted Cyclopentadienyl and Boratabenzene Ligands for the Synthesis of Heterometallic Complexes and Clusters ; loop_ _publ_author_name _publ_author_address N.Auvray ; Laboratoire de Chimie de coordination, UMR CNRS 7513 Universite Louis Pasteur Strasbourg France ; 'T.Basu Baul' ; Institut fuer Anorganische Chemie RWTH Aachen Prof.-Pirlet-Str.1 52074 Aachen Germany ; P.Braunstein ; Laboratoire de Chimie de coordination, UMR CNRS 7513 Universite Louis Pasteur Strasbourg France ; P.Croizat ; Laboratoire de Chimie de coordination, UMR CNRS 7513 Universite Louis Pasteur Strasbourg France ; U.Englert ; Institut fuer Anorganische Chemie RWTH Aachen Prof.-Pirlet-Str.1 52074 Aachen Germany ; ; G.E.Herberich ; ; Institut fuer Anorganische Chemie RWTH Aachen Prof.-Pirlet-Str.1 52074 Aachen Germany ; R.Welter ; Laboratoire DECMET, UMR CNRS 7177 Universite Louis Pasteur Strasbourg France ; _publ_section_references ; Blessing, R.H. (1987). Crystallogr. Rev. 1, 3-58. Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. A.L. Spek, PLATON 98, Utrecht University, The Netherland, 1998. KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands. Otwinowski, Z. & Minor, W. (1997), Methods in Enzymology, 276, 307-326. Sheldrick, G.M. (1997). SHELXL97. Program for the refinement of crystal structures. University of Gottingen. Germany. ; data_bb3 _database_code_depnum_ccdc_archive 'CCDC 297952' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H23 B Cl Hg Mo N O3' _chemical_formula_sum 'C16 H23 B Cl Hg Mo N O3' _chemical_formula_weight 620.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 .6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B .0013 .0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_h-m 'P21/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.0320(12) _cell_length_b 14.026(3) _cell_length_c 19.843(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.908(8) _cell_angle_gamma 90.00 _cell_volume 3981.0(10) _cell_formula_units_Z 8 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8 _cell_measurement_theta_max 10 _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.069 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2352 _exptl_absorpt_coefficient_mu 8.480 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.513 _exptl_absorpt_correction_T_max 0.897 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 Enraf_Nonius_CAD4 _diffrn_measurement_method \q/2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% -2.92 _diffrn_reflns_number 11589 _diffrn_reflns_av_R_equivalents 0.0872 _diffrn_reflns_av_sigmaI/netI 0.1789 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 26.99 _reflns_number_total 8648 _reflns_number_gt 4197 _reflns_threshold_expression >2sigma(I) _computing_data_collection CAD4_(Enraf-Nonius,_1977) _computing_cell_refinement CAD4_(Enraf-Nonius,_1977) _computing_data_reduction PROCESS_MolEN_(Fair,_1990) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000062(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8648 _refine_ls_number_parameters 446 _refine_ls_number_restraints 202 _refine_ls_R_factor_all 0.1873 _refine_ls_R_factor_gt 0.0790 _refine_ls_wR_factor_ref 0.0940 _refine_ls_wR_factor_gt 0.0791 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.000 _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 Hg1 Hg 0.30759(5) 0.00166(4) 0.19477(4) 0.02779(15) Uani 1 1 d U . . Cl1 Cl 0.3784(3) 0.1504(3) 0.2431(2) 0.0378(10) Uani 1 1 d U . . Mo1 Mo 0.23343(8) -0.16832(9) 0.14450(6) 0.0203(3) Uani 1 1 d U . . C1 C 0.3172(10) -0.1474(10) 0.0850(7) 0.024(2) Uani 1 1 d U . . O1 O 0.3662(8) -0.1412(8) 0.0512(5) 0.047(3) Uani 1 1 d U . . C2 C 0.1331(10) -0.0687(12) 0.1108(7) 0.029(3) Uani 1 1 d U . . O2 O 0.0701(7) -0.0215(8) 0.0880(6) 0.051(3) Uani 1 1 d U . . C3 C 0.1574(10) -0.2211(11) 0.0546(7) 0.029(3) Uani 1 1 d U . . O3 O 0.1116(7) -0.2534(9) 0.0009(5) 0.053(3) Uani 1 1 d U . . C4 C 0.2034(8) -0.1872(10) 0.2548(6) 0.0210(19) Uani 1 1 d U . . H4 H 0.1673 -0.1385 0.2646 0.027 Uiso 1 1 calc R . . C5 C 0.1592(9) -0.2603(10) 0.2111(7) 0.024(2) Uani 1 1 d U . . C6 C 0.2129(9) -0.3212(10) 0.1782(6) 0.022(2) Uani 1 1 d U . . H6 H 0.1822 -0.3684 0.1467 0.029 Uiso 1 1 calc R . . C7 C 0.3105(10) -0.3100(9) 0.1933(7) 0.022(2) Uani 1 1 d U . . C8 C 0.3555(9) -0.2388(9) 0.2384(7) 0.0202(19) Uani 1 1 d U . . H8 H 0.4160 -0.2230 0.2394 0.026 Uiso 1 1 calc R . . N1 N 0.3587(7) -0.1374(8) 0.3522(5) 0.022(2) Uani 1 1 d U . . B1 B 0.3109(11) -0.1829(12) 0.2881(8) 0.024(3) Uani 1 1 d U . . C9 C 0.4598(9) -0.1451(10) 0.3887(7) 0.024(3) Uani 1 1 d U . . H9 H 0.4710 -0.1153 0.4353 0.032 Uiso 1 1 calc R . . C10 C 0.3045(10) -0.0862(10) 0.3934(7) 0.031(3) Uani 1 1 d U . . H10 H 0.2403 -0.0790 0.3619 0.040 Uiso 1 1 calc R . . C11 C 0.4925(10) -0.2457(10) 0.4020(7) 0.034(4) Uani 1 1 d U . . H11A H 0.4531 -0.2796 0.4238 0.044 Uiso 1 1 calc R . . H11B H 0.5558 -0.2466 0.4330 0.044 Uiso 1 1 calc R . . H11C H 0.4898 -0.2756 0.3580 0.044 Uiso 1 1 calc R . . C12 C 0.5152(10) -0.0872(11) 0.3502(7) 0.042(4) Uani 1 1 d U . . H12A H 0.4996 -0.1082 0.3019 0.055 Uiso 1 1 calc R . . H12B H 0.5809 -0.0961 0.3732 0.055 Uiso 1 1 calc R . . H12C H 0.5000 -0.0209 0.3514 0.055 Uiso 1 1 calc R . . C14 C 0.3426(11) 0.0125(10) 0.4138(8) 0.039(4) Uani 1 1 d U . . H14A H 0.4052 0.0081 0.4455 0.051 Uiso 1 1 calc R . . H14B H 0.3040 0.0453 0.4368 0.051 Uiso 1 1 calc R . . H14C H 0.3429 0.0469 0.3720 0.051 Uiso 1 1 calc R . . C13 C 0.2993(12) -0.1413(12) 0.4565(8) 0.051(5) Uani 1 1 d U . . H13A H 0.2687 -0.2011 0.4414 0.066 Uiso 1 1 calc R . . H13B H 0.2645 -0.1054 0.4811 0.066 Uiso 1 1 calc R . . H13C H 0.3613 -0.1526 0.4876 0.066 Uiso 1 1 calc R . . C15 C 0.0542(8) -0.2769(11) 0.1876(7) 0.035(4) Uani 1 1 d U . . H15A H 0.0229 -0.2186 0.1918 0.046 Uiso 1 1 calc R . . H15B H 0.0394 -0.3249 0.2170 0.046 Uiso 1 1 calc R . . H15C H 0.0339 -0.2977 0.1392 0.046 Uiso 1 1 calc R . . C16 C 0.3609(9) -0.3772(10) 0.1574(7) 0.034(4) Uani 1 1 d U . . H16A H 0.4044 -0.3417 0.1405 0.044 Uiso 1 1 calc R . . H16B H 0.3161 -0.4079 0.1182 0.044 Uiso 1 1 calc R . . H16C H 0.3940 -0.4244 0.1907 0.044 Uiso 1 1 calc R . . Hg2 Hg 0.19609(5) 0.21392(4) 0.30360(4) 0.02876(16) Uani 1 1 d U . . Cl2 Cl 0.1225(3) 0.0665(3) 0.2561(2) 0.0378(10) Uani 1 1 d U . . Mo2 Mo 0.26469(9) 0.38034(9) 0.36462(6) 0.0212(3) Uani 1 1 d U . . C1A C 0.3722(10) 0.2864(11) 0.3982(7) 0.029(3) Uani 1 1 d U . . O1A O 0.4322(7) 0.2351(8) 0.4150(6) 0.054(3) Uani 1 1 d U . . C2A C 0.1645(10) 0.3447(11) 0.4060(7) 0.034(3) Uani 1 1 d U . . O2A O 0.1060(7) 0.3318(8) 0.4311(5) 0.051(3) Uani 1 1 d U . . C3A C 0.3203(11) 0.4169(11) 0.4648(7) 0.033(3) Uani 1 1 d U . . O3A O 0.3512(8) 0.4336(8) 0.5244(5) 0.056(3) Uani 1 1 d U . . C4A C 0.1509(9) 0.4658(10) 0.2738(7) 0.026(2) Uani 1 1 d U . . H4A H 0.0887 0.4517 0.2685 0.033 Uiso 1 1 calc R . . C5A C 0.1993(10) 0.5311(10) 0.3268(7) 0.030(2) Uani 1 1 d U . . C6A C 0.2991(9) 0.5371(10) 0.3453(7) 0.027(2) Uani 1 1 d U . . H6A H 0.3305 0.5800 0.3802 0.035 Uiso 1 1 calc R . . C7A C 0.3525(9) 0.4797(10) 0.3122(7) 0.025(2) Uani 1 1 d U . . C8A C 0.3059(9) 0.4128(11) 0.2613(6) 0.024(2) Uani 1 1 d U . . H8A H 0.3397 0.3640 0.2489 0.031 Uiso 1 1 calc R . . B2 B 0.1988(10) 0.4183(13) 0.2253(8) 0.023(3) Uani 1 1 d U . . N2 N 0.1538(7) 0.3748(8) 0.1568(5) 0.023(2) Uani 1 1 d U . . C9A C 0.2044(10) 0.3237(12) 0.1171(8) 0.036(3) Uani 1 1 d U . . H9A H 0.2693 0.3197 0.1477 0.047 Uiso 1 1 calc R . . C10A C 0.0508(8) 0.3809(10) 0.1195(7) 0.020(3) Uani 1 1 d U . . H10A H 0.0390 0.3505 0.0731 0.025 Uiso 1 1 calc R . . C11A C 0.2068(10) 0.3737(11) 0.0498(8) 0.041(4) Uani 1 1 d U . . H11D H 0.2545 0.3455 0.0333 0.053 Uiso 1 1 calc R . . H11E H 0.2203 0.4401 0.0594 0.053 Uiso 1 1 calc R . . H11F H 0.1472 0.3670 0.0142 0.053 Uiso 1 1 calc R . . C12A C 0.1717(11) 0.2240(11) 0.1002(7) 0.040(4) Uani 1 1 d U . . H12D H 0.1561 0.1970 0.1395 0.052 Uiso 1 1 calc R . . H12E H 0.2205 0.1870 0.0910 0.052 Uiso 1 1 calc R . . H12F H 0.1175 0.2235 0.0590 0.052 Uiso 1 1 calc R . . C13A C 0.0170(9) 0.4822(10) 0.1069(8) 0.034(4) Uani 1 1 d U . . H13D H -0.0497 0.4827 0.0861 0.044 Uiso 1 1 calc R . . H13E H 0.0455 0.5126 0.0753 0.044 Uiso 1 1 calc R . . H13F H 0.0337 0.5159 0.1511 0.044 Uiso 1 1 calc R . . C14A C -0.0040(9) 0.3263(11) 0.1593(7) 0.034(4) Uani 1 1 d U . . H14D H 0.0001 0.3588 0.2027 0.044 Uiso 1 1 calc R . . H14E H 0.0215 0.2633 0.1697 0.044 Uiso 1 1 calc R . . H14F H -0.0682 0.3221 0.1307 0.044 Uiso 1 1 calc R . . C15A C 0.1503(10) 0.5925(10) 0.3659(8) 0.041(4) Uani 1 1 d U . . H15D H 0.1407 0.6548 0.3450 0.053 Uiso 1 1 calc R . . H15E H 0.1878 0.5973 0.4146 0.053 Uiso 1 1 calc R . . H15F H 0.0910 0.5646 0.3631 0.053 Uiso 1 1 calc R . . C16A C 0.4570(8) 0.4886(11) 0.3369(7) 0.035(4) Uani 1 1 d U . . H16D H 0.4845 0.4278 0.3333 0.046 Uiso 1 1 calc R . . H16E H 0.4774 0.5094 0.3853 0.046 Uiso 1 1 calc R . . H16F H 0.4760 0.5342 0.3080 0.046 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 Hg1 0.0316(3) 0.0180(3) 0.0313(3) -0.0037(3) 0.0062(3) -0.0014(3) Cl1 0.034(2) 0.025(2) 0.050(3) -0.011(2) 0.007(2) -0.0069(19) Mo1 0.0212(7) 0.0176(7) 0.0201(7) -0.0021(6) 0.0035(5) -0.0002(6) C1 0.035(6) 0.016(6) 0.022(6) 0.005(4) 0.009(5) 0.002(5) O1 0.067(8) 0.042(7) 0.047(7) -0.001(6) 0.039(6) -0.005(6) C2 0.030(5) 0.033(6) 0.017(7) -0.002(4) -0.002(4) 0.010(4) O2 0.034(6) 0.044(8) 0.060(8) 0.003(7) -0.009(6) 0.015(5) C3 0.031(6) 0.032(7) 0.021(3) -0.005(4) 0.005(4) -0.003(5) O3 0.047(7) 0.076(10) 0.029(6) -0.016(6) 0.001(5) -0.023(6) C4 0.024(4) 0.018(5) 0.022(4) -0.001(4) 0.008(4) 0.008(4) C5 0.024(4) 0.025(5) 0.027(6) -0.004(4) 0.012(4) -0.001(4) C6 0.031(4) 0.021(3) 0.020(6) -0.006(3) 0.014(5) -0.005(4) C7 0.030(4) 0.019(3) 0.022(5) 0.004(3) 0.018(4) 0.005(3) C8 0.020(4) 0.023(4) 0.020(4) 0.005(3) 0.009(3) 0.004(4) N1 0.029(4) 0.025(6) 0.017(5) 0.003(4) 0.015(4) -0.005(4) B1 0.022(5) 0.028(9) 0.023(3) -0.002(5) 0.007(4) 0.004(6) C9 0.032(5) 0.026(7) 0.019(7) -0.011(6) 0.013(4) -0.007(6) C10 0.038(8) 0.027(8) 0.025(7) -0.001(5) 0.009(7) 0.011(7) C11 0.052(9) 0.028(7) 0.014(8) -0.009(6) -0.001(7) 0.002(6) C12 0.033(7) 0.048(10) 0.045(10) -0.007(8) 0.010(8) -0.029(8) C14 0.040(9) 0.031(7) 0.048(11) -0.008(7) 0.015(8) 0.004(8) C13 0.079(13) 0.055(11) 0.034(9) -0.009(8) 0.041(9) -0.019(11) C15 0.027(5) 0.036(10) 0.047(10) 0.004(8) 0.017(6) -0.004(5) C16 0.032(7) 0.025(7) 0.050(10) -0.009(6) 0.022(7) 0.004(6) Hg2 0.0335(3) 0.0192(3) 0.0301(3) -0.0037(3) 0.0046(3) -0.0030(3) Cl2 0.040(2) 0.023(2) 0.049(3) -0.007(2) 0.010(2) -0.0053(19) Mo2 0.0259(7) 0.0170(7) 0.0176(7) -0.0013(6) 0.0024(6) 0.0006(6) C1A 0.034(5) 0.020(6) 0.026(7) 0.003(5) -0.001(4) 0.004(4) O1A 0.048(7) 0.039(8) 0.062(8) -0.005(7) -0.001(6) 0.022(5) C2A 0.041(6) 0.040(7) 0.024(7) 0.001(4) 0.014(5) -0.004(6) O2A 0.043(7) 0.067(9) 0.049(7) -0.003(7) 0.024(5) -0.014(6) C3A 0.058(8) 0.016(7) 0.016(3) 0.001(3) -0.002(4) -0.004(6) O3A 0.078(8) 0.037(7) 0.027(4) -0.018(6) -0.023(6) 0.008(7) C4A 0.025(4) 0.027(4) 0.021(4) 0.004(3) 0.002(3) 0.003(4) C5A 0.032(5) 0.020(3) 0.030(6) 0.001(3) -0.002(4) 0.008(4) C6A 0.034(5) 0.017(3) 0.021(6) 0.004(4) -0.003(5) 0.001(4) C7A 0.023(4) 0.022(5) 0.024(6) 0.002(4) -0.002(4) -0.005(4) C8A 0.017(4) 0.034(6) 0.015(4) 0.000(4) -0.002(3) -0.006(4) B2 0.015(5) 0.033(10) 0.018(3) 0.000(4) 0.000(4) -0.012(7) N2 0.017(4) 0.026(6) 0.020(5) -0.001(4) -0.003(3) -0.002(4) C9A 0.019(7) 0.052(9) 0.029(6) -0.008(6) -0.004(6) 0.011(7) C10A 0.012(4) 0.025(7) 0.016(7) 0.001(6) -0.004(4) -0.001(5) C11A 0.040(10) 0.044(10) 0.045(9) -0.022(7) 0.023(8) -0.018(9) C12A 0.060(11) 0.037(7) 0.015(8) 0.001(6) -0.001(7) 0.022(8) C13A 0.028(8) 0.026(7) 0.042(10) -0.001(7) 0.004(7) 0.005(6) C14A 0.031(7) 0.031(8) 0.041(9) -0.006(7) 0.014(7) -0.009(7) C15A 0.042(8) 0.020(7) 0.051(10) -0.010(7) 0.000(7) 0.012(6) C16A 0.024(4) 0.047(11) 0.028(8) -0.011(8) -0.003(5) -0.015(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 Hg1 Cl1 2.404(4) . ? Hg1 Mo1 2.6904(16) . ? Mo1 C3 1.944(14) . ? Mo1 C1 1.995(14) . ? Mo1 C2 2.013(15) . ? Mo1 C6 2.295(13) . ? Mo1 C7 2.353(13) . ? Mo1 C5 2.358(13) . ? Mo1 C4 2.381(12) . ? Mo1 C8 2.390(12) . ? C1 O1 1.141(14) . ? C2 O2 1.130(15) . ? C3 O3 1.169(15) . ? C4 C5 1.374(17) . ? C4 B1 1.547(18) . ? C4 H4 0.9300 . ? C5 C6 1.459(17) . ? C5 C15 1.521(16) . ? C6 C7 1.413(17) . ? C6 H6 0.9300 . ? C7 C8 1.371(17) . ? C7 C16 1.518(17) . ? C8 B1 1.565(19) . ? C8 H8 0.9300 . ? N1 B1 1.406(18) . ? N1 C9 1.473(16) . ? N1 C10 1.504(16) . ? C9 C11 1.491(18) . ? C9 C12 1.525(17) . ? C9 H9 0.9800 . ? C10 C13 1.493(18) . ? C10 C14 1.505(18) . ? C10 H10 0.9800 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? Hg2 Cl2 2.397(4) . ? Hg2 Mo2 2.6852(15) . ? Mo2 C3A 1.972(14) . ? Mo2 C2A 1.989(15) . ? Mo2 C1A 2.032(15) . ? Mo2 C6A 2.317(14) . ? Mo2 C5A 2.355(14) . ? Mo2 C8A 2.361(12) . ? Mo2 C7A 2.369(13) . ? Mo2 C4A 2.390(13) . ? C1A O1A 1.121(15) . ? C2A O2A 1.150(15) . ? C3A O3A 1.154(15) . ? C4A C5A 1.415(17) . ? C4A B2 1.522(19) . ? C4A H4A 0.9300 . ? C5A C6A 1.434(18) . ? C5A C15A 1.495(18) . ? C6A C7A 1.431(17) . ? C6A H6A 0.9300 . ? C7A C8A 1.398(17) . ? C7A C16A 1.500(16) . ? C8A B2 1.549(17) . ? C8A H8A 0.9300 . ? B2 N2 1.453(17) . ? N2 C9A 1.441(16) . ? N2 C10A 1.500(14) . ? C9A C12A 1.487(19) . ? C9A C11A 1.519(19) . ? C9A H9A 0.9800 . ? C10A C13A 1.504(17) . ? C10A C14A 1.512(17) . ? C10A H10A 0.9800 . ? C11A H11D 0.9600 . ? C11A H11E 0.9600 . ? C11A H11F 0.9600 . ? C12A H12D 0.9600 . ? C12A H12E 0.9600 . ? C12A H12F 0.9600 . ? C13A H13D 0.9600 . ? C13A H13E 0.9600 . ? C13A H13F 0.9600 . ? C14A H14D 0.9600 . ? C14A H14E 0.9600 . ? C14A H14F 0.9600 . ? C15A H15D 0.9600 . ? C15A H15E 0.9600 . ? C15A H15F 0.9600 . ? C16A H16D 0.9600 . ? C16A H16E 0.9600 . ? C16A H16F 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Hg1 Mo1 177.84(11) . . ? C3 Mo1 C1 79.2(6) . . ? C3 Mo1 C2 77.9(6) . . ? C1 Mo1 C2 104.3(6) . . ? C3 Mo1 C6 79.5(5) . . ? C1 Mo1 C6 118.4(5) . . ? C2 Mo1 C6 126.2(5) . . ? C3 Mo1 C7 97.6(6) . . ? C1 Mo1 C7 92.7(5) . . ? C2 Mo1 C7 161.1(5) . . ? C6 Mo1 C7 35.4(4) . . ? C3 Mo1 C5 93.4(5) . . ? C1 Mo1 C5 154.9(5) . . ? C2 Mo1 C5 97.5(5) . . ? C6 Mo1 C5 36.5(4) . . ? C7 Mo1 C5 64.2(5) . . ? C3 Mo1 C4 125.2(5) . . ? C1 Mo1 C4 153.2(5) . . ? C2 Mo1 C4 92.7(5) . . ? C6 Mo1 C4 63.1(4) . . ? C7 Mo1 C4 74.7(4) . . ? C5 Mo1 C4 33.7(4) . . ? C3 Mo1 C8 130.6(6) . . ? C1 Mo1 C8 92.8(5) . . ? C2 Mo1 C8 149.7(5) . . ? C6 Mo1 C8 61.7(4) . . ? C7 Mo1 C8 33.6(4) . . ? C5 Mo1 C8 73.7(4) . . ? C4 Mo1 C8 63.6(4) . . ? C3 Mo1 Hg1 137.5(5) . . ? C1 Mo1 Hg1 79.9(4) . . ? C2 Mo1 Hg1 72.0(4) . . ? C6 Mo1 Hg1 142.9(3) . . ? C7 Mo1 Hg1 120.0(4) . . ? C5 Mo1 Hg1 119.4(3) . . ? C4 Mo1 Hg1 86.1(3) . . ? C8 Mo1 Hg1 86.9(3) . . ? O1 C1 Mo1 175.9(13) . . ? O2 C2 Mo1 171.8(14) . . ? O3 C3 Mo1 179.4(14) . . ? C5 C4 B1 122.5(12) . . ? C5 C4 Mo1 72.2(7) . . ? B1 C4 Mo1 85.5(8) . . ? C5 C4 H4 118.7 . . ? B1 C4 H4 118.7 . . ? Mo1 C4 H4 113.5 . . ? C4 C5 C6 119.5(12) . . ? C4 C5 C15 124.2(12) . . ? C6 C5 C15 116.0(12) . . ? C4 C5 Mo1 74.0(8) . . ? C6 C5 Mo1 69.4(7) . . ? C15 C5 Mo1 122.5(9) . . ? C7 C6 C5 121.4(12) . . ? C7 C6 Mo1 74.6(8) . . ? C5 C6 Mo1 74.1(8) . . ? C7 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? Mo1 C6 H6 123.5 . . ? C8 C7 C6 119.5(12) . . ? C8 C7 C16 122.7(13) . . ? C6 C7 C16 117.8(12) . . ? C8 C7 Mo1 74.7(8) . . ? C6 C7 Mo1 70.1(8) . . ? C16 C7 Mo1 125.7(9) . . ? C7 C8 B1 123.7(12) . . ? C7 C8 Mo1 71.7(8) . . ? B1 C8 Mo1 84.7(8) . . ? C7 C8 H8 118.2 . . ? B1 C8 H8 118.2 . . ? Mo1 C8 H8 115.4 . . ? B1 N1 C9 125.1(11) . . ? B1 N1 C10 119.8(11) . . ? C9 N1 C10 114.7(10) . . ? N1 B1 C4 125.5(12) . . ? N1 B1 C8 126.8(12) . . ? C4 B1 C8 107.7(12) . . ? N1 C9 C11 113.0(12) . . ? N1 C9 C12 110.7(11) . . ? C11 C9 C12 113.1(12) . . ? N1 C9 H9 106.5 . . ? C11 C9 H9 106.5 . . ? C12 C9 H9 106.5 . . ? C13 C10 N1 112.7(12) . . ? C13 C10 C14 111.4(13) . . ? N1 C10 C14 111.1(12) . . ? C13 C10 H10 107.1 . . ? N1 C10 H10 107.1 . . ? C14 C10 H10 107.1 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C14 H14A 109.5 . . ? C10 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C10 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C5 C15 H15A 109.5 . . ? C5 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C5 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C7 C16 H16A 109.5 . . ? C7 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C7 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Cl2 Hg2 Mo2 173.72(11) . . ? C3A Mo2 C2A 77.8(6) . . ? C3A Mo2 C1A 77.9(6) . . ? C2A Mo2 C1A 109.2(6) . . ? C3A Mo2 C6A 82.7(5) . . ? C2A Mo2 C6A 122.9(6) . . ? C1A Mo2 C6A 118.3(5) . . ? C3A Mo2 C5A 95.4(6) . . ? C2A Mo2 C5A 93.6(6) . . ? C1A Mo2 C5A 154.0(6) . . ? C6A Mo2 C5A 35.7(4) . . ? C3A Mo2 C8A 133.0(5) . . ? C2A Mo2 C8A 147.3(5) . . ? C1A Mo2 C8A 90.8(5) . . ? C6A Mo2 C8A 62.7(5) . . ? C5A Mo2 C8A 75.3(5) . . ? C3A Mo2 C7A 99.8(5) . . ? C2A Mo2 C7A 157.6(6) . . ? C1A Mo2 C7A 91.8(5) . . ? C6A Mo2 C7A 35.5(4) . . ? C5A Mo2 C7A 64.3(5) . . ? C8A Mo2 C7A 34.4(4) . . ? C3A Mo2 C4A 127.8(6) . . ? C2A Mo2 C4A 88.9(5) . . ? C1A Mo2 C4A 152.2(5) . . ? C6A Mo2 C4A 62.9(5) . . ? C5A Mo2 C4A 34.7(4) . . ? C8A Mo2 C4A 64.3(5) . . ? C7A Mo2 C4A 74.9(5) . . ? C3A Mo2 Hg2 131.7(4) . . ? C2A Mo2 Hg2 74.5(4) . . ? C1A Mo2 Hg2 75.0(4) . . ? C6A Mo2 Hg2 145.5(3) . . ? C5A Mo2 Hg2 124.9(3) . . ? C8A Mo2 Hg2 86.7(3) . . ? C7A Mo2 Hg2 120.1(3) . . ? C4A Mo2 Hg2 90.5(3) . . ? O1A C1A Mo2 178.1(14) . . ? O2A C2A Mo2 174.5(14) . . ? O3A C3A Mo2 176.3(14) . . ? C5A C4A B2 121.2(13) . . ? C5A C4A Mo2 71.3(8) . . ? B2 C4A Mo2 83.7(8) . . ? C5A C4A H4A 119.4 . . ? B2 C4A H4A 119.4 . . ? Mo2 C4A H4A 116.1 . . ? C4A C5A C6A 119.1(13) . . ? C4A C5A C15A 122.4(13) . . ? C6A C5A C15A 118.5(13) . . ? C4A C5A Mo2 74.0(8) . . ? C6A C5A Mo2 70.7(8) . . ? C15A C5A Mo2 125.1(10) . . ? C7A C6A C5A 122.7(13) . . ? C7A C6A Mo2 74.2(8) . . ? C5A C6A Mo2 73.6(8) . . ? C7A C6A H6A 118.6 . . ? C5A C6A H6A 118.6 . . ? Mo2 C6A H6A 125.4 . . ? C8A C7A C6A 118.8(12) . . ? C8A C7A C16A 122.3(13) . . ? C6A C7A C16A 118.8(12) . . ? C8A C7A Mo2 72.5(8) . . ? C6A C7A Mo2 70.2(7) . . ? C16A C7A Mo2 125.0(9) . . ? C7A C8A B2 121.2(13) . . ? C7A C8A Mo2 73.1(8) . . ? B2 C8A Mo2 84.1(8) . . ? C7A C8A H8A 119.4 . . ? B2 C8A H8A 119.4 . . ? Mo2 C8A H8A 113.6 . . ? N2 B2 C4A 126.9(12) . . ? N2 B2 C8A 122.0(13) . . ? C4A B2 C8A 110.9(11) . . ? C9A N2 B2 123.2(11) . . ? C9A N2 C10A 113.4(10) . . ? B2 N2 C10A 123.4(11) . . ? N2 C9A C12A 113.5(13) . . ? N2 C9A C11A 114.2(13) . . ? C12A C9A C11A 109.3(12) . . ? N2 C9A H9A 106.4 . . ? C12A C9A H9A 106.4 . . ? C11A C9A H9A 106.4 . . ? N2 C10A C13A 112.4(11) . . ? N2 C10A C14A 111.0(11) . . ? C13A C10A C14A 110.8(12) . . ? N2 C10A H10A 107.5 . . ? C13A C10A H10A 107.5 . . ? C14A C10A H10A 107.5 . . ? C9A C11A H11D 109.5 . . ? C9A C11A H11E 109.5 . . ? H11D C11A H11E 109.5 . . ? C9A C11A H11F 109.5 . . ? H11D C11A H11F 109.5 . . ? H11E C11A H11F 109.5 . . ? C9A C12A H12D 109.5 . . ? C9A C12A H12E 109.5 . . ? H12D C12A H12E 109.5 . . ? C9A C12A H12F 109.5 . . ? H12D C12A H12F 109.5 . . ? H12E C12A H12F 109.5 . . ? C10A C13A H13D 109.5 . . ? C10A C13A H13E 109.5 . . ? H13D C13A H13E 109.5 . . ? C10A C13A H13F 109.5 . . ? H13D C13A H13F 109.5 . . ? H13E C13A H13F 109.5 . . ? C10A C14A H14D 109.5 . . ? C10A C14A H14E 109.5 . . ? H14D C14A H14E 109.5 . . ? C10A C14A H14F 109.5 . . ? H14D C14A H14F 109.5 . . ? H14E C14A H14F 109.5 . . ? C5A C15A H15D 109.5 . . ? C5A C15A H15E 109.5 . . ? H15D C15A H15E 109.5 . . ? C5A C15A H15F 109.5 . . ? H15D C15A H15F 109.5 . . ? H15E C15A H15F 109.5 . . ? C7A C16A H16D 109.5 . . ? C7A C16A H16E 109.5 . . ? H16D C16A H16E 109.5 . . ? C7A C16A H16F 109.5 . . ? H16D C16A H16F 109.5 . . ? H16E C16A H16F 109.5 . . ? _diffrn_measured_fraction_theta_max .997 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full .997 _refine_diff_density_max 1.198 _refine_diff_density_min -1.311 _refine_diff_density_rms .285 # Attachment 'Complex 16.cif' data_welt48 _database_code_depnum_ccdc_archive 'CCDC 297953' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H38 Mo2 N4 O6 Pt' _chemical_formula_sum 'C30 H38 Mo2 N4 O6 Pt' _chemical_formula_weight 937.61 _chemical_absolute_configuration ? 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 8.530(5) _cell_length_b 17.111(5) _cell_length_c 12.321(5) _cell_angle_alpha 90.00 _cell_angle_beta 108.30(5) _cell_angle_gamma 90.00 _cell_volume 1707.3(13) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10879 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.824 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 4.855 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4965 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0897 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 30.04 _reflns_number_total 4964 _reflns_number_gt 3556 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0395P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4964 _refine_ls_number_parameters 196 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0588 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.1098 _refine_ls_wR_factor_gt 0.0778 _refine_ls_goodness_of_fit_ref 0.926 _refine_ls_restrained_S_all 0.926 _refine_ls_shift/su_max 0.000 _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 Pt Pt 0.0000 0.0000 0.0000 0.02957(10) Uani 1 2 d S . . Mo Mo -0.01187(6) -0.07998(2) -0.20700(3) 0.02695(12) Uani 1 1 d . . . O1 O -0.3230(6) -0.1143(3) -0.1321(4) 0.0563(12) Uani 1 1 d . . . O2 O 0.0757(6) 0.0981(2) -0.2000(4) 0.0513(12) Uani 1 1 d . . . O3 O -0.2874(7) -0.0260(3) -0.4250(4) 0.0691(15) Uani 1 1 d . . . N1 N -0.3050(6) 0.0993(3) -0.1318(4) 0.0356(10) Uani 1 1 d . . . N2 N 0.0248(6) -0.1871(3) -0.4371(4) 0.0380(11) Uani 1 1 d . . . C1 C -0.2055(7) -0.0980(3) -0.1549(5) 0.0377(13) Uani 1 1 d . . . C2 C 0.0403(7) 0.0332(3) -0.1958(5) 0.0359(12) Uani 1 1 d . . . C3 C -0.1855(8) -0.0463(4) -0.3443(5) 0.0413(14) Uani 1 1 d . . . C4 C 0.0389(6) -0.2128(3) -0.2348(4) 0.0295(11) Uani 1 1 d . . . H4 H -0.0493 -0.2490 -0.2471 0.035 Uiso 1 1 calc . . . C5 C 0.1464(6) -0.1882(3) -0.1263(4) 0.0304(11) Uani 1 1 d . . . H5 H 0.1457 -0.2068 -0.0538 0.036 Uiso 1 1 calc . . . C6 C 0.2534(7) -0.1315(3) -0.1460(5) 0.0354(12) Uani 1 1 d . . . H6 H 0.3376 -0.1048 -0.0888 0.042 Uiso 1 1 calc . . . C7 C 0.2139(7) -0.1208(3) -0.2667(5) 0.0356(12) Uani 1 1 d . . . H7 H 0.2645 -0.0845 -0.3036 0.043 Uiso 1 1 calc . . . C8 C 0.0863(7) -0.1737(3) -0.3212(4) 0.0306(11) Uani 1 1 d . . . C9 C 0.0514(10) -0.1245(4) -0.5096(5) 0.0539(18) Uani 1 1 d . . . H9A H -0.0170 -0.0793 -0.5050 0.081 Uiso 1 1 calc . . . H9B H 0.0210 -0.1427 -0.5889 0.081 Uiso 1 1 calc . . . H9C H 0.1680 -0.1092 -0.4837 0.081 Uiso 1 1 calc . . . C10 C -0.1327(9) -0.2253(4) -0.4767(5) 0.0491(16) Uani 1 1 d . . . H10A H -0.1266 -0.2755 -0.4372 0.074 Uiso 1 1 calc . . . H10B H -0.1623 -0.2343 -0.5592 0.074 Uiso 1 1 calc . . . H10C H -0.2166 -0.1923 -0.4607 0.074 Uiso 1 1 calc . . . C11 C -0.1911(7) 0.0650(3) -0.0781(4) 0.0340(12) Uani 1 1 d . . . C12 C -0.4509(7) 0.1334(3) -0.2128(5) 0.0404(13) Uani 1 1 d . . . C13 C -0.5132(11) 0.1970(6) -0.1532(7) 0.091(3) Uani 1 1 d . . . H13A H -0.5479 0.1743 -0.0914 0.137 Uiso 1 1 calc . . . H13B H -0.6074 0.2231 -0.2080 0.137 Uiso 1 1 calc . . . H13C H -0.4249 0.2351 -0.1213 0.137 Uiso 1 1 calc . . . C14 C -0.5732(9) 0.0674(5) -0.2553(8) 0.075(2) Uani 1 1 d . . . H14A H -0.5244 0.0274 -0.2919 0.113 Uiso 1 1 calc . . . H14B H -0.6740 0.0878 -0.3108 0.113 Uiso 1 1 calc . . . H14C H -0.6002 0.0441 -0.1907 0.113 Uiso 1 1 calc . . . C15 C -0.4009(9) 0.1637(5) -0.3119(6) 0.069(2) Uani 1 1 d . . . H15A H -0.3305 0.2098 -0.2878 0.104 Uiso 1 1 calc . . . H15B H -0.4998 0.1779 -0.3748 0.104 Uiso 1 1 calc . . . H15C H -0.3399 0.1230 -0.3377 0.104 Uiso 1 1 calc . . . 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 Pt 0.03395(17) 0.03119(16) 0.02331(14) -0.00202(11) 0.00860(11) 0.00855(12) Mo 0.0358(2) 0.0219(2) 0.0245(2) -0.00121(17) 0.01145(17) 0.00141(18) O1 0.042(3) 0.049(3) 0.084(4) 0.002(2) 0.030(3) -0.006(2) O2 0.088(4) 0.025(2) 0.051(3) -0.0021(18) 0.036(2) 0.001(2) O3 0.075(4) 0.072(3) 0.042(3) 0.000(3) -0.007(3) 0.023(3) N1 0.036(3) 0.036(3) 0.034(2) 0.000(2) 0.009(2) 0.005(2) N2 0.061(3) 0.027(2) 0.030(2) -0.0038(19) 0.020(2) -0.001(2) C1 0.041(3) 0.025(3) 0.047(3) 0.000(2) 0.013(3) 0.000(2) C2 0.049(3) 0.027(3) 0.038(3) -0.001(2) 0.022(3) 0.003(2) C3 0.053(4) 0.039(3) 0.029(3) -0.002(2) 0.009(3) 0.008(3) C4 0.036(3) 0.023(2) 0.033(3) -0.001(2) 0.016(2) 0.000(2) C5 0.035(3) 0.027(2) 0.030(3) -0.002(2) 0.011(2) 0.003(2) C6 0.030(3) 0.034(3) 0.042(3) -0.009(2) 0.011(2) 0.002(2) C7 0.046(3) 0.028(3) 0.041(3) -0.004(2) 0.026(3) -0.002(2) C8 0.043(3) 0.023(2) 0.030(2) -0.005(2) 0.016(2) 0.003(2) C9 0.094(5) 0.042(4) 0.035(3) 0.001(3) 0.032(3) -0.001(4) C10 0.064(4) 0.048(4) 0.031(3) -0.009(3) 0.009(3) 0.002(3) C11 0.040(3) 0.033(3) 0.030(3) -0.004(2) 0.014(2) 0.006(2) C12 0.030(3) 0.041(3) 0.045(3) 0.009(3) 0.004(2) 0.005(2) C13 0.085(6) 0.096(7) 0.076(6) -0.002(5) 0.001(5) 0.065(5) C14 0.041(4) 0.070(5) 0.101(6) 0.021(5) 0.003(4) -0.014(4) C15 0.053(4) 0.077(5) 0.071(5) 0.035(4) 0.010(4) 0.000(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 Pt C11 1.958(6) . ? Pt C11 1.958(6) 3 ? Pt Mo 2.8680(10) . ? Pt Mo 2.8681(10) 3 ? Mo C3 1.953(6) . ? Mo C1 1.976(6) . ? Mo C2 1.983(6) . ? Mo C6 2.322(6) . ? Mo C5 2.323(5) . ? Mo C4 2.358(5) . ? Mo C7 2.372(5) . ? Mo C8 2.448(5) . ? O1 C1 1.156(7) . ? O2 C2 1.156(7) . ? O3 C3 1.150(7) . ? N1 C11 1.150(7) . ? N1 C12 1.451(7) . ? N2 C8 1.376(6) . ? N2 C10 1.435(8) . ? N2 C9 1.458(8) . ? C4 C8 1.419(7) . ? C4 C5 1.427(7) . ? C4 H4 0.9500 . ? C5 C6 1.404(7) . ? C5 H5 0.9500 . ? C6 C7 1.430(8) . ? C6 H6 0.9500 . ? C7 C8 1.414(8) . ? C7 H7 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C12 C13 1.500(10) . ? C12 C15 1.506(9) . ? C12 C14 1.516(9) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Pt C11 180.0 . 3 ? C11 Pt Mo 92.44(15) . . ? C11 Pt Mo 87.56(15) 3 . ? C11 Pt Mo 87.56(15) . 3 ? C11 Pt Mo 92.44(15) 3 3 ? Mo Pt Mo 180.0 . 3 ? C3 Mo C1 81.0(3) . . ? C3 Mo C2 82.2(3) . . ? C1 Mo C2 108.8(2) . . ? C3 Mo C6 142.1(2) . . ? C1 Mo C6 131.6(2) . . ? C2 Mo C6 100.0(2) . . ? C3 Mo C5 141.9(2) . . ? C1 Mo C5 99.7(2) . . ? C2 Mo C5 131.4(2) . . ? C6 Mo C5 35.18(18) . . ? C3 Mo C4 106.4(2) . . ? C1 Mo C4 96.1(2) . . ? C2 Mo C4 154.7(2) . . ? C6 Mo C4 58.44(19) . . ? C5 Mo C4 35.48(17) . . ? C3 Mo C7 106.7(2) . . ? C1 Mo C7 153.9(2) . . ? C2 Mo C7 97.1(2) . . ? C6 Mo C7 35.45(19) . . ? C5 Mo C7 58.59(19) . . ? C4 Mo C7 57.83(18) . . ? C3 Mo C8 89.9(2) . . ? C1 Mo C8 123.8(2) . . ? C2 Mo C8 124.8(2) . . ? C6 Mo C8 57.54(18) . . ? C5 Mo C8 57.74(17) . . ? C4 Mo C8 34.28(16) . . ? C7 Mo C8 34.07(18) . . ? C3 Mo Pt 115.77(17) . . ? C1 Mo Pt 65.48(17) . . ? C2 Mo Pt 61.80(15) . . ? C6 Mo Pt 97.73(14) . . ? C5 Mo Pt 98.41(13) . . ? C4 Mo Pt 129.21(12) . . ? C7 Mo Pt 127.63(15) . . ? C8 Mo Pt 154.27(13) . . ? C11 N1 C12 171.2(5) . . ? C8 N2 C10 116.1(5) . . ? C8 N2 C9 115.6(5) . . ? C10 N2 C9 115.8(5) . . ? O1 C1 Mo 173.4(5) . . ? O2 C2 Mo 172.4(5) . . ? O3 C3 Mo 179.7(6) . . ? C8 C4 C5 108.3(5) . . ? C8 C4 Mo 76.4(3) . . ? C5 C4 Mo 70.9(3) . . ? C8 C4 H4 125.9 . . ? C5 C4 H4 125.9 . . ? Mo C4 H4 118.7 . . ? C6 C5 C4 107.7(5) . . ? C6 C5 Mo 72.4(3) . . ? C4 C5 Mo 73.6(3) . . ? C6 C5 H5 126.2 . . ? C4 C5 H5 126.2 . . ? Mo C5 H5 119.7 . . ? C5 C6 C7 108.4(5) . . ? C5 C6 Mo 72.4(3) . . ? C7 C6 Mo 74.2(3) . . ? C5 C6 H6 125.8 . . ? C7 C6 H6 125.8 . . ? Mo C6 H6 119.4 . . ? C8 C7 C6 107.9(5) . . ? C8 C7 Mo 75.9(3) . . ? C6 C7 Mo 70.4(3) . . ? C8 C7 H7 126.1 . . ? C6 C7 H7 126.1 . . ? Mo C7 H7 119.5 . . ? N2 C8 C7 125.8(5) . . ? N2 C8 C4 126.5(5) . . ? C7 C8 C4 107.7(4) . . ? N2 C8 Mo 128.1(4) . . ? C7 C8 Mo 70.0(3) . . ? C4 C8 Mo 69.4(3) . . ? N2 C9 H9A 109.5 . . ? N2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C10 H10A 109.5 . . ? N2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 Pt 174.3(5) . . ? N1 C12 C13 108.3(5) . . ? N1 C12 C15 107.2(5) . . ? C13 C12 C15 112.4(6) . . ? N1 C12 C14 106.6(5) . . ? C13 C12 C14 113.5(6) . . ? C15 C12 C14 108.4(6) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.130 _refine_diff_density_min -1.650 _refine_diff_density_rms 0.319 # Attachment 'Complex 17.cif' data_croizat _database_code_depnum_ccdc_archive 'CCDC 297954' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H30 Mo2 N4 O6 Pt, 2(O C4 H8)' _chemical_formula_sum 'C42 H46 Mo2 N4 O8 Pt' _chemical_formula_weight 1121.80 _chemical_absolute_configuration . 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.518(5) _cell_length_b 11.117(5) _cell_length_c 12.785(5) _cell_angle_alpha 94.91(5) _cell_angle_beta 109.36(5) _cell_angle_gamma 107.20(5) _cell_volume 1068.3(9) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 22809 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.744 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 3.899 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6095 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1680 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 30.04 _reflns_number_total 6094 _reflns_number_gt 3564 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0367P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6094 _refine_ls_number_parameters 259 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1475 _refine_ls_R_factor_gt 0.0744 _refine_ls_wR_factor_ref 0.1687 _refine_ls_wR_factor_gt 0.1426 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_restrained_S_all 0.980 _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 Pt Pt 0.0000 0.0000 0.5000 0.04091(19) Uani 1 2 d S . . Mo Mo -0.32287(10) -0.09476(6) 0.30588(6) 0.0420(2) Uani 1 1 d . . . O1 O -0.3692(10) -0.1021(7) 0.5390(6) 0.0632(19) Uani 1 1 d . . . O2 O 0.0084(10) -0.1385(7) 0.2792(6) 0.0596(18) Uani 1 1 d . . . O3 O -0.4465(13) -0.3926(7) 0.2675(7) 0.088(3) Uani 1 1 d . . . O4 O 0.0774(15) 0.2528(9) 0.1892(9) 0.106(3) Uani 1 1 d . . . N1 N 0.0236(11) 0.1697(7) 0.4655(6) 0.0478(19) Uani 1 1 d . . . N2 N -0.6995(13) -0.2065(9) 0.0658(8) 0.063(2) Uani 1 1 d . . . C1 C -0.3392(13) -0.0988(9) 0.4567(9) 0.050(2) Uani 1 1 d . . . C2 C -0.1047(14) -0.1161(8) 0.2990(8) 0.046(2) Uani 1 1 d . . . C3 C -0.3980(15) -0.2796(10) 0.2851(9) 0.060(3) Uani 1 1 d . . . C4 C -0.5724(14) -0.0339(10) 0.2344(9) 0.058(3) Uani 1 1 d . . . H4 H -0.6623 -0.0597 0.2646 0.070 Uiso 1 1 calc . . . C5 C -0.4164(15) 0.0796(10) 0.2804(9) 0.055(2) Uani 1 1 d . . . H5 H -0.3874 0.1445 0.3439 0.066 Uiso 1 1 calc . . . C6 C -0.3161(13) 0.0765(9) 0.2146(9) 0.053(2) Uani 1 1 d . . . H6 H -0.2058 0.1399 0.2256 0.064 Uiso 1 1 calc . . . C7 C -0.4042(13) -0.0358(9) 0.1286(7) 0.048(2) Uani 1 1 d . . . H7 H -0.3609 -0.0635 0.0748 0.057 Uiso 1 1 calc . . . C8 C -0.5687(14) -0.0999(9) 0.1371(8) 0.051(2) Uani 1 1 d . . . C9 C -0.8306(16) -0.2863(12) 0.1045(10) 0.077(3) Uani 1 1 d . . . H9A H -0.7930 -0.3566 0.1324 0.115 Uiso 1 1 calc . . . H9B H -0.9457 -0.3220 0.0413 0.115 Uiso 1 1 calc . . . H9C H -0.8411 -0.2337 0.1657 0.115 Uiso 1 1 calc . . . C10 C -0.6500(16) -0.2843(10) -0.0080(8) 0.066(3) Uani 1 1 d . . . H10A H -0.6287 -0.2387 -0.0670 0.099 Uiso 1 1 calc . . . H10B H -0.7463 -0.3671 -0.0433 0.099 Uiso 1 1 calc . . . H10C H -0.5419 -0.2991 0.0371 0.099 Uiso 1 1 calc . . . C11 C 0.0514(13) 0.2723(8) 0.4484(8) 0.046(2) Uani 1 1 d . . . C12 C 0.0953(14) 0.4025(8) 0.4289(8) 0.050(2) Uani 1 1 d . . . C13 C -0.0250(14) 0.4404(9) 0.3499(9) 0.057(2) Uani 1 1 d . . . H13 H -0.1398 0.3807 0.3052 0.068 Uiso 1 1 calc . . . C14 C 0.0235(17) 0.5671(9) 0.3361(9) 0.063(3) Uani 1 1 d . . . H14 H -0.0598 0.5946 0.2830 0.075 Uiso 1 1 calc . . . C15 C 0.1882(17) 0.6516(9) 0.3975(10) 0.064(3) Uani 1 1 d . . . H15 H 0.2199 0.7380 0.3876 0.077 Uiso 1 1 calc . . . C16 C 0.3093(16) 0.6124(9) 0.4741(10) 0.065(3) Uani 1 1 d . . . H16 H 0.4253 0.6717 0.5161 0.078 Uiso 1 1 calc . . . C17 C 0.2641(15) 0.4876(9) 0.4908(9) 0.059(3) Uani 1 1 d . . . H17 H 0.3481 0.4608 0.5441 0.071 Uiso 1 1 calc . . . C18 C 0.244(2) 0.3406(18) 0.2168(17) 0.143(8) Uani 1 1 d . . . H18A H 0.3189 0.3416 0.2951 0.171 Uiso 1 1 calc . . . H18B H 0.2363 0.4275 0.2140 0.171 Uiso 1 1 calc . . . C19 C 0.323(2) 0.3110(14) 0.1424(16) 0.124(7) Uani 1 1 d . . . H19A H 0.4456 0.3158 0.1848 0.149 Uiso 1 1 calc . . . H19B H 0.3247 0.3714 0.0898 0.149 Uiso 1 1 calc . . . C20 C 0.208(2) 0.1749(11) 0.0779(12) 0.083(4) Uani 1 1 d . . . H20A H 0.1496 0.1726 -0.0037 0.099 Uiso 1 1 calc . . . H20B H 0.2785 0.1172 0.0869 0.099 Uiso 1 1 calc . . . C21 C 0.077(2) 0.1392(11) 0.1320(14) 0.094(5) Uani 1 1 d . . . H21A H -0.0421 0.0912 0.0740 0.112 Uiso 1 1 calc . . . H21B H 0.1091 0.0836 0.1860 0.112 Uiso 1 1 calc . . . 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 Pt 0.0456(3) 0.0275(2) 0.0467(3) 0.0135(2) 0.0135(2) 0.0111(2) Mo 0.0461(5) 0.0372(4) 0.0438(5) 0.0124(4) 0.0172(4) 0.0144(4) O1 0.063(5) 0.068(4) 0.055(4) 0.011(3) 0.031(4) 0.007(4) O2 0.063(5) 0.060(4) 0.061(4) 0.011(3) 0.028(4) 0.024(4) O3 0.105(7) 0.037(4) 0.093(6) 0.016(4) 0.018(5) 0.008(4) O4 0.107(8) 0.073(6) 0.129(9) -0.007(6) 0.066(7) 0.003(5) N1 0.064(5) 0.034(4) 0.047(5) 0.008(3) 0.020(4) 0.020(4) N2 0.071(6) 0.070(6) 0.054(6) 0.017(4) 0.028(5) 0.026(5) C1 0.047(6) 0.049(5) 0.053(6) 0.005(4) 0.020(5) 0.016(4) C2 0.061(6) 0.041(4) 0.045(5) 0.018(4) 0.020(5) 0.026(4) C3 0.062(7) 0.047(5) 0.062(7) 0.012(5) 0.016(5) 0.014(5) C4 0.056(6) 0.069(6) 0.056(6) 0.015(5) 0.015(5) 0.036(5) C5 0.063(7) 0.053(5) 0.058(6) 0.016(5) 0.026(5) 0.028(5) C6 0.046(6) 0.051(5) 0.064(6) 0.025(5) 0.021(5) 0.016(4) C7 0.051(6) 0.053(5) 0.040(5) 0.013(4) 0.017(4) 0.019(4) C8 0.063(7) 0.044(5) 0.048(6) 0.010(4) 0.017(5) 0.024(5) C9 0.055(7) 0.081(8) 0.072(8) 0.008(6) 0.018(6) 0.001(6) C10 0.070(7) 0.064(6) 0.042(6) 0.001(5) 0.010(5) 0.011(6) C11 0.051(5) 0.035(4) 0.048(5) 0.010(4) 0.016(4) 0.014(4) C12 0.074(7) 0.032(4) 0.055(6) 0.011(4) 0.033(5) 0.023(4) C13 0.062(7) 0.053(5) 0.061(6) 0.015(5) 0.025(5) 0.025(5) C14 0.092(9) 0.042(5) 0.072(7) 0.023(5) 0.038(7) 0.037(6) C15 0.092(9) 0.037(5) 0.087(8) 0.026(5) 0.054(7) 0.025(6) C16 0.078(8) 0.034(5) 0.084(8) 0.010(5) 0.044(7) 0.006(5) C17 0.060(7) 0.043(5) 0.066(7) 0.011(5) 0.018(5) 0.012(5) C18 0.112(14) 0.119(13) 0.145(16) -0.066(12) 0.072(13) -0.035(11) C19 0.120(14) 0.084(10) 0.163(16) -0.034(10) 0.102(13) -0.014(9) C20 0.112(11) 0.064(7) 0.094(10) 0.012(6) 0.055(9) 0.042(7) C21 0.094(10) 0.048(6) 0.143(13) -0.001(7) 0.066(10) 0.011(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt N1 1.942(7) . ? Pt N1 1.942(7) 2_556 ? Pt C2 2.509(9) 2_556 ? Pt C2 2.509(9) . ? Pt C1 2.611(10) . ? Pt C1 2.611(10) 2_556 ? Pt Mo 2.854(3) . ? Pt Mo 2.854(3) 2_556 ? Mo C3 1.928(10) . ? Mo C2 1.970(11) . ? Mo C1 1.982(11) . ? Mo C5 2.312(9) . ? Mo C6 2.314(9) . ? Mo C4 2.341(10) . ? Mo C7 2.351(9) . ? Mo C8 2.440(10) . ? O1 C1 1.164(11) . ? O2 C2 1.161(11) . ? O3 C3 1.177(12) . ? O4 C18 1.372(18) . ? O4 C21 1.404(14) . ? N1 C11 1.150(10) . ? N2 C8 1.356(13) . ? N2 C9 1.460(15) . ? N2 C10 1.468(14) . ? C4 C8 1.403(14) . ? C4 C5 1.437(15) . ? C4 H4 0.9500 . ? C5 C6 1.389(14) . ? C5 H5 0.9500 . ? C6 C7 1.412(13) . ? C6 H6 0.9500 . ? C7 C8 1.416(14) . ? C7 H7 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.449(11) . ? C12 C13 1.375(14) . ? C12 C17 1.379(14) . ? C13 C14 1.390(13) . ? C13 H13 0.9500 . ? C14 C15 1.353(16) . ? C14 H14 0.9500 . ? C15 C16 1.372(16) . ? C15 H15 0.9500 . ? C16 C17 1.381(13) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.40(2) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.516(18) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.474(18) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pt N1 179.999(1) . 2_556 ? N1 Pt C2 84.1(3) . 2_556 ? N1 Pt C2 95.9(3) 2_556 2_556 ? N1 Pt C2 95.9(3) . . ? N1 Pt C2 84.1(3) 2_556 . ? C2 Pt C2 179.998(1) 2_556 . ? N1 Pt C1 102.2(3) . . ? N1 Pt C1 77.8(3) 2_556 . ? C2 Pt C1 99.7(3) 2_556 . ? C2 Pt C1 80.3(3) . . ? N1 Pt C1 77.8(3) . 2_556 ? N1 Pt C1 102.2(3) 2_556 2_556 ? C2 Pt C1 80.3(3) 2_556 2_556 ? C2 Pt C1 99.7(3) . 2_556 ? C1 Pt C1 180.0(4) . 2_556 ? N1 Pt Mo 87.1(2) . . ? N1 Pt Mo 92.9(2) 2_556 . ? C2 Pt Mo 137.5(2) 2_556 . ? C2 Pt Mo 42.5(2) . . ? C1 Pt Mo 42.2(2) . . ? C1 Pt Mo 137.8(2) 2_556 . ? N1 Pt Mo 92.9(2) . 2_556 ? N1 Pt Mo 87.1(2) 2_556 2_556 ? C2 Pt Mo 42.5(2) 2_556 2_556 ? C2 Pt Mo 137.5(2) . 2_556 ? C1 Pt Mo 137.8(2) . 2_556 ? C1 Pt Mo 42.2(2) 2_556 2_556 ? Mo Pt Mo 180.00(3) . 2_556 ? C3 Mo C2 82.0(4) . . ? C3 Mo C1 85.3(4) . . ? C2 Mo C1 113.4(4) . . ? C3 Mo C5 145.1(4) . . ? C2 Mo C5 128.7(4) . . ? C1 Mo C5 94.5(4) . . ? C3 Mo C6 144.9(4) . . ? C2 Mo C6 97.2(4) . . ? C1 Mo C6 125.7(4) . . ? C5 Mo C6 34.9(4) . . ? C3 Mo C4 109.1(4) . . ? C2 Mo C4 151.8(4) . . ? C1 Mo C4 93.7(4) . . ? C5 Mo C4 36.0(4) . . ? C6 Mo C4 58.5(4) . . ? C3 Mo C7 109.6(4) . . ? C2 Mo C7 93.9(4) . . ? C1 Mo C7 150.7(4) . . ? C5 Mo C7 58.6(3) . . ? C6 Mo C7 35.2(3) . . ? C4 Mo C7 58.0(4) . . ? C3 Mo C8 93.3(4) . . ? C2 Mo C8 122.5(4) . . ? C1 Mo C8 123.3(4) . . ? C5 Mo C8 57.8(3) . . ? C6 Mo C8 57.3(3) . . ? C4 Mo C8 34.1(3) . . ? C7 Mo C8 34.3(3) . . ? C3 Mo Pt 105.7(3) . . ? C2 Mo Pt 59.4(3) . . ? C1 Mo Pt 62.3(3) . . ? C5 Mo Pt 105.1(3) . . ? C6 Mo Pt 103.9(3) . . ? C4 Mo Pt 135.5(3) . . ? C7 Mo Pt 131.6(2) . . ? C8 Mo Pt 160.8(2) . . ? C18 O4 C21 105.6(12) . . ? C11 N1 Pt 174.7(8) . . ? C8 N2 C9 119.9(9) . . ? C8 N2 C10 116.7(9) . . ? C9 N2 C10 111.9(9) . . ? O1 C1 Mo 172.0(9) . . ? O1 C1 Pt 112.0(7) . . ? Mo C1 Pt 75.5(3) . . ? O2 C2 Mo 170.1(8) . . ? O2 C2 Pt 111.7(7) . . ? Mo C2 Pt 78.2(3) . . ? O3 C3 Mo 177.2(10) . . ? C8 C4 C5 108.1(10) . . ? C8 C4 Mo 76.9(6) . . ? C5 C4 Mo 70.9(6) . . ? C8 C4 H4 126.0 . . ? C5 C4 H4 126.0 . . ? Mo C4 H4 118.1 . . ? C6 C5 C4 107.2(9) . . ? C6 C5 Mo 72.6(6) . . ? C4 C5 Mo 73.1(5) . . ? C6 C5 H5 126.4 . . ? C4 C5 H5 126.4 . . ? Mo C5 H5 119.8 . . ? C5 C6 C7 109.1(9) . . ? C5 C6 Mo 72.5(6) . . ? C7 C6 Mo 73.8(5) . . ? C5 C6 H6 125.4 . . ? C7 C6 H6 125.4 . . ? Mo C6 H6 120.0 . . ? C6 C7 C8 107.7(8) . . ? C6 C7 Mo 70.9(5) . . ? C8 C7 Mo 76.3(5) . . ? C6 C7 H7 126.2 . . ? C8 C7 H7 126.2 . . ? Mo C7 H7 118.5 . . ? N2 C8 C4 125.5(10) . . ? N2 C8 C7 126.9(9) . . ? C4 C8 C7 107.6(9) . . ? N2 C8 Mo 126.4(6) . . ? C4 C8 Mo 69.1(6) . . ? C7 C8 Mo 69.4(5) . . ? N2 C9 H9A 109.5 . . ? N2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C10 H10A 109.5 . . ? N2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C12 177.3(11) . . ? C13 C12 C17 120.6(9) . . ? C13 C12 C11 121.6(10) . . ? C17 C12 C11 117.8(9) . . ? C12 C13 C14 119.1(10) . . ? C12 C13 H13 120.5 . . ? C14 C13 H13 120.5 . . ? C15 C14 C13 120.7(10) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 120.0(9) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C17 120.7(11) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C12 C17 C16 119.0(10) . . ? C12 C17 H17 120.5 . . ? C16 C17 H17 120.5 . . ? O4 C18 C19 111.2(12) . . ? O4 C18 H18A 109.4 . . ? C19 C18 H18A 109.4 . . ? O4 C18 H18B 109.4 . . ? C19 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? C18 C19 C20 105.4(12) . . ? C18 C19 H19A 110.7 . . ? C20 C19 H19A 110.7 . . ? C18 C19 H19B 110.7 . . ? C20 C19 H19B 110.7 . . ? H19A C19 H19B 108.8 . . ? C21 C20 C19 102.6(10) . . ? C21 C20 H20A 111.3 . . ? C19 C20 H20A 111.3 . . ? C21 C20 H20B 111.3 . . ? C19 C20 H20B 111.3 . . ? H20A C20 H20B 109.2 . . ? O4 C21 C20 108.0(10) . . ? O4 C21 H21A 110.1 . . ? C20 C21 H21A 110.1 . . ? O4 C21 H21B 110.1 . . ? C20 C21 H21B 110.1 . . ? H21A C21 H21B 108.4 . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 2.060 _refine_diff_density_min -1.443 _refine_diff_density_rms 0.173 data_shelxl _database_code_depnum_ccdc_archive 'CCDC 297955' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H10 Cl Mo N O3' _chemical_formula_sum 'C10 H10 Cl Mo N O3' _chemical_formula_weight 323.58 _chemical_absolute_configuration . loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.8250(3) _cell_length_b 10.7520(3) _cell_length_c 12.8080(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.38(5) _cell_angle_gamma 90.00 _cell_volume 1199.07(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2720 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.792 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 640 _exptl_absorpt_coefficient_mu 1.306 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5481 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0649 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 30.04 _reflns_number_total 3489 _reflns_number_gt 2511 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3489 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0666 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.0865 _refine_ls_wR_factor_gt 0.0765 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _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 Mo Mo 0.79176(3) 0.22875(2) 0.124530(18) 0.02364(9) Uani 1 1 d . . . Cl Cl 0.99516(10) 0.14706(7) 0.26915(6) 0.0388(2) Uani 1 1 d . . . O1 O 0.6017(3) 0.2353(2) 0.3110(2) 0.0527(7) Uani 1 1 d . . . O3 O 0.4635(3) 0.1636(2) 0.00570(19) 0.0546(7) Uani 1 1 d . . . O2 O 0.8504(3) -0.04156(19) 0.04144(17) 0.0471(6) Uani 1 1 d . . . N N 1.1374(3) 0.4028(2) 0.18372(19) 0.0330(6) Uani 1 1 d . . . C1 C 0.6717(4) 0.2265(2) 0.2437(3) 0.0332(7) Uani 1 1 d . . . C3 C 0.5834(4) 0.1894(3) 0.0472(2) 0.0342(7) Uani 1 1 d . . . C2 C 0.8257(4) 0.0538(3) 0.0734(2) 0.0313(7) Uani 1 1 d . . . C4 C 0.8563(4) 0.4370(3) 0.1529(2) 0.0338(7) Uani 1 1 d . . . H4 H 0.8420 0.4704 0.2192 0.041 Uiso 1 1 calc . . . C5 C 0.7416(4) 0.4231(3) 0.0635(3) 0.0425(8) Uani 1 1 d . . . H5 H 0.6393 0.4533 0.0566 0.051 Uiso 1 1 calc . . . C6 C 0.8051(4) 0.3567(3) -0.0141(2) 0.0394(8) Uani 1 1 d . . . H6 H 0.7526 0.3341 -0.0822 0.047 Uiso 1 1 calc . . . C7 C 0.9598(4) 0.3295(3) 0.0268(2) 0.0310(7) Uani 1 1 d . . . H7 H 1.0266 0.2787 -0.0060 0.037 Uiso 1 1 calc . . . C8 C 0.9984(3) 0.3921(2) 0.1267(2) 0.0251(6) Uani 1 1 d . . . C9 C 1.1574(5) 0.4571(3) 0.2898(3) 0.0539(10) Uani 1 1 d . . . H9A H 1.1239 0.5442 0.2849 0.081 Uiso 1 1 calc . . . H9B H 1.2659 0.4530 0.3219 0.081 Uiso 1 1 calc . . . H9C H 1.0956 0.4107 0.3335 0.081 Uiso 1 1 calc . . . C10 C 1.2677(4) 0.3404(3) 0.1512(3) 0.0505(9) Uani 1 1 d . . . H10A H 1.2588 0.2505 0.1614 0.076 Uiso 1 1 calc . . . H10B H 1.3628 0.3707 0.1938 0.076 Uiso 1 1 calc . . . H10C H 1.2694 0.3578 0.0763 0.076 Uiso 1 1 calc . . . 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 Mo 0.02625(15) 0.02258(14) 0.02232(15) 0.00139(9) 0.00466(11) -0.00063(10) Cl 0.0425(5) 0.0361(4) 0.0335(4) 0.0087(3) -0.0064(4) -0.0001(3) O1 0.069(2) 0.0481(13) 0.0499(16) 0.0001(11) 0.0358(15) 0.0000(13) O3 0.0320(15) 0.0695(17) 0.0593(16) -0.0057(13) -0.0016(12) -0.0098(13) O2 0.0546(17) 0.0300(11) 0.0590(15) -0.0101(11) 0.0165(12) -0.0013(12) N 0.0296(15) 0.0357(13) 0.0326(14) 0.0001(11) 0.0015(12) -0.0073(12) C1 0.042(2) 0.0260(14) 0.0332(18) 0.0019(13) 0.0111(15) -0.0044(14) C3 0.0311(18) 0.0382(16) 0.0342(17) 0.0010(14) 0.0081(14) -0.0022(15) C2 0.0306(18) 0.0332(16) 0.0303(16) 0.0000(13) 0.0056(13) -0.0044(14) C4 0.040(2) 0.0251(14) 0.0385(18) -0.0022(13) 0.0139(15) 0.0006(14) C5 0.0258(18) 0.0310(16) 0.069(2) 0.0179(16) 0.0033(17) 0.0038(14) C6 0.044(2) 0.0414(17) 0.0289(17) 0.0160(14) -0.0066(15) -0.0114(16) C7 0.0380(19) 0.0313(15) 0.0256(15) -0.0009(12) 0.0112(14) -0.0086(14) C8 0.0304(16) 0.0190(12) 0.0270(15) 0.0050(11) 0.0078(13) -0.0030(12) C9 0.069(3) 0.051(2) 0.0359(19) -0.0031(16) -0.0067(18) -0.023(2) C10 0.034(2) 0.044(2) 0.073(3) 0.0087(18) 0.0075(19) 0.0031(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 Mo C3 1.987(3) . ? Mo C1 1.995(3) . ? Mo C2 2.030(3) . ? Mo C5 2.250(3) . ? Mo C6 2.264(3) . ? Mo C4 2.324(3) . ? Mo C7 2.354(3) . ? Mo Cl 2.5182(14) . ? Mo C8 2.529(3) . ? O1 C1 1.142(4) . ? O3 C3 1.138(4) . ? O2 C2 1.138(3) . ? N C8 1.327(4) . ? N C10 1.449(4) . ? N C9 1.463(4) . ? C4 C5 1.406(5) . ? C4 C8 1.434(4) . ? C4 H4 0.9500 . ? C5 C6 1.412(5) . ? C5 H5 0.9500 . ? C6 C7 1.411(4) . ? C6 H6 0.9500 . ? C7 C8 1.437(4) . ? C7 H7 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Mo C1 79.34(13) . . ? C3 Mo C2 79.35(13) . . ? C1 Mo C2 111.11(11) . . ? C3 Mo C5 84.89(13) . . ? C1 Mo C5 100.25(12) . . ? C2 Mo C5 141.25(13) . . ? C3 Mo C6 84.30(12) . . ? C1 Mo C6 135.17(13) . . ? C2 Mo C6 106.32(12) . . ? C5 Mo C6 36.45(12) . . ? C3 Mo C4 117.78(12) . . ? C1 Mo C4 92.25(11) . . ? C2 Mo C4 153.88(12) . . ? C5 Mo C4 35.76(12) . . ? C6 Mo C4 59.62(11) . . ? C3 Mo C7 116.41(12) . . ? C1 Mo C7 150.62(10) . . ? C2 Mo C7 96.66(11) . . ? C5 Mo C7 59.56(12) . . ? C6 Mo C7 35.51(11) . . ? C4 Mo C7 58.70(10) . . ? C3 Mo Cl 141.57(10) . . ? C1 Mo Cl 80.60(10) . . ? C2 Mo Cl 77.83(9) . . ? C5 Mo Cl 130.97(9) . . ? C6 Mo Cl 131.82(9) . . ? C4 Mo Cl 95.40(8) . . ? C7 Mo Cl 96.68(8) . . ? C3 Mo C8 139.50(11) . . ? C1 Mo C8 118.16(11) . . ? C2 Mo C8 120.21(11) . . ? C5 Mo C8 57.26(10) . . ? C6 Mo C8 57.11(10) . . ? C4 Mo C8 34.03(9) . . ? C7 Mo C8 33.99(9) . . ? Cl Mo C8 78.93(7) . . ? C8 N C10 120.5(3) . . ? C8 N C9 120.4(3) . . ? C10 N C9 118.1(3) . . ? O1 C1 Mo 174.5(2) . . ? O3 C3 Mo 177.4(3) . . ? O2 C2 Mo 176.1(3) . . ? C5 C4 C8 108.4(3) . . ? C5 C4 Mo 69.23(16) . . ? C8 C4 Mo 80.84(16) . . ? C5 C4 H4 125.8 . . ? C8 C4 H4 125.8 . . ? Mo C4 H4 116.0 . . ? C4 C5 C6 108.1(3) . . ? C4 C5 Mo 75.00(17) . . ? C6 C5 Mo 72.31(17) . . ? C4 C5 H5 125.9 . . ? C6 C5 H5 125.9 . . ? Mo C5 H5 118.6 . . ? C7 C6 C5 108.3(3) . . ? C7 C6 Mo 75.75(17) . . ? C5 C6 Mo 71.24(16) . . ? C7 C6 H6 125.8 . . ? C5 C6 H6 125.8 . . ? Mo C6 H6 119.0 . . ? C6 C7 C8 107.9(3) . . ? C6 C7 Mo 68.74(17) . . ? C8 C7 Mo 79.68(16) . . ? C6 C7 H7 126.0 . . ? C8 C7 H7 126.0 . . ? Mo C7 H7 117.4 . . ? N C8 C4 127.4(3) . . ? N C8 C7 126.5(3) . . ? C4 C8 C7 106.0(3) . . ? N C8 Mo 131.81(19) . . ? C4 C8 Mo 65.13(15) . . ? C7 C8 Mo 66.34(15) . . ? N C9 H9A 109.5 . . ? N C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N C10 H10A 109.5 . . ? N C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 Mo C1 O1 -94(3) . . . . ? C2 Mo C1 O1 -169(3) . . . . ? C5 Mo C1 O1 -12(3) . . . . ? C6 Mo C1 O1 -24(3) . . . . ? C4 Mo C1 O1 23(3) . . . . ? C7 Mo C1 O1 32(3) . . . . ? Cl Mo C1 O1 118(3) . . . . ? C8 Mo C1 O1 47(3) . . . . ? C1 Mo C3 O3 -48(7) . . . . ? C2 Mo C3 O3 66(7) . . . . ? C5 Mo C3 O3 -149(7) . . . . ? C6 Mo C3 O3 174(7) . . . . ? C4 Mo C3 O3 -135(7) . . . . ? C7 Mo C3 O3 158(7) . . . . ? Cl Mo C3 O3 12(7) . . . . ? C8 Mo C3 O3 -169(7) . . . . ? C3 Mo C2 O2 117(4) . . . . ? C1 Mo C2 O2 -169(4) . . . . ? C5 Mo C2 O2 49(4) . . . . ? C6 Mo C2 O2 36(4) . . . . ? C4 Mo C2 O2 -17(4) . . . . ? C7 Mo C2 O2 1(4) . . . . ? Cl Mo C2 O2 -95(4) . . . . ? C8 Mo C2 O2 -25(4) . . . . ? C3 Mo C4 C5 -25.4(2) . . . . ? C1 Mo C4 C5 -104.5(2) . . . . ? C2 Mo C4 C5 101.5(3) . . . . ? C6 Mo C4 C5 38.60(19) . . . . ? C7 Mo C4 C5 80.2(2) . . . . ? Cl Mo C4 C5 174.74(19) . . . . ? C8 Mo C4 C5 113.7(3) . . . . ? C3 Mo C4 C8 -139.09(18) . . . . ? C1 Mo C4 C8 141.78(19) . . . . ? C2 Mo C4 C8 -12.2(3) . . . . ? C5 Mo C4 C8 -113.7(3) . . . . ? C6 Mo C4 C8 -75.13(18) . . . . ? C7 Mo C4 C8 -33.54(16) . . . . ? Cl Mo C4 C8 61.01(16) . . . . ? C8 C4 C5 C6 7.0(3) . . . . ? Mo C4 C5 C6 -65.3(2) . . . . ? C8 C4 C5 Mo 72.22(19) . . . . ? C3 Mo C5 C4 157.6(2) . . . . ? C1 Mo C5 C4 79.5(2) . . . . ? C2 Mo C5 C4 -136.4(2) . . . . ? C6 Mo C5 C4 -115.0(3) . . . . ? C7 Mo C5 C4 -77.6(2) . . . . ? Cl Mo C5 C4 -6.9(3) . . . . ? C8 Mo C5 C4 -37.52(17) . . . . ? C3 Mo C5 C6 -87.3(2) . . . . ? C1 Mo C5 C6 -165.5(2) . . . . ? C2 Mo C5 C6 -21.4(3) . . . . ? C4 Mo C5 C6 115.0(3) . . . . ? C7 Mo C5 C6 37.48(18) . . . . ? Cl Mo C5 C6 108.1(2) . . . . ? C8 Mo C5 C6 77.5(2) . . . . ? C4 C5 C6 C7 -0.2(3) . . . . ? Mo C5 C6 C7 -67.3(2) . . . . ? C4 C5 C6 Mo 67.0(2) . . . . ? C3 Mo C6 C7 -155.5(2) . . . . ? C1 Mo C6 C7 135.9(2) . . . . ? C2 Mo C6 C7 -78.3(2) . . . . ? C5 Mo C6 C7 115.4(3) . . . . ? C4 Mo C6 C7 77.56(19) . . . . ? Cl Mo C6 C7 9.8(2) . . . . ? C8 Mo C6 C7 37.46(16) . . . . ? C3 Mo C6 C5 89.1(2) . . . . ? C1 Mo C6 C5 20.5(3) . . . . ? C2 Mo C6 C5 166.25(19) . . . . ? C4 Mo C6 C5 -37.86(19) . . . . ? C7 Mo C6 C5 -115.4(3) . . . . ? Cl Mo C6 C5 -105.6(2) . . . . ? C8 Mo C6 C5 -78.0(2) . . . . ? C5 C6 C7 C8 -6.6(3) . . . . ? Mo C6 C7 C8 -70.86(19) . . . . ? C5 C6 C7 Mo 64.3(2) . . . . ? C3 Mo C7 C6 27.5(2) . . . . ? C1 Mo C7 C6 -90.0(3) . . . . ? C2 Mo C7 C6 108.9(2) . . . . ? C5 Mo C7 C6 -38.49(19) . . . . ? C4 Mo C7 C6 -80.4(2) . . . . ? Cl Mo C7 C6 -172.67(18) . . . . ? C8 Mo C7 C6 -114.0(3) . . . . ? C3 Mo C7 C8 141.46(18) . . . . ? C1 Mo C7 C8 24.0(3) . . . . ? C2 Mo C7 C8 -137.15(18) . . . . ? C5 Mo C7 C8 75.49(19) . . . . ? C6 Mo C7 C8 114.0(3) . . . . ? C4 Mo C7 C8 33.58(16) . . . . ? Cl Mo C7 C8 -58.69(17) . . . . ? C10 N C8 C4 173.3(3) . . . . ? C9 N C8 C4 5.0(4) . . . . ? C10 N C8 C7 -4.8(4) . . . . ? C9 N C8 C7 -173.1(2) . . . . ? C10 N C8 Mo 84.8(3) . . . . ? C9 N C8 Mo -83.5(3) . . . . ? C5 C4 C8 N 170.8(3) . . . . ? Mo C4 C8 N -124.8(3) . . . . ? C5 C4 C8 C7 -10.8(3) . . . . ? Mo C4 C8 C7 53.59(18) . . . . ? C5 C4 C8 Mo -64.41(19) . . . . ? C6 C7 C8 N -171.0(3) . . . . ? Mo C7 C8 N 125.5(3) . . . . ? C6 C7 C8 C4 10.6(3) . . . . ? Mo C7 C8 C4 -52.86(18) . . . . ? C6 C7 C8 Mo 63.5(2) . . . . ? C3 Mo C8 N -177.9(3) . . . . ? C1 Mo C8 N 74.5(3) . . . . ? C2 Mo C8 N -67.2(3) . . . . ? C5 Mo C8 N 158.5(3) . . . . ? C6 Mo C8 N -157.8(3) . . . . ? C4 Mo C8 N 119.0(3) . . . . ? C7 Mo C8 N -118.6(4) . . . . ? Cl Mo C8 N 1.5(3) . . . . ? C3 Mo C8 C4 63.2(2) . . . . ? C1 Mo C8 C4 -44.5(2) . . . . ? C2 Mo C8 C4 173.80(17) . . . . ? C5 Mo C8 C4 39.50(18) . . . . ? C6 Mo C8 C4 83.19(19) . . . . ? C7 Mo C8 C4 122.4(3) . . . . ? Cl Mo C8 C4 -117.46(17) . . . . ? C3 Mo C8 C7 -59.2(2) . . . . ? C1 Mo C8 C7 -166.91(18) . . . . ? C2 Mo C8 C7 51.4(2) . . . . ? C5 Mo C8 C7 -82.9(2) . . . . ? C6 Mo C8 C7 -39.20(19) . . . . ? C4 Mo C8 C7 -122.4(3) . . . . ? Cl Mo C8 C7 120.15(17) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.033 _refine_diff_density_min -1.069 _refine_diff_density_rms 0.128 # Attachment 'Complex 20.cif' data_croizat_sur _database_code_depnum_ccdc_archive 'CCDC 297956' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H15 Cl Mo N2 O3 Pt' _chemical_formula_sum 'C17 H15 Cl Mo N2 O3 Pt' _chemical_formula_weight 621.79 _chemical_absolute_configuration . 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' 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' 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' Pt Pt -1.7033 8.3905 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4770(10) _cell_length_b 9.6370(10) _cell_length_c 10.4300(10) _cell_angle_alpha 82.48(5) _cell_angle_beta 83.48(5) _cell_angle_gamma 73.05(5) _cell_volume 900.49(16) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 18849 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 32.032 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.293 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 584 _exptl_absorpt_coefficient_mu 8.622 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6235 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1346 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 32.20 _reflns_number_total 6234 _reflns_number_gt 3771 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6234 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0985 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1059 _refine_ls_wR_factor_gt 0.0898 _refine_ls_goodness_of_fit_ref 0.855 _refine_ls_restrained_S_all 0.855 _refine_ls_shift/su_max 0.000 _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 Pt Pt 0.47332(3) 0.23392(3) 0.14904(3) 0.02807(9) Uani 1 1 d . . . Mo Mo 0.72886(6) 0.13795(7) 0.27513(5) 0.02932(14) Uani 1 1 d . . . Cl Cl 0.2687(2) 0.3203(2) 0.01534(18) 0.0398(4) Uani 1 1 d . . . O1 O 0.5489(7) 0.4359(7) 0.3750(6) 0.0605(17) Uani 1 1 d . . . O2 O 0.5311(5) -0.0716(5) 0.3708(5) 0.0382(12) Uani 1 1 d . . . O3 O 0.8159(6) 0.0533(7) 0.5635(5) 0.0528(15) Uani 1 1 d . . . N1 N 0.3351(6) 0.2581(6) 0.3041(6) 0.0316(13) Uani 1 1 d . . . N2 N 0.6301(6) 0.2077(6) -0.0090(5) 0.0291(12) Uani 1 1 d . . . C1 C 0.6130(9) 0.3229(9) 0.3413(7) 0.0395(17) Uani 1 1 d . . . C2 C 0.5987(8) 0.0109(8) 0.3370(6) 0.0329(15) Uani 1 1 d . . . C3 C 0.7850(8) 0.0857(9) 0.4575(7) 0.0395(17) Uani 1 1 d . . . C4 C 0.8335(8) 0.0075(8) 0.0995(7) 0.0338(16) Uani 1 1 d . . . H4 H 0.8040 -0.0749 0.0848 0.041 Uiso 1 1 calc . . . C5 C 0.9501(9) 0.0073(9) 0.1724(7) 0.045(2) Uani 1 1 d . . . H5 H 1.0144 -0.0760 0.2158 0.054 Uiso 1 1 calc . . . C6 C 0.9543(8) 0.1544(9) 0.1696(7) 0.0411(18) Uani 1 1 d . . . H6 H 1.0225 0.1853 0.2110 0.049 Uiso 1 1 calc . . . C7 C 0.8430(8) 0.2452(8) 0.0966(7) 0.0382(17) Uani 1 1 d . . . H7 H 0.8208 0.3482 0.0796 0.046 Uiso 1 1 calc . . . C8 C 0.7689(7) 0.1547(7) 0.0525(6) 0.0286(14) Uani 1 1 d . . . C9 C 0.6163(9) 0.3517(9) -0.0897(7) 0.046(2) Uani 1 1 d . . . H9A H 0.6222 0.4244 -0.0346 0.068 Uiso 1 1 calc . . . H9B H 0.5209 0.3836 -0.1281 0.068 Uiso 1 1 calc . . . H9C H 0.6967 0.3407 -0.1588 0.068 Uiso 1 1 calc . . . C10 C 0.6104(9) 0.1043(9) -0.0949(8) 0.048(2) Uani 1 1 d . . . H10A H 0.6918 0.0876 -0.1630 0.072 Uiso 1 1 calc . . . H10B H 0.5162 0.1456 -0.1346 0.072 Uiso 1 1 calc . . . H10C H 0.6101 0.0116 -0.0436 0.072 Uiso 1 1 calc . . . C11 C 0.2582(7) 0.2784(7) 0.3974(7) 0.0328(15) Uani 1 1 d . . . C12 C 0.1603(8) 0.3141(7) 0.5114(6) 0.0322(15) Uani 1 1 d . . . C13 C 0.0183(8) 0.3043(8) 0.5223(7) 0.0393(17) Uani 1 1 d . . . H13 H -0.0155 0.2662 0.4559 0.047 Uiso 1 1 calc . . . C14 C -0.0768(9) 0.3496(9) 0.6296(8) 0.049(2) Uani 1 1 d . . . H14 H -0.1764 0.3459 0.6351 0.058 Uiso 1 1 calc . . . C15 C -0.0265(11) 0.3996(9) 0.7273(7) 0.053(2) Uani 1 1 d . . . H15 H -0.0908 0.4298 0.8015 0.063 Uiso 1 1 calc . . . C16 C 0.1179(11) 0.4063(9) 0.7180(8) 0.053(2) Uani 1 1 d . . . H16 H 0.1524 0.4407 0.7863 0.063 Uiso 1 1 calc . . . C17 C 0.2126(9) 0.3636(9) 0.6109(8) 0.0452(19) Uani 1 1 d . . . H17 H 0.3120 0.3680 0.6051 0.054 Uiso 1 1 calc . . . 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 Pt 0.03062(14) 0.02924(14) 0.02615(14) -0.00454(10) 0.00029(10) -0.01144(10) Mo 0.0291(3) 0.0375(3) 0.0243(3) -0.0065(2) 0.0019(2) -0.0140(3) Cl 0.0450(10) 0.0384(10) 0.0379(10) 0.0000(8) -0.0135(8) -0.0127(8) O1 0.065(4) 0.058(4) 0.067(4) -0.036(3) 0.010(3) -0.024(3) O2 0.037(3) 0.041(3) 0.038(3) -0.002(2) -0.001(2) -0.016(2) O3 0.053(3) 0.079(4) 0.034(3) -0.004(3) -0.012(3) -0.028(3) N1 0.026(3) 0.030(3) 0.037(3) 0.000(3) -0.005(3) -0.006(2) N2 0.032(3) 0.032(3) 0.024(3) -0.005(2) 0.002(2) -0.011(2) C1 0.047(4) 0.044(4) 0.034(4) -0.014(3) -0.001(3) -0.019(4) C2 0.034(4) 0.041(4) 0.025(3) -0.005(3) -0.001(3) -0.010(3) C3 0.031(4) 0.057(5) 0.035(4) -0.005(4) -0.002(3) -0.021(4) C4 0.033(4) 0.038(4) 0.031(4) -0.005(3) 0.007(3) -0.012(3) C5 0.043(4) 0.051(5) 0.032(4) -0.003(4) 0.006(3) 0.000(4) C6 0.033(4) 0.068(6) 0.028(4) -0.010(4) 0.001(3) -0.022(4) C7 0.044(4) 0.041(4) 0.035(4) -0.009(3) 0.013(3) -0.025(3) C8 0.025(3) 0.038(4) 0.023(3) -0.009(3) 0.007(3) -0.011(3) C9 0.041(4) 0.056(5) 0.033(4) 0.007(4) 0.009(3) -0.013(4) C10 0.053(5) 0.059(5) 0.044(5) -0.032(4) -0.003(4) -0.023(4) C11 0.023(3) 0.032(4) 0.040(4) -0.001(3) 0.000(3) -0.005(3) C12 0.039(4) 0.030(4) 0.027(3) -0.005(3) 0.002(3) -0.011(3) C13 0.042(4) 0.041(4) 0.037(4) -0.004(3) 0.003(3) -0.016(3) C14 0.047(5) 0.056(5) 0.043(5) -0.009(4) 0.015(4) -0.021(4) C15 0.070(6) 0.050(5) 0.029(4) -0.005(4) 0.016(4) -0.011(4) C16 0.073(6) 0.051(5) 0.031(4) -0.011(4) -0.014(4) -0.005(5) C17 0.045(5) 0.043(5) 0.049(5) -0.009(4) -0.011(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 Pt N1 1.956(6) . ? Pt N2 2.079(5) . ? Pt Cl 2.401(2) . ? Pt Mo 2.7475(14) . ? Mo C1 1.967(8) . ? Mo C2 1.983(7) . ? Mo C3 1.995(8) . ? Mo C8 2.302(6) . ? Mo C4 2.320(7) . ? Mo C7 2.323(7) . ? Mo C6 2.328(7) . ? Mo C5 2.331(8) . ? O1 C1 1.159(9) . ? O2 C2 1.157(8) . ? O3 C3 1.155(8) . ? N1 C11 1.149(8) . ? N2 C8 1.455(9) . ? N2 C10 1.486(9) . ? N2 C9 1.505(9) . ? C4 C5 1.411(11) . ? C4 C8 1.417(9) . ? C4 H4 0.9500 . ? C5 C6 1.426(11) . ? C5 H5 0.9500 . ? C6 C7 1.388(11) . ? C6 H6 0.9500 . ? C7 C8 1.414(9) . ? C7 H7 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.437(9) . ? C12 C13 1.367(10) . ? C12 C17 1.391(10) . ? C13 C14 1.387(10) . ? C13 H13 0.9500 . ? C14 C15 1.369(12) . ? C14 H14 0.9500 . ? C15 C16 1.380(13) . ? C15 H15 0.9500 . ? C16 C17 1.379(12) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pt N2 176.7(2) . . ? N1 Pt Cl 89.83(17) . . ? N2 Pt Cl 93.37(16) . . ? N1 Pt Mo 96.94(16) . . ? N2 Pt Mo 79.83(15) . . ? Cl Pt Mo 173.11(5) . . ? C1 Mo C2 101.4(3) . . ? C1 Mo C3 83.1(3) . . ? C2 Mo C3 81.2(3) . . ? C1 Mo C8 113.4(3) . . ? C2 Mo C8 110.8(3) . . ? C3 Mo C8 155.9(3) . . ? C1 Mo C4 149.0(3) . . ? C2 Mo C4 93.1(3) . . ? C3 Mo C4 126.5(3) . . ? C8 Mo C4 35.7(2) . . ? C1 Mo C7 95.3(3) . . ? C2 Mo C7 146.3(3) . . ? C3 Mo C7 130.1(3) . . ? C8 Mo C7 35.6(2) . . ? C4 Mo C7 59.8(2) . . ? C1 Mo C6 111.8(3) . . ? C2 Mo C6 146.7(3) . . ? C3 Mo C6 100.2(3) . . ? C8 Mo C6 58.2(2) . . ? C4 Mo C6 59.1(3) . . ? C7 Mo C6 34.7(3) . . ? C1 Mo C5 147.3(3) . . ? C2 Mo C5 111.1(3) . . ? C3 Mo C5 98.0(3) . . ? C8 Mo C5 58.6(3) . . ? C4 Mo C5 35.3(3) . . ? C7 Mo C5 59.1(3) . . ? C6 Mo C5 35.6(3) . . ? C1 Mo Pt 72.8(2) . . ? C2 Mo Pt 70.3(2) . . ? C3 Mo Pt 137.5(2) . . ? C8 Mo Pt 66.26(17) . . ? C4 Mo Pt 86.85(18) . . ? C7 Mo Pt 87.4(2) . . ? C6 Mo Pt 120.98(19) . . ? C5 Mo Pt 121.1(2) . . ? C11 N1 Pt 175.6(6) . . ? C8 N2 C10 112.8(5) . . ? C8 N2 C9 112.3(5) . . ? C10 N2 C9 107.3(6) . . ? C8 N2 Pt 102.6(4) . . ? C10 N2 Pt 112.1(4) . . ? C9 N2 Pt 109.9(4) . . ? O1 C1 Mo 176.2(7) . . ? O2 C2 Mo 175.1(6) . . ? O3 C3 Mo 178.6(7) . . ? C5 C4 C8 106.5(6) . . ? C5 C4 Mo 72.8(4) . . ? C8 C4 Mo 71.4(4) . . ? C5 C4 H4 126.7 . . ? C8 C4 H4 126.7 . . ? Mo C4 H4 120.9 . . ? C4 C5 C6 107.8(7) . . ? C4 C5 Mo 71.9(4) . . ? C6 C5 Mo 72.1(4) . . ? C4 C5 H5 126.1 . . ? C6 C5 H5 126.1 . . ? Mo C5 H5 121.7 . . ? C7 C6 C5 109.2(7) . . ? C7 C6 Mo 72.4(4) . . ? C5 C6 Mo 72.3(4) . . ? C7 C6 H6 125.4 . . ? C5 C6 H6 125.4 . . ? Mo C6 H6 121.6 . . ? C6 C7 C8 106.8(7) . . ? C6 C7 Mo 72.8(4) . . ? C8 C7 Mo 71.4(4) . . ? C6 C7 H7 126.6 . . ? C8 C7 H7 126.6 . . ? Mo C7 H7 121.0 . . ? C7 C8 C4 109.7(6) . . ? C7 C8 N2 124.5(6) . . ? C4 C8 N2 124.7(6) . . ? C7 C8 Mo 73.0(4) . . ? C4 C8 Mo 72.8(4) . . ? N2 C8 Mo 111.3(4) . . ? N2 C9 H9A 109.5 . . ? N2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C10 H10A 109.5 . . ? N2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C12 176.1(7) . . ? C13 C12 C17 120.1(7) . . ? C13 C12 C11 122.0(7) . . ? C17 C12 C11 118.0(7) . . ? C12 C13 C14 120.5(7) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C15 C14 C13 119.7(8) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C14 C15 C16 119.9(7) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C17 C16 C15 120.8(8) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C16 C17 C12 119.0(7) . . ? C16 C17 H17 120.5 . . ? C12 C17 H17 120.5 . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 32.20 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.854 _refine_diff_density_min -1.846 _refine_diff_density_rms 0.234