Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global #========================================================================= # 1. SUBMISSION DETAILS _publ_contact_author ; Professor N.G. Connelly, School of Chemistry, Cantocks Close, University of Bristol. Bristol. BS8 1TS. ; _publ_contact_author_phone '0117 928 8162' _publ_contact_author_fax '0117 929 0509' _publ_contact_author_email Neil.Connelly@bristol.ac.uk _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; ; #========================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_Cambridge 186 _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #========================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Molybdenum-based alkyne-isocyanide coupling reactions: synthesis of a reactive diiminometallacyclopentene complex ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Adams, Christopher J.' ; School of Chemistry University of Bristol Cantocks Close BS8 1TS. Bristol, UK ; 'Anderson, Kirsty M.' ; School of Chemistry University of Bristol Cantocks Close BS8 1TS. Bristol, UK ; 'Bartlett, Ian M.' ; School of Chemistry University of Bristol Cantocks Close BS8 1TS. Bristol, UK ; 'Connelly, Neil G.' ; School of Chemistry University of Bristol Cantocks Close BS8 1TS. Bristol, UK ; 'Paget, Timothy J.' ; School of Chemistry University of Bristol Cantocks Close BS8 1TS. Bristol, UK ; 'Phetmung, Hirihattaya' ; School of Chemistry University of Bristol Cantocks Close BS8 1TS. Bristol, UK ; 'Orpen, A. Guy' ; School of Chemistry University of Bristol Cantocks Close BS8 1TS. Bristol, UK ; 'Smith, David W.' ; ? ; #========================================================================= # 4. TEXT # # # N.G. CONNELLY # data_3 _database_code_CSD 155026 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H59 B F4 Mo N4 O' _chemical_formula_weight 914.76 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' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.409(9) _cell_length_b 13.762(4) _cell_length_c 20.048(6) _cell_angle_alpha 90.00 _cell_angle_beta 99.402(18) _cell_angle_gamma 90.00 _cell_volume 4739(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 68 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.282 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1912 _exptl_absorpt_coefficient_mu 0.332 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.760949 _exptl_absorpt_correction_T_max 0.934761 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Siemens CCD Area Diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 24924 _diffrn_reflns_av_R_equivalents 0.1868 _diffrn_reflns_av_sigmaI/netI 0.2191 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8349 _reflns_number_gt 3602 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0493P)^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 8349 _refine_ls_number_parameters 563 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2035 _refine_ls_R_factor_gt 0.0719 _refine_ls_wR_factor_ref 0.1580 _refine_ls_wR_factor_gt 0.1151 _refine_ls_goodness_of_fit_ref 0.973 _refine_ls_restrained_S_all 0.973 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.32444(4) 0.16428(5) 1.14200(3) 0.03309(19) Uani 1 1 d . . . N1 N 0.2168(3) 0.2722(5) 1.0176(3) 0.0414(17) Uani 1 1 d . . . N2 N 0.4468(4) 0.2819(4) 1.0672(3) 0.0428(17) Uani 1 1 d . . . N3 N 0.4152(3) 0.2853(4) 1.2695(3) 0.0381(16) Uani 1 1 d . . . N4 N 0.1794(4) 0.2305(4) 1.2129(3) 0.0389(16) Uani 1 1 d . . . C1 C 0.2722(4) 0.0140(5) 1.1082(4) 0.038(2) Uani 1 1 d . . . C2 C 0.3430(5) 0.0276(5) 1.0803(4) 0.048(2) Uani 1 1 d . . . C3 C 0.4060(5) 0.0317(5) 1.1345(5) 0.051(2) Uani 1 1 d . . . C4 C 0.3761(5) 0.0201(5) 1.1952(4) 0.046(2) Uani 1 1 d . . . C5 C 0.2949(4) 0.0091(5) 1.1796(4) 0.038(2) Uani 1 1 d . . . C6 C 0.1932(4) -0.0054(6) 1.0697(4) 0.058(2) Uani 1 1 d . . . H6A H 0.1873 -0.0752 1.0605 0.087 Uiso 1 1 calc R . . H6B H 0.1864 0.0303 1.0268 0.087 Uiso 1 1 calc R . . H6C H 0.1538 0.0159 1.0964 0.087 Uiso 1 1 calc R . . C7 C 0.3484(6) 0.0273(6) 1.0050(4) 0.084(3) Uani 1 1 d . . . H7A H 0.3614 -0.0382 0.9913 0.126 Uiso 1 1 calc R . . H7B H 0.3889 0.0729 0.9964 0.126 Uiso 1 1 calc R . . H7C H 0.2982 0.0471 0.9790 0.126 Uiso 1 1 calc R . . C8 C 0.4919(5) 0.0370(6) 1.1269(6) 0.099(4) Uani 1 1 d . . . H8A H 0.5138 -0.0288 1.1286 0.148 Uiso 1 1 calc R . . H8B H 0.5204 0.0759 1.1638 0.148 Uiso 1 1 calc R . . H8C H 0.4966 0.0671 1.0835 0.148 Uiso 1 1 calc R . . C9 C 0.4240(5) 0.0136(6) 1.2652(4) 0.079(3) Uani 1 1 d . . . H9A H 0.4415 -0.0535 1.2741 0.118 Uiso 1 1 calc R . . H9B H 0.3920 0.0335 1.2988 0.118 Uiso 1 1 calc R . . H9C H 0.4693 0.0565 1.2680 0.118 Uiso 1 1 calc R . . C10 C 0.2412(5) -0.0129(5) 1.2294(4) 0.056(2) Uani 1 1 d . . . H10A H 0.2411 -0.0830 1.2379 0.083 Uiso 1 1 calc R . . H10B H 0.1883 0.0085 1.2108 0.083 Uiso 1 1 calc R . . H10C H 0.2593 0.0215 1.2719 0.083 Uiso 1 1 calc R . . C11 C 0.2550(4) 0.2328(6) 1.0648(4) 0.039(2) Uani 1 1 d . . . C12 C 0.1790(4) 0.3407(7) 0.9710(4) 0.045(2) Uani 1 1 d . . . C13 C 0.1664(5) 0.4336(7) 0.9940(5) 0.059(3) Uani 1 1 d . . . C14 C 0.1908(5) 0.4618(7) 1.0658(4) 0.076(3) Uani 1 1 d . . . H14A H 0.2472 0.4532 1.0784 0.114 Uiso 1 1 calc R . . H14B H 0.1640 0.4207 1.0947 0.114 Uiso 1 1 calc R . . H14C H 0.1774 0.5300 1.0719 0.114 Uiso 1 1 calc R . . C15 C 0.1306(6) 0.4985(7) 0.9449(7) 0.084(3) Uani 1 1 d . . . H15A H 0.1208 0.5635 0.9570 0.101 Uiso 1 1 calc R . . C16 C 0.1095(6) 0.4685(10) 0.8793(6) 0.089(4) Uani 1 1 d . . . H16A H 0.0833 0.5134 0.8475 0.107 Uiso 1 1 calc R . . C17 C 0.1240(6) 0.3780(9) 0.8571(5) 0.079(3) Uani 1 1 d . . . H17A H 0.1104 0.3616 0.8107 0.095 Uiso 1 1 calc R . . C18 C 0.1596(5) 0.3087(7) 0.9043(5) 0.056(3) Uani 1 1 d . . . C19 C 0.1777(5) 0.2098(7) 0.8812(4) 0.067(3) Uani 1 1 d . . . H19A H 0.1661 0.1615 0.9141 0.101 Uiso 1 1 calc R . . H19B H 0.2330 0.2062 0.8772 0.101 Uiso 1 1 calc R . . H19C H 0.1460 0.1967 0.8371 0.101 Uiso 1 1 calc R . . C20 C 0.4017(4) 0.2433(5) 1.0963(4) 0.038(2) Uani 1 1 d . . . C21 C 0.4953(4) 0.3293(6) 1.0291(4) 0.0447(19) Uani 1 1 d . . . C22 C 0.4617(5) 0.3682(6) 0.9667(4) 0.053(2) Uani 1 1 d . . . C23 C 0.3770(5) 0.3544(7) 0.9404(4) 0.072(3) Uani 1 1 d . . . H23A H 0.3634 0.3883 0.8970 0.108 Uiso 1 1 calc R . . H23B H 0.3462 0.3810 0.9729 0.108 Uiso 1 1 calc R . . H23C H 0.3658 0.2849 0.9339 0.108 Uiso 1 1 calc R . . C24 C 0.5100(6) 0.4172(7) 0.9312(4) 0.069(3) Uani 1 1 d . . . H24A H 0.4890 0.4455 0.8890 0.083 Uiso 1 1 calc R . . C25 C 0.5897(7) 0.4269(7) 0.9555(6) 0.080(3) Uani 1 1 d . . . H25A H 0.6220 0.4611 0.9296 0.096 Uiso 1 1 calc R . . C26 C 0.6214(5) 0.3873(7) 1.0166(6) 0.072(3) Uani 1 1 d . . . H26A H 0.6755 0.3947 1.0327 0.087 Uiso 1 1 calc R . . C27 C 0.5750(5) 0.3359(6) 1.0558(4) 0.053(2) Uani 1 1 d . . . C28 C 0.6076(5) 0.2904(7) 1.1216(5) 0.073(3) Uani 1 1 d . . . H28A H 0.5755 0.3083 1.1556 0.109 Uiso 1 1 calc R . . H28B H 0.6610 0.3134 1.1361 0.109 Uiso 1 1 calc R . . H28C H 0.6077 0.2196 1.1165 0.109 Uiso 1 1 calc R . . C29 C 0.3817(4) 0.2435(6) 1.2233(4) 0.0348(19) Uani 1 1 d . . . C30 C 0.4541(4) 0.3459(6) 1.3197(3) 0.0333(18) Uani 1 1 d . . . C31 C 0.4801(4) 0.4361(6) 1.3009(3) 0.0330(18) Uani 1 1 d . . . C32 C 0.4645(5) 0.4686(6) 1.2283(4) 0.054(2) Uani 1 1 d . . . H32A H 0.4117 0.4494 1.2079 0.080 Uiso 1 1 calc R . . H32B H 0.5022 0.4381 1.2036 0.080 Uiso 1 1 calc R . . H32C H 0.4695 0.5394 1.2263 0.080 Uiso 1 1 calc R . . C33 C 0.5179(4) 0.4959(6) 1.3498(4) 0.043(2) Uani 1 1 d . . . H33A H 0.5362 0.5576 1.3380 0.051 Uiso 1 1 calc R . . C34 C 0.5296(5) 0.4661(7) 1.4164(4) 0.055(2) Uani 1 1 d . . . H34A H 0.5559 0.5080 1.4503 0.067 Uiso 1 1 calc R . . C35 C 0.5039(5) 0.3768(6) 1.4350(4) 0.047(2) Uani 1 1 d . . . H35A H 0.5125 0.3583 1.4813 0.057 Uiso 1 1 calc R . . C36 C 0.4657(4) 0.3142(6) 1.3868(4) 0.039(2) Uani 1 1 d . . . C37 C 0.4374(5) 0.2149(6) 1.4053(4) 0.058(2) Uani 1 1 d . . . H37A H 0.4529 0.2040 1.4539 0.087 Uiso 1 1 calc R . . H37B H 0.4606 0.1646 1.3802 0.087 Uiso 1 1 calc R . . H37C H 0.3806 0.2121 1.3937 0.087 Uiso 1 1 calc R . . C38 C 0.2330(4) 0.2098(5) 1.1872(3) 0.0347(19) Uani 1 1 d . . . C39 C 0.1108(4) 0.2476(5) 1.2398(4) 0.0367(18) Uani 1 1 d . . . C40 C 0.1163(4) 0.2575(5) 1.3100(4) 0.0371(19) Uani 1 1 d . . . C41 C 0.1936(4) 0.2485(6) 1.3559(4) 0.052(2) Uani 1 1 d . . . H41A H 0.1867 0.2610 1.4027 0.078 Uiso 1 1 calc R . . H41B H 0.2302 0.2960 1.3424 0.078 Uiso 1 1 calc R . . H41C H 0.2142 0.1828 1.3524 0.078 Uiso 1 1 calc R . . C42 C 0.0479(5) 0.2751(5) 1.3340(4) 0.051(2) Uani 1 1 d . . . H42A H 0.0494 0.2842 1.3811 0.061 Uiso 1 1 calc R . . C43 C -0.0224(5) 0.2797(6) 1.2917(4) 0.052(2) Uani 1 1 d . . . H43A H -0.0689 0.2892 1.3099 0.062 Uiso 1 1 calc R . . C44 C -0.0256(5) 0.2708(5) 1.2230(4) 0.048(2) Uani 1 1 d . . . H44A H -0.0744 0.2759 1.1941 0.057 Uiso 1 1 calc R . . C45 C 0.0408(5) 0.2546(5) 1.1951(4) 0.045(2) Uani 1 1 d . . . C46 C 0.0385(4) 0.2473(6) 1.1197(4) 0.056(2) Uani 1 1 d . . . H46A H 0.0714 0.1932 1.1097 0.083 Uiso 1 1 calc R . . H46B H 0.0578 0.3080 1.1029 0.083 Uiso 1 1 calc R . . H46C H -0.0152 0.2361 1.0974 0.083 Uiso 1 1 calc R . . B1 B -0.1994(6) 0.2213(9) 1.0575(6) 0.059(3) Uani 1 1 d . . . F1 F -0.1973(3) 0.2780(4) 1.1134(2) 0.0781(16) Uani 1 1 d . . . F2 F -0.2698(3) 0.1815(4) 1.0359(2) 0.0810(16) Uani 1 1 d . . . F3 F -0.1415(3) 0.1569(5) 1.0654(3) 0.149(3) Uani 1 1 d . . . F4 F -0.1878(4) 0.2831(5) 1.0050(3) 0.134(3) Uani 1 1 d . . . C103 C -0.3115(6) -0.0403(10) 1.2011(7) 0.122(5) Uani 1 1 d . . . H11D H -0.3637 -0.0260 1.2124 0.146 Uiso 1 1 calc R . . H11E H -0.3180 -0.0882 1.1638 0.146 Uiso 1 1 calc R . . C102 C -0.2664(9) -0.0779(10) 1.2549(7) 0.122(4) Uani 1 1 d . . . H11F H -0.2493 -0.1440 1.2446 0.147 Uiso 1 1 calc R . . H11G H -0.2955 -0.0822 1.2933 0.147 Uiso 1 1 calc R . . C104 C -0.2801(11) 0.0414(15) 1.1813(9) 0.216(9) Uani 1 1 d . . . H11H H -0.3216 0.0906 1.1697 0.259 Uiso 1 1 calc R . . H11I H -0.2578 0.0277 1.1399 0.259 Uiso 1 1 calc R . . C101 C -0.1965(9) -0.0115(12) 1.2728(7) 0.149(6) Uani 1 1 d . . . H11J H -0.1494 -0.0411 1.2596 0.179 Uiso 1 1 calc R . . H11K H -0.1863 0.0023 1.3220 0.179 Uiso 1 1 calc R . . O101 O -0.2198(11) 0.0812(11) 1.2322(8) 0.262(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0336(3) 0.0298(4) 0.0368(3) -0.0005(4) 0.0085(3) -0.0018(4) N1 0.040(4) 0.050(5) 0.035(4) 0.005(4) 0.010(3) -0.006(3) N2 0.043(4) 0.038(4) 0.052(4) 0.002(3) 0.019(3) 0.000(3) N3 0.040(4) 0.037(4) 0.039(4) -0.005(3) 0.010(3) -0.005(3) N4 0.038(4) 0.032(4) 0.049(4) -0.002(3) 0.013(3) -0.004(3) C1 0.034(5) 0.038(5) 0.040(5) -0.006(4) 0.002(4) 0.001(4) C2 0.073(6) 0.025(5) 0.052(5) -0.009(4) 0.027(5) -0.014(4) C3 0.045(5) 0.021(5) 0.090(7) 0.003(5) 0.024(5) -0.002(4) C4 0.054(6) 0.013(5) 0.067(6) -0.008(4) 0.000(5) 0.005(4) C5 0.037(5) 0.042(5) 0.038(5) 0.004(4) 0.014(4) -0.004(4) C6 0.054(6) 0.051(6) 0.065(6) -0.010(5) -0.004(5) -0.007(4) C7 0.150(10) 0.052(7) 0.067(6) -0.017(5) 0.069(6) -0.015(6) C8 0.048(6) 0.046(6) 0.211(12) 0.003(7) 0.047(7) 0.007(5) C9 0.088(8) 0.038(6) 0.091(7) 0.008(5) -0.042(6) -0.006(5) C10 0.080(6) 0.031(5) 0.061(6) 0.009(4) 0.026(5) -0.002(4) C11 0.036(5) 0.051(6) 0.032(5) -0.011(4) 0.012(4) -0.010(4) C12 0.035(4) 0.061(6) 0.038(5) 0.021(5) -0.003(4) -0.002(5) C13 0.053(6) 0.039(6) 0.088(8) 0.009(6) 0.019(5) 0.002(5) C14 0.087(8) 0.064(7) 0.076(7) -0.004(6) 0.008(6) -0.004(6) C15 0.069(8) 0.045(7) 0.132(10) 0.018(7) -0.005(7) 0.003(6) C16 0.071(8) 0.104(11) 0.082(9) 0.056(8) -0.020(7) -0.007(8) C17 0.067(7) 0.093(9) 0.070(7) 0.021(7) -0.013(6) -0.006(7) C18 0.039(5) 0.066(8) 0.063(6) 0.016(6) 0.011(5) -0.003(5) C19 0.053(6) 0.103(8) 0.045(5) -0.004(5) 0.007(5) -0.007(6) C20 0.039(5) 0.030(5) 0.045(5) -0.002(4) 0.010(4) 0.002(4) C21 0.042(5) 0.040(5) 0.059(5) 0.001(5) 0.030(4) 0.003(5) C22 0.079(7) 0.039(6) 0.051(5) -0.002(4) 0.039(5) -0.012(5) C23 0.082(7) 0.076(8) 0.056(5) 0.004(5) 0.006(5) -0.012(6) C24 0.094(8) 0.062(7) 0.061(6) 0.003(5) 0.038(6) 0.007(6) C25 0.109(9) 0.042(6) 0.109(9) 0.010(6) 0.079(8) 0.000(6) C26 0.056(6) 0.054(7) 0.118(9) -0.007(6) 0.047(6) -0.005(5) C27 0.054(5) 0.034(5) 0.079(6) -0.005(5) 0.038(5) 0.004(5) C28 0.046(6) 0.066(7) 0.108(8) 0.008(6) 0.018(6) -0.002(5) C29 0.026(4) 0.038(5) 0.043(5) 0.006(4) 0.010(4) 0.002(4) C30 0.035(4) 0.029(5) 0.038(4) -0.002(4) 0.010(3) -0.009(4) C31 0.038(5) 0.040(5) 0.019(4) 0.002(4) 0.000(3) 0.006(4) C32 0.066(6) 0.041(6) 0.058(6) 0.005(5) 0.022(5) 0.004(5) C33 0.042(5) 0.048(6) 0.039(5) 0.000(4) 0.009(4) 0.000(4) C34 0.043(6) 0.059(7) 0.061(6) -0.021(5) -0.001(5) 0.013(5) C35 0.061(6) 0.049(6) 0.030(5) 0.000(4) 0.000(4) 0.010(5) C36 0.040(5) 0.041(6) 0.037(5) 0.001(4) 0.012(4) 0.013(4) C37 0.067(6) 0.052(6) 0.061(6) 0.014(5) 0.031(5) 0.004(5) C38 0.039(5) 0.027(5) 0.036(4) 0.006(4) 0.001(4) -0.009(4) C39 0.042(5) 0.019(4) 0.050(5) -0.002(4) 0.013(4) -0.006(4) C40 0.041(5) 0.029(5) 0.041(5) 0.008(4) 0.007(4) 0.001(4) C41 0.065(6) 0.047(5) 0.048(5) -0.001(5) 0.019(5) -0.002(4) C42 0.067(6) 0.042(5) 0.051(5) -0.008(4) 0.030(5) -0.004(5) C43 0.048(6) 0.041(5) 0.075(7) -0.012(5) 0.032(5) 0.005(4) C44 0.041(5) 0.034(5) 0.066(6) 0.001(4) 0.004(5) 0.001(4) C45 0.058(6) 0.027(5) 0.049(5) -0.006(4) 0.010(5) -0.002(4) C46 0.052(6) 0.058(6) 0.057(6) -0.003(5) 0.012(4) -0.005(5) B1 0.049(7) 0.074(9) 0.056(7) -0.026(7) 0.009(6) -0.003(6) F1 0.073(4) 0.092(4) 0.066(3) -0.032(3) -0.001(3) -0.001(3) F2 0.062(3) 0.069(4) 0.108(4) -0.026(3) 0.002(3) -0.011(3) F3 0.098(5) 0.127(6) 0.192(6) -0.096(5) -0.062(4) 0.076(4) F4 0.169(7) 0.148(7) 0.096(4) -0.010(4) 0.055(4) -0.059(5) C103 0.062(8) 0.118(12) 0.168(13) 0.091(10) -0.036(8) -0.029(7) C102 0.151(14) 0.102(11) 0.128(11) 0.019(10) 0.064(10) 0.013(11) C104 0.23(2) 0.20(2) 0.189(19) 0.096(17) -0.071(16) -0.054(16) C101 0.184(16) 0.116(13) 0.124(11) 0.029(10) -0.046(11) -0.020(12) O101 0.35(2) 0.218(16) 0.212(14) 0.047(13) 0.019(13) -0.093(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C11 2.033(8) . ? Mo1 C38 2.054(8) . ? Mo1 C20 2.058(8) . ? Mo1 C29 2.075(8) . ? Mo1 C2 2.303(7) . ? Mo1 C1 2.316(7) . ? Mo1 C3 2.332(8) . ? Mo1 C5 2.349(7) . ? Mo1 C4 2.360(7) . ? N1 C11 1.195(8) . ? N1 C12 1.412(9) . ? N2 C20 1.178(8) . ? N2 C21 1.390(9) . ? N3 C29 1.164(8) . ? N3 C30 1.394(9) . ? N4 C38 1.173(8) . ? N4 C39 1.407(8) . ? C1 C5 1.423(9) . ? C1 C2 1.446(9) . ? C1 C6 1.487(9) . ? C2 C3 1.413(10) . ? C2 C7 1.528(10) . ? C3 C4 1.407(10) . ? C3 C8 1.531(10) . ? C4 C5 1.406(10) . ? C4 C9 1.514(10) . ? C5 C10 1.506(9) . ? C12 C13 1.389(11) . ? C12 C18 1.395(11) . ? C13 C15 1.398(12) . ? C13 C14 1.485(11) . ? C15 C16 1.369(13) . ? C16 C17 1.359(13) . ? C17 C18 1.413(12) . ? C18 C19 1.488(11) . ? C21 C22 1.397(10) . ? C21 C27 1.407(10) . ? C22 C24 1.365(11) . ? C22 C23 1.496(11) . ? C24 C25 1.399(12) . ? C25 C26 1.372(12) . ? C26 C27 1.406(11) . ? C27 C28 1.487(10) . ? C30 C31 1.394(9) . ? C30 C36 1.397(9) . ? C31 C33 1.364(9) . ? C31 C32 1.503(9) . ? C33 C34 1.380(10) . ? C34 C35 1.380(10) . ? C35 C36 1.380(9) . ? C36 C37 1.518(10) . ? C39 C45 1.394(10) . ? C39 C40 1.402(9) . ? C40 C42 1.376(9) . ? C40 C41 1.507(9) . ? C42 C43 1.371(10) . ? C43 C44 1.374(10) . ? C44 C45 1.382(10) . ? C45 C46 1.509(9) . ? B1 F3 1.333(11) . ? B1 F2 1.347(11) . ? B1 F1 1.361(10) . ? B1 F4 1.392(12) . ? C103 C102 1.330(13) . ? C103 C104 1.340(17) . ? C102 C101 1.517(15) . ? C104 O101 1.447(16) . ? C101 O101 1.532(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 C11 Mo1 C38 77.7(3) . . ? C11 Mo1 C20 76.5(3) . . ? C38 Mo1 C20 130.2(3) . . ? C11 Mo1 C29 120.2(3) . . ? C38 Mo1 C29 78.5(3) . . ? C20 Mo1 C29 78.8(3) . . ? C11 Mo1 C2 95.1(3) . . ? C38 Mo1 C2 132.3(3) . . ? C20 Mo1 C2 91.9(3) . . ? C29 Mo1 C2 139.4(3) . . ? C11 Mo1 C1 92.0(3) . . ? C38 Mo1 C1 96.1(3) . . ? C20 Mo1 C1 126.6(3) . . ? C29 Mo1 C1 144.5(3) . . ? C2 Mo1 C1 36.5(2) . . ? C11 Mo1 C3 127.3(3) . . ? C38 Mo1 C3 142.3(3) . . ? C20 Mo1 C3 86.3(3) . . ? C29 Mo1 C3 104.0(3) . . ? C2 Mo1 C3 35.5(3) . . ? C1 Mo1 C3 59.8(3) . . ? C11 Mo1 C5 122.1(3) . . ? C38 Mo1 C5 84.8(3) . . ? C20 Mo1 C5 144.7(3) . . ? C29 Mo1 C5 109.2(3) . . ? C2 Mo1 C5 59.1(2) . . ? C1 Mo1 C5 35.5(2) . . ? C3 Mo1 C5 58.4(3) . . ? C11 Mo1 C4 150.4(3) . . ? C38 Mo1 C4 108.9(3) . . ? C20 Mo1 C4 114.6(3) . . ? C29 Mo1 C4 89.3(3) . . ? C2 Mo1 C4 58.6(3) . . ? C1 Mo1 C4 58.9(2) . . ? C3 Mo1 C4 34.9(3) . . ? C5 Mo1 C4 34.7(2) . . ? C11 N1 C12 165.2(8) . . ? C20 N2 C21 175.6(8) . . ? C29 N3 C30 172.7(7) . . ? C38 N4 C39 174.1(7) . . ? C5 C1 C2 106.3(6) . . ? C5 C1 C6 126.5(7) . . ? C2 C1 C6 126.7(7) . . ? C5 C1 Mo1 73.5(4) . . ? C2 C1 Mo1 71.2(4) . . ? C6 C1 Mo1 126.7(5) . . ? C3 C2 C1 108.2(6) . . ? C3 C2 C7 126.6(8) . . ? C1 C2 C7 125.0(8) . . ? C3 C2 Mo1 73.4(4) . . ? C1 C2 Mo1 72.3(4) . . ? C7 C2 Mo1 124.7(5) . . ? C4 C3 C2 108.1(7) . . ? C4 C3 C8 126.6(9) . . ? C2 C3 C8 125.0(8) . . ? C4 C3 Mo1 73.6(4) . . ? C2 C3 Mo1 71.1(4) . . ? C8 C3 Mo1 125.8(5) . . ? C5 C4 C3 108.7(7) . . ? C5 C4 C9 125.5(8) . . ? C3 C4 C9 125.7(8) . . ? C5 C4 Mo1 72.2(4) . . ? C3 C4 Mo1 71.5(4) . . ? C9 C4 Mo1 125.5(5) . . ? C4 C5 C1 108.8(6) . . ? C4 C5 C10 125.8(7) . . ? C1 C5 C10 125.2(7) . . ? C4 C5 Mo1 73.0(4) . . ? C1 C5 Mo1 71.0(4) . . ? C10 C5 Mo1 126.0(5) . . ? N1 C11 Mo1 176.9(6) . . ? C13 C12 C18 125.6(9) . . ? C13 C12 N1 118.4(8) . . ? C18 C12 N1 115.9(9) . . ? C12 C13 C15 115.4(9) . . ? C12 C13 C14 121.8(8) . . ? C15 C13 C14 122.7(10) . . ? C16 C15 C13 120.2(10) . . ? C17 C16 C15 123.7(11) . . ? C16 C17 C18 118.9(10) . . ? C12 C18 C17 116.0(9) . . ? C12 C18 C19 123.9(9) . . ? C17 C18 C19 120.0(9) . . ? N2 C20 Mo1 174.6(6) . . ? N2 C21 C22 118.0(7) . . ? N2 C21 C27 118.1(7) . . ? C22 C21 C27 123.9(7) . . ? C24 C22 C21 116.9(9) . . ? C24 C22 C23 122.3(9) . . ? C21 C22 C23 120.7(7) . . ? C22 C24 C25 121.7(9) . . ? C26 C25 C24 120.3(9) . . ? C25 C26 C27 120.9(9) . . ? C26 C27 C21 116.2(8) . . ? C26 C27 C28 122.5(8) . . ? C21 C27 C28 121.3(7) . . ? N3 C29 Mo1 177.8(7) . . ? C31 C30 N3 118.5(6) . . ? C31 C30 C36 122.5(7) . . ? N3 C30 C36 119.0(7) . . ? C33 C31 C30 118.8(6) . . ? C33 C31 C32 120.3(7) . . ? C30 C31 C32 120.8(7) . . ? C31 C33 C34 119.6(8) . . ? C35 C34 C33 121.5(8) . . ? C34 C35 C36 120.5(7) . . ? C35 C36 C30 117.1(7) . . ? C35 C36 C37 122.0(7) . . ? C30 C36 C37 120.9(7) . . ? N4 C38 Mo1 176.2(6) . . ? C45 C39 C40 123.2(7) . . ? C45 C39 N4 118.2(7) . . ? C40 C39 N4 118.6(7) . . ? C42 C40 C39 116.6(7) . . ? C42 C40 C41 122.7(7) . . ? C39 C40 C41 120.8(7) . . ? C43 C42 C40 121.9(7) . . ? C42 C43 C44 120.1(8) . . ? C43 C44 C45 121.4(7) . . ? C44 C45 C39 116.9(7) . . ? C44 C45 C46 122.0(7) . . ? C39 C45 C46 121.1(7) . . ? F3 B1 F2 113.5(10) . . ? F3 B1 F1 111.4(9) . . ? F2 B1 F1 113.5(8) . . ? F3 B1 F4 107.3(9) . . ? F2 B1 F4 104.1(9) . . ? F1 B1 F4 106.5(9) . . ? C102 C103 C104 110.5(12) . . ? C103 C102 C101 107.6(11) . . ? C103 C104 O101 113.1(14) . . ? C102 C101 O101 104.0(11) . . ? C104 O101 C101 99.1(13) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.395 _refine_diff_density_min -0.369 _refine_diff_density_rms 0.086 #===END data_4 _database_code_CSD 155027 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H28 N2' _chemical_formula_weight 440.56 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.8714(11) _cell_length_b 14.597(2) _cell_length_c 19.138(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.475(16) _cell_angle_gamma 90.00 _cell_volume 2477.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 148 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.181 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.767853 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Siemens CCD area detector' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 13017 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0244 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4376 _reflns_number_gt 3415 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0585P)^2^+0.1085P] 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 4376 _refine_ls_number_parameters 311 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0996 _refine_ls_wR_factor_gt 0.0935 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 N1 N 0.07910(12) 0.72635(7) 0.10803(5) 0.0332(3) Uani 1 1 d . . . N2 N 0.17289(12) 0.66980(7) 0.26826(5) 0.0315(3) Uani 1 1 d . . . C2 C 0.02341(13) 0.76794(9) 0.04516(6) 0.0313(3) Uani 1 1 d . . . C3 C 0.07736(14) 0.85380(9) 0.02549(6) 0.0343(3) Uani 1 1 d . . . C4 C 0.18869(16) 0.90497(10) 0.07147(7) 0.0448(3) Uani 1 1 d . . . H4A H 0.2730 0.8645 0.0844 0.067 Uiso 1 1 calc R . . H4B H 0.1390 0.9255 0.1138 0.067 Uiso 1 1 calc R . . H4C H 0.2266 0.9582 0.0462 0.067 Uiso 1 1 calc R . . C5 C 0.02709(16) 0.88908(10) -0.03842(7) 0.0418(3) Uani 1 1 d . . . H5A H 0.0614 0.9476 -0.0528 0.050 Uiso 1 1 calc R . . C6 C -0.07200(17) 0.84054(11) -0.08153(7) 0.0460(4) Uani 1 1 d . . . H6A H -0.1068 0.8662 -0.1246 0.055 Uiso 1 1 calc R . . C7 C -0.11981(16) 0.75505(10) -0.06161(7) 0.0430(4) Uani 1 1 d . . . H7A H -0.1860 0.7216 -0.0919 0.052 Uiso 1 1 calc R . . C8 C -0.07357(14) 0.71643(9) 0.00177(7) 0.0361(3) Uani 1 1 d . . . C9 C -0.12345(18) 0.62235(10) 0.02383(8) 0.0494(4) Uani 1 1 d . . . H9A H -0.0350 0.5857 0.0375 0.074 Uiso 1 1 calc R . . H9B H -0.1775 0.5925 -0.0152 0.074 Uiso 1 1 calc R . . H9C H -0.1903 0.6277 0.0636 0.074 Uiso 1 1 calc R . . C10 C 0.27270(14) 0.62468(8) 0.22119(6) 0.0309(3) Uani 1 1 d . . . C11 C 0.40882(15) 0.66690(9) 0.20551(7) 0.0366(3) Uani 1 1 d . . . C12 C 0.44752(18) 0.75965(11) 0.23434(8) 0.0516(4) Uani 1 1 d . . . H12A H 0.4430 0.7582 0.2854 0.077 Uiso 1 1 calc R . . H12B H 0.3753 0.8049 0.2158 0.077 Uiso 1 1 calc R . . H12C H 0.5495 0.7765 0.2207 0.077 Uiso 1 1 calc R . . C13 C 0.50431(16) 0.62177(11) 0.16011(7) 0.0488(4) Uani 1 1 d . . . H13A H 0.5970 0.6496 0.1483 0.059 Uiso 1 1 calc R . . C14 C 0.46705(19) 0.53779(12) 0.13212(8) 0.0539(4) Uani 1 1 d . . . H14A H 0.5333 0.5082 0.1011 0.065 Uiso 1 1 calc R . . C15 C 0.33312(19) 0.49676(10) 0.14930(8) 0.0504(4) Uani 1 1 d . . . H15A H 0.3087 0.4383 0.1303 0.060 Uiso 1 1 calc R . . C16 C 0.23291(16) 0.53898(9) 0.19379(7) 0.0389(3) Uani 1 1 d . . . C17 C 0.08333(19) 0.49690(11) 0.20958(9) 0.0586(4) Uani 1 1 d . . . H17A H 0.0734 0.4918 0.2603 0.088 Uiso 1 1 calc R . . H17B H 0.0767 0.4358 0.1885 0.088 Uiso 1 1 calc R . . H17C H 0.0022 0.5356 0.1903 0.088 Uiso 1 1 calc R . . C18 C 0.07397(13) 0.72126(8) 0.23990(6) 0.0288(3) Uani 1 1 d . . . C19 C -0.04443(13) 0.78450(8) 0.26546(6) 0.0287(3) Uani 1 1 d . . . C20 C -0.07975(13) 0.81563(8) 0.19881(6) 0.0294(3) Uani 1 1 d . . . C21 C 0.03110(14) 0.75155(8) 0.16671(6) 0.0293(3) Uani 1 1 d . . . C22 C -0.17923(13) 0.88691(8) 0.16938(6) 0.0310(3) Uani 1 1 d . . . C23 C -0.17908(16) 0.97456(9) 0.19877(7) 0.0397(3) Uani 1 1 d . . . H23A H -0.1145 0.9879 0.2378 0.048 Uiso 1 1 calc R . . C24 C -0.27280(18) 1.04190(10) 0.17111(8) 0.0517(4) Uani 1 1 d . . . H24A H -0.2714 1.1016 0.1909 0.062 Uiso 1 1 calc R . . C25 C -0.36839(18) 1.02283(11) 0.11479(8) 0.0534(4) Uani 1 1 d . . . H25A H -0.4344 1.0688 0.0968 0.064 Uiso 1 1 calc R . . C26 C -0.36781(16) 0.93692(11) 0.08483(8) 0.0460(4) Uani 1 1 d . . . H26A H -0.4329 0.9239 0.0459 0.055 Uiso 1 1 calc R . . C27 C -0.27265(14) 0.86958(9) 0.11132(7) 0.0359(3) Uani 1 1 d . . . H27A H -0.2710 0.8110 0.0897 0.043 Uiso 1 1 calc R . . C28 C -0.09697(13) 0.80207(8) 0.33585(6) 0.0293(3) Uani 1 1 d . . . C29 C -0.01497(15) 0.76618(9) 0.39269(7) 0.0358(3) Uani 1 1 d . . . H29A H 0.0710 0.7290 0.3851 0.043 Uiso 1 1 calc R . . C30 C -0.05875(17) 0.78464(10) 0.46033(7) 0.0437(4) Uani 1 1 d . . . H30A H -0.0010 0.7613 0.4988 0.052 Uiso 1 1 calc R . . C31 C -0.18549(16) 0.83668(10) 0.47216(7) 0.0433(4) Uani 1 1 d . . . H31A H -0.2146 0.8494 0.5186 0.052 Uiso 1 1 calc R . . C32 C -0.26990(15) 0.87017(9) 0.41590(7) 0.0391(3) Uani 1 1 d . . . H32A H -0.3586 0.9047 0.4239 0.047 Uiso 1 1 calc R . . C33 C -0.22613(14) 0.85382(9) 0.34837(7) 0.0345(3) Uani 1 1 d . . . H33A H -0.2841 0.8779 0.3102 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 N1 0.0364(6) 0.0362(6) 0.0271(6) 0.0003(5) 0.0039(5) 0.0058(5) N2 0.0352(6) 0.0296(6) 0.0299(6) 0.0006(4) 0.0024(5) 0.0021(5) C2 0.0311(6) 0.0385(7) 0.0247(6) -0.0008(5) 0.0057(5) 0.0102(6) C3 0.0330(6) 0.0399(7) 0.0300(7) 0.0005(6) 0.0035(5) 0.0051(6) C4 0.0428(8) 0.0483(9) 0.0431(8) 0.0061(7) -0.0038(6) -0.0032(7) C5 0.0478(8) 0.0439(8) 0.0338(7) 0.0060(6) 0.0040(6) 0.0057(7) C6 0.0556(9) 0.0522(9) 0.0299(7) 0.0008(6) -0.0051(7) 0.0132(7) C7 0.0413(8) 0.0518(9) 0.0358(8) -0.0094(6) -0.0035(6) 0.0071(7) C8 0.0354(7) 0.0405(8) 0.0327(7) -0.0062(6) 0.0063(6) 0.0066(6) C9 0.0553(9) 0.0484(9) 0.0448(9) -0.0067(7) 0.0064(7) -0.0044(7) C10 0.0364(7) 0.0304(7) 0.0260(6) 0.0026(5) -0.0003(5) 0.0079(5) C11 0.0377(7) 0.0427(8) 0.0295(7) 0.0042(6) 0.0009(6) 0.0032(6) C12 0.0528(9) 0.0554(10) 0.0468(9) -0.0012(7) 0.0067(7) -0.0168(8) C13 0.0412(8) 0.0677(11) 0.0377(8) 0.0080(7) 0.0068(6) 0.0126(8) C14 0.0609(10) 0.0626(11) 0.0384(8) -0.0023(7) 0.0049(7) 0.0337(9) C15 0.0689(11) 0.0374(8) 0.0443(9) -0.0078(7) -0.0080(8) 0.0209(8) C16 0.0473(8) 0.0301(7) 0.0390(8) 0.0010(6) -0.0050(6) 0.0060(6) C17 0.0646(10) 0.0379(8) 0.0730(11) -0.0046(8) -0.0017(9) -0.0095(8) C18 0.0324(6) 0.0272(6) 0.0271(6) 0.0013(5) 0.0044(5) -0.0013(5) C19 0.0291(6) 0.0277(6) 0.0296(7) -0.0012(5) 0.0034(5) -0.0022(5) C20 0.0301(6) 0.0299(7) 0.0284(7) -0.0015(5) 0.0046(5) -0.0003(5) C21 0.0313(6) 0.0289(7) 0.0279(7) -0.0003(5) 0.0031(5) 0.0019(5) C22 0.0309(6) 0.0338(7) 0.0286(7) 0.0028(5) 0.0084(5) 0.0042(5) C23 0.0466(8) 0.0371(8) 0.0355(8) 0.0000(6) 0.0057(6) 0.0053(6) C24 0.0677(10) 0.0378(8) 0.0501(9) 0.0030(7) 0.0133(8) 0.0156(8) C25 0.0546(9) 0.0539(10) 0.0521(9) 0.0155(8) 0.0086(8) 0.0235(8) C26 0.0381(7) 0.0585(10) 0.0414(8) 0.0090(7) 0.0019(6) 0.0100(7) C27 0.0326(7) 0.0403(8) 0.0349(7) 0.0011(6) 0.0052(6) 0.0033(6) C28 0.0320(6) 0.0279(6) 0.0281(7) -0.0009(5) 0.0057(5) -0.0064(5) C29 0.0381(7) 0.0366(7) 0.0329(7) 0.0018(6) 0.0041(6) -0.0039(6) C30 0.0497(8) 0.0533(9) 0.0281(7) 0.0036(6) 0.0021(6) -0.0092(7) C31 0.0501(8) 0.0498(9) 0.0306(7) -0.0063(6) 0.0147(6) -0.0171(7) C32 0.0379(7) 0.0406(8) 0.0395(8) -0.0067(6) 0.0148(6) -0.0073(6) C33 0.0339(7) 0.0365(7) 0.0334(7) -0.0013(6) 0.0063(6) -0.0040(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 N1 C21 1.2659(16) . ? N1 C2 1.4248(15) . ? N2 C18 1.2666(16) . ? N2 C10 1.4389(15) . ? C2 C3 1.3967(18) . ? C2 C8 1.3994(18) . ? C3 C5 1.3900(18) . ? C3 C4 1.5043(19) . ? C5 C6 1.385(2) . ? C6 C7 1.375(2) . ? C7 C8 1.3899(19) . ? C8 C9 1.506(2) . ? C10 C11 1.3952(18) . ? C10 C16 1.3982(18) . ? C11 C13 1.3944(19) . ? C11 C12 1.498(2) . ? C13 C14 1.375(2) . ? C14 C15 1.378(2) . ? C15 C16 1.391(2) . ? C16 C17 1.500(2) . ? C18 C19 1.4905(17) . ? C18 C21 1.5081(17) . ? C19 C20 1.3826(17) . ? C19 C28 1.4594(17) . ? C20 C22 1.4672(17) . ? C20 C21 1.5002(17) . ? C22 C27 1.3922(18) . ? C22 C23 1.3977(18) . ? C23 C24 1.384(2) . ? C24 C25 1.383(2) . ? C25 C26 1.379(2) . ? C26 C27 1.3834(19) . ? C28 C29 1.3951(18) . ? C28 C33 1.3982(18) . ? C29 C30 1.3875(18) . ? C30 C31 1.380(2) . ? C31 C32 1.385(2) . ? C32 C33 1.3798(18) . ? 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 C21 N1 C2 120.54(11) . . ? C18 N2 C10 115.71(10) . . ? C3 C2 C8 122.14(12) . . ? C3 C2 N1 119.75(11) . . ? C8 C2 N1 117.82(12) . . ? C5 C3 C2 117.72(12) . . ? C5 C3 C4 121.45(12) . . ? C2 C3 C4 120.82(11) . . ? C6 C5 C3 121.26(14) . . ? C7 C6 C5 119.65(13) . . ? C6 C7 C8 121.60(13) . . ? C7 C8 C2 117.57(13) . . ? C7 C8 C9 122.15(13) . . ? C2 C8 C9 120.27(12) . . ? C11 C10 C16 121.74(12) . . ? C11 C10 N2 118.84(11) . . ? C16 C10 N2 119.40(11) . . ? C13 C11 C10 117.93(13) . . ? C13 C11 C12 121.28(13) . . ? C10 C11 C12 120.75(12) . . ? C14 C13 C11 121.35(15) . . ? C13 C14 C15 119.66(14) . . ? C14 C15 C16 121.48(14) . . ? C15 C16 C10 117.84(14) . . ? C15 C16 C17 121.64(13) . . ? C10 C16 C17 120.45(13) . . ? N2 C18 C19 135.47(11) . . ? N2 C18 C21 136.66(11) . . ? C19 C18 C21 87.72(9) . . ? C20 C19 C28 136.36(12) . . ? C20 C19 C18 92.61(10) . . ? C28 C19 C18 131.02(11) . . ? C19 C20 C22 134.99(11) . . ? C19 C20 C21 92.14(10) . . ? C22 C20 C21 132.78(11) . . ? N1 C21 C20 141.58(12) . . ? N1 C21 C18 131.01(11) . . ? C20 C21 C18 87.42(9) . . ? C27 C22 C23 118.80(12) . . ? C27 C22 C20 121.16(12) . . ? C23 C22 C20 120.03(12) . . ? C24 C23 C22 120.14(14) . . ? C25 C24 C23 120.37(14) . . ? C26 C25 C24 119.90(14) . . ? C25 C26 C27 120.17(14) . . ? C26 C27 C22 120.57(13) . . ? C29 C28 C33 118.84(11) . . ? C29 C28 C19 118.76(11) . . ? C33 C28 C19 122.39(11) . . ? C30 C29 C28 120.11(13) . . ? C31 C30 C29 120.57(13) . . ? C30 C31 C32 119.56(12) . . ? C33 C32 C31 120.50(13) . . ? C32 C33 C28 120.37(13) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.127 _refine_diff_density_min -0.190 _refine_diff_density_rms 0.035 #===END data_5 _database_code_CSD 155028 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H44 B Cl2 F4 Mo N3' _chemical_formula_weight 796.41 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' 'B' 'B' 0.0013 0.0007 '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' 'F' 'F' 0.0171 0.0103 '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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.989(5) _cell_length_b 15.553(5) _cell_length_c 16.489(5) _cell_angle_alpha 90.00 _cell_angle_beta 113.917(14) _cell_angle_gamma 90.00 _cell_volume 3748(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 76 _cell_measurement_theta_min 5 _cell_measurement_theta_max 50 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1640 _exptl_absorpt_coefficient_mu 0.543 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.835985 _exptl_absorpt_correction_T_max 0.987650 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Siemens CCD Area Diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 19503 _diffrn_reflns_av_R_equivalents 0.0952 _diffrn_reflns_av_sigmaI/netI 0.1169 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _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 1.88 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6568 _reflns_number_gt 3923 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0492P)^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 6568 _refine_ls_number_parameters 453 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1248 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1279 _refine_ls_wR_factor_gt 0.1025 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 0.74196(3) -0.12953(3) 0.24813(3) 0.02202(15) Uani 1 1 d . . . N1 N 0.5609(3) -0.0890(3) 0.2849(3) 0.0335(12) Uani 1 1 d . . . N2 N 0.8502(3) -0.1072(3) 0.1173(3) 0.0278(11) Uani 1 1 d . . . C1 C 0.6275(4) -0.1029(4) 0.2753(4) 0.0288(14) Uani 1 1 d . . . C2 C 0.8212(4) -0.1166(4) 0.1702(4) 0.0279(13) Uani 1 1 d . . . N3 N 0.7340(3) 0.0098(3) 0.2260(3) 0.0260(12) Uani 1 1 d . . . C3 C 0.7878(3) -0.0100(4) 0.3043(4) 0.0256(14) Uani 1 1 d . . . C4 C 0.8418(4) 0.0430(3) 0.3833(4) 0.0315(15) Uani 1 1 d . . . H5A H 0.9071 0.0401 0.3932 0.038 Uiso 1 1 calc R . . H5B H 0.8361 0.0175 0.4358 0.038 Uiso 1 1 calc R . . C11 C 0.7853(4) -0.2699(4) 0.2557(4) 0.0282(14) Uani 1 1 d . . . C12 C 0.8647(4) -0.2261(3) 0.3136(4) 0.0277(14) Uani 1 1 d . . . C13 C 0.8476(4) -0.1899(4) 0.3848(4) 0.0261(14) Uani 1 1 d . . . C14 C 0.7577(4) -0.2143(3) 0.3728(3) 0.0241(13) Uani 1 1 d . . . C15 C 0.7173(4) -0.2630(3) 0.2908(4) 0.0253(13) Uani 1 1 d . . . C16 C 0.7756(4) -0.3237(4) 0.1770(4) 0.0405(16) Uani 1 1 d . . . H16A H 0.7875 -0.3841 0.1951 0.061 Uiso 1 1 calc R . . H16B H 0.8196 -0.3043 0.1534 0.061 Uiso 1 1 calc R . . H16C H 0.7134 -0.3180 0.1312 0.061 Uiso 1 1 calc R . . C17 C 0.9570(4) -0.2254(4) 0.3108(4) 0.0381(16) Uani 1 1 d . . . H17A H 0.9978 -0.2647 0.3560 0.057 Uiso 1 1 calc R . . H17B H 0.9823 -0.1671 0.3225 0.057 Uiso 1 1 calc R . . H17C H 0.9514 -0.2440 0.2520 0.057 Uiso 1 1 calc R . . C18 C 0.9182(4) -0.1489(4) 0.4658(4) 0.0351(15) Uani 1 1 d . . . H18A H 0.9554 -0.1936 0.5061 0.053 Uiso 1 1 calc R . . H18B H 0.8878 -0.1145 0.4957 0.053 Uiso 1 1 calc R . . H18C H 0.9575 -0.1116 0.4484 0.053 Uiso 1 1 calc R . . C19 C 0.7194(4) -0.2029(4) 0.4410(4) 0.0347(15) Uani 1 1 d . . . H19A H 0.7445 -0.2472 0.4869 0.052 Uiso 1 1 calc R . . H19B H 0.6526 -0.2083 0.4128 0.052 Uiso 1 1 calc R . . H19C H 0.7359 -0.1459 0.4681 0.052 Uiso 1 1 calc R . . C20 C 0.6278(4) -0.3100(4) 0.2587(4) 0.0377(16) Uani 1 1 d . . . H20A H 0.6391 -0.3716 0.2706 0.057 Uiso 1 1 calc R . . H20B H 0.5945 -0.3008 0.1947 0.057 Uiso 1 1 calc R . . H20C H 0.5912 -0.2883 0.2897 0.057 Uiso 1 1 calc R . . C21 C 0.4867(4) -0.0706(4) 0.3074(4) 0.0395(17) Uani 1 1 d . . . C22 C 0.4082(4) -0.1207(5) 0.2706(5) 0.055(2) Uani 1 1 d . . . C23 C 0.3384(5) -0.1027(6) 0.2980(6) 0.072(3) Uani 1 1 d . . . H23A H 0.2836 -0.1355 0.2754 0.086 Uiso 1 1 calc R . . C24 C 0.3482(5) -0.0381(7) 0.3573(6) 0.072(3) Uani 1 1 d . . . H24A H 0.3008 -0.0283 0.3769 0.086 Uiso 1 1 calc R . . C25 C 0.4241(5) 0.0126(5) 0.3890(5) 0.060(2) Uani 1 1 d . . . H25 H 0.4271 0.0592 0.4273 0.072 Uiso 1 1 calc R . . C26 C 0.4974(4) -0.0028(4) 0.3659(4) 0.0436(18) Uani 1 1 d . . . C27 C 0.3989(5) -0.1919(5) 0.2044(6) 0.083(3) Uani 1 1 d . . . H27A H 0.3342 -0.1996 0.1652 0.124 Uiso 1 1 calc R . . H27B H 0.4233 -0.2456 0.2364 0.124 Uiso 1 1 calc R . . H27C H 0.4333 -0.1763 0.1691 0.124 Uiso 1 1 calc R . . C28 C 0.5821(4) 0.0510(4) 0.4006(5) 0.0532(19) Uani 1 1 d . . . H28A H 0.5924 0.0757 0.3508 0.080 Uiso 1 1 calc R . . H28B H 0.6345 0.0152 0.4364 0.080 Uiso 1 1 calc R . . H28C H 0.5748 0.0974 0.4374 0.080 Uiso 1 1 calc R . . C31 C 0.7185(4) 0.0831(3) 0.1694(4) 0.0259(13) Uani 1 1 d . . . C32 C 0.7934(4) 0.1243(4) 0.1626(4) 0.0317(14) Uani 1 1 d . . . C33 C 0.7752(4) 0.1943(4) 0.1064(4) 0.0431(17) Uani 1 1 d . . . H33A H 0.8247 0.2241 0.1012 0.052 Uiso 1 1 calc R . . C34 C 0.6877(5) 0.2217(4) 0.0581(5) 0.0511(19) Uani 1 1 d . . . H34A H 0.6771 0.2704 0.0205 0.061 Uiso 1 1 calc R . . C35 C 0.6150(4) 0.1794(4) 0.0638(4) 0.0429(17) Uani 1 1 d . . . H35A H 0.5546 0.1985 0.0290 0.051 Uiso 1 1 calc R . . C36 C 0.6285(4) 0.1080(4) 0.1205(4) 0.0329(15) Uani 1 1 d . . . C37 C 0.5485(4) 0.0644(4) 0.1266(4) 0.0451(18) Uani 1 1 d . . . H37A H 0.5514 0.0709 0.1868 0.068 Uiso 1 1 calc R . . H37B H 0.5496 0.0031 0.1130 0.068 Uiso 1 1 calc R . . H37C H 0.4919 0.0904 0.0840 0.068 Uiso 1 1 calc R . . C38 C 0.8918(4) 0.0968(4) 0.2139(4) 0.0389(16) Uani 1 1 d . . . H38A H 0.9265 0.1063 0.1775 0.058 Uiso 1 1 calc R . . H38B H 0.8936 0.0356 0.2287 0.058 Uiso 1 1 calc R . . H38C H 0.9189 0.1306 0.2685 0.058 Uiso 1 1 calc R . . C41 C 0.8739(4) -0.0938(4) 0.0444(4) 0.0279(14) Uani 1 1 d . . . C42 C 0.9601(4) -0.1203(4) 0.0514(4) 0.0279(13) Uani 1 1 d . . . C43 C 0.9798(4) -0.1080(4) -0.0228(4) 0.0370(16) Uani 1 1 d . . . H43A H 1.0372 -0.1260 -0.0211 0.044 Uiso 1 1 calc R . . C44 C 0.9170(4) -0.0699(4) -0.0988(4) 0.0374(16) Uani 1 1 d . . . H44A H 0.9318 -0.0623 -0.1486 0.045 Uiso 1 1 calc R . . C45 C 0.8337(4) -0.0431(4) -0.1033(4) 0.0375(16) Uani 1 1 d . . . H45A H 0.7922 -0.0161 -0.1559 0.045 Uiso 1 1 calc R . . C46 C 0.8085(4) -0.0547(4) -0.0318(4) 0.0325(15) Uani 1 1 d . . . C47 C 0.7176(4) -0.0262(4) -0.0361(4) 0.0430(17) Uani 1 1 d . . . H47A H 0.6864 -0.0749 -0.0228 0.065 Uiso 1 1 calc R . . H47B H 0.6804 -0.0045 -0.0957 0.065 Uiso 1 1 calc R . . H47C H 0.7264 0.0196 0.0074 0.065 Uiso 1 1 calc R . . C48 C 1.0288(4) -0.1603(4) 0.1351(4) 0.0412(17) Uani 1 1 d . . . H48A H 1.0066 -0.2167 0.1441 0.062 Uiso 1 1 calc R . . H48B H 1.0372 -0.1230 0.1857 0.062 Uiso 1 1 calc R . . H48C H 1.0874 -0.1671 0.1299 0.062 Uiso 1 1 calc R . . B1 B 0.8800(5) 0.4733(5) 0.1241(5) 0.0393(19) Uani 1 1 d . . . F1 F 0.8085(2) 0.5205(2) 0.0628(2) 0.0380(9) Uani 1 1 d . . . F2 F 0.9563(2) 0.4804(2) 0.1069(2) 0.0550(11) Uani 1 1 d . . . F3 F 0.8971(3) 0.4975(3) 0.2072(2) 0.0940(18) Uani 1 1 d . . . F4 F 0.8538(3) 0.3877(3) 0.1153(4) 0.1032(18) Uani 1 1 d . . . Cl1 Cl 0.62411(10) -0.15796(10) 0.09844(10) 0.0369(4) Uani 1 1 d . . . Cl2 Cl 0.80827(12) 0.15323(10) 0.37502(12) 0.0507(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0253(3) 0.0260(3) 0.0187(3) 0.0017(3) 0.0129(2) -0.0001(2) N1 0.030(3) 0.042(3) 0.034(3) 0.010(2) 0.020(3) 0.003(2) N2 0.034(3) 0.033(3) 0.025(3) 0.003(2) 0.020(2) 0.002(2) C1 0.025(3) 0.031(4) 0.027(3) 0.002(3) 0.007(3) -0.005(3) C2 0.027(3) 0.030(4) 0.025(3) -0.002(3) 0.008(3) 0.003(3) N3 0.023(3) 0.028(3) 0.028(3) 0.002(2) 0.012(2) 0.001(2) C3 0.021(3) 0.033(4) 0.027(4) 0.001(3) 0.014(3) 0.004(3) C4 0.038(4) 0.026(4) 0.030(4) 0.003(3) 0.013(3) 0.001(3) C11 0.045(4) 0.024(3) 0.025(3) 0.002(3) 0.024(3) 0.003(3) C12 0.031(3) 0.026(3) 0.030(4) 0.004(3) 0.016(3) 0.004(3) C13 0.031(3) 0.026(3) 0.020(3) 0.002(3) 0.009(3) 0.008(2) C14 0.034(3) 0.023(3) 0.019(3) 0.002(2) 0.015(3) 0.002(3) C15 0.034(3) 0.022(3) 0.021(3) 0.004(3) 0.012(3) -0.001(3) C16 0.063(4) 0.033(4) 0.032(4) -0.001(3) 0.026(4) 0.005(3) C17 0.038(4) 0.051(4) 0.034(4) 0.018(3) 0.024(3) 0.009(3) C18 0.040(4) 0.032(4) 0.029(4) 0.002(3) 0.009(3) 0.005(3) C19 0.042(4) 0.046(4) 0.026(3) 0.000(3) 0.024(3) -0.001(3) C20 0.049(4) 0.034(4) 0.033(4) 0.003(3) 0.020(3) -0.008(3) C21 0.030(4) 0.058(5) 0.042(4) 0.021(4) 0.027(3) 0.010(3) C22 0.031(4) 0.066(5) 0.074(5) 0.026(5) 0.027(4) 0.002(4) C23 0.036(4) 0.102(8) 0.083(7) 0.051(6) 0.031(5) 0.016(4) C24 0.053(5) 0.115(8) 0.074(7) 0.053(6) 0.054(5) 0.041(5) C25 0.070(6) 0.078(6) 0.052(5) 0.035(4) 0.045(5) 0.042(5) C26 0.045(4) 0.059(5) 0.035(4) 0.023(3) 0.024(4) 0.020(4) C27 0.056(5) 0.068(6) 0.120(8) -0.008(6) 0.031(6) -0.022(4) C28 0.066(5) 0.051(5) 0.050(5) 0.000(4) 0.030(4) 0.010(4) C31 0.031(3) 0.023(3) 0.023(3) 0.005(3) 0.010(3) 0.006(3) C32 0.038(3) 0.025(3) 0.036(4) 0.001(3) 0.020(3) -0.005(3) C33 0.047(4) 0.039(4) 0.046(4) 0.016(3) 0.022(4) -0.002(3) C34 0.055(5) 0.039(4) 0.050(5) 0.019(3) 0.012(4) 0.002(4) C35 0.037(4) 0.044(4) 0.039(4) 0.010(3) 0.006(3) 0.005(3) C36 0.031(3) 0.031(4) 0.034(4) 0.003(3) 0.010(3) -0.003(3) C37 0.028(3) 0.051(4) 0.051(4) 0.018(4) 0.011(3) 0.008(3) C38 0.030(3) 0.043(4) 0.047(4) 0.012(3) 0.019(3) -0.002(3) C41 0.040(4) 0.027(3) 0.026(3) -0.006(3) 0.023(3) -0.005(3) C42 0.040(3) 0.026(3) 0.024(3) -0.005(3) 0.020(3) -0.004(3) C43 0.051(4) 0.037(4) 0.036(4) -0.009(3) 0.030(4) -0.006(3) C44 0.062(4) 0.037(4) 0.027(4) -0.006(3) 0.032(4) -0.015(3) C45 0.052(4) 0.042(4) 0.020(3) 0.001(3) 0.016(3) -0.005(3) C46 0.043(4) 0.030(4) 0.030(4) -0.008(3) 0.021(3) -0.009(3) C47 0.046(4) 0.053(5) 0.030(4) 0.011(3) 0.016(3) 0.008(3) C48 0.045(4) 0.051(4) 0.035(4) -0.001(3) 0.024(3) 0.004(3) B1 0.037(4) 0.052(5) 0.030(5) 0.002(4) 0.015(4) 0.005(4) F1 0.0360(19) 0.053(2) 0.032(2) 0.0094(17) 0.0209(17) 0.0110(16) F2 0.032(2) 0.079(3) 0.061(3) 0.011(2) 0.026(2) 0.0044(18) F3 0.103(4) 0.151(5) 0.025(2) 0.007(3) 0.022(3) 0.071(3) F4 0.079(3) 0.052(3) 0.173(6) 0.022(3) 0.046(4) -0.003(2) Cl1 0.0353(9) 0.0477(10) 0.0220(8) -0.0011(7) 0.0057(7) -0.0058(7) Cl2 0.0657(12) 0.0355(10) 0.0469(11) -0.0064(8) 0.0188(10) 0.0038(8) _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 C3 2.074(6) . ? Mo1 C1 2.094(6) . ? Mo1 C2 2.148(6) . ? Mo1 N3 2.192(4) . ? Mo1 C15 2.276(5) . ? Mo1 C11 2.279(6) . ? Mo1 C12 2.357(5) . ? Mo1 C14 2.369(5) . ? Mo1 C13 2.393(5) . ? Mo1 Cl1 2.4631(16) . ? N1 C1 1.158(6) . ? N1 C21 1.409(7) . ? N2 C2 1.152(6) . ? N2 C41 1.415(7) . ? N3 C3 1.265(6) . ? N3 C31 1.431(6) . ? C3 C4 1.486(7) . ? C4 Cl2 1.786(6) . ? C11 C12 1.416(7) . ? C11 C15 1.428(7) . ? C11 C16 1.498(7) . ? C12 C13 1.424(7) . ? C12 C17 1.495(7) . ? C13 C14 1.421(7) . ? C13 C18 1.498(7) . ? C14 C15 1.453(7) . ? C14 C19 1.492(7) . ? C15 C20 1.500(7) . ? C21 C22 1.390(9) . ? C21 C26 1.392(9) . ? C22 C23 1.392(9) . ? C22 C27 1.519(10) . ? C23 C24 1.365(11) . ? C24 C25 1.361(11) . ? C25 C26 1.392(8) . ? C26 C28 1.495(9) . ? C31 C36 1.388(7) . ? C31 C32 1.403(7) . ? C32 C33 1.381(8) . ? C32 C38 1.515(7) . ? C33 C34 1.368(8) . ? C34 C35 1.370(8) . ? C35 C36 1.411(8) . ? C36 C37 1.486(7) . ? C41 C42 1.397(7) . ? C41 C46 1.406(8) . ? C42 C43 1.396(7) . ? C42 C48 1.505(8) . ? C43 C44 1.381(8) . ? C44 C45 1.367(8) . ? C45 C46 1.405(8) . ? C46 C47 1.493(7) . ? B1 F3 1.337(8) . ? B1 F2 1.365(8) . ? B1 F4 1.386(8) . ? B1 F1 1.389(8) . ? 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 Mo1 C1 84.7(2) . . ? C3 Mo1 C2 89.7(2) . . ? C1 Mo1 C2 152.6(2) . . ? C3 Mo1 N3 34.36(18) . . ? C1 Mo1 N3 80.98(18) . . ? C2 Mo1 N3 79.42(18) . . ? C3 Mo1 C15 138.9(2) . . ? C1 Mo1 C15 80.7(2) . . ? C2 Mo1 C15 119.2(2) . . ? N3 Mo1 C15 161.21(18) . . ? C3 Mo1 C11 142.2(2) . . ? C1 Mo1 C11 116.8(2) . . ? C2 Mo1 C11 83.3(2) . . ? N3 Mo1 C11 162.16(17) . . ? C15 Mo1 C11 36.55(18) . . ? C3 Mo1 C12 106.8(2) . . ? C1 Mo1 C12 131.7(2) . . ? C2 Mo1 C12 75.56(19) . . ? N3 Mo1 C12 133.43(17) . . ? C15 Mo1 C12 59.59(19) . . ? C11 Mo1 C12 35.51(18) . . ? C3 Mo1 C14 102.5(2) . . ? C1 Mo1 C14 73.7(2) . . ? C2 Mo1 C14 133.69(19) . . ? N3 Mo1 C14 132.29(17) . . ? C15 Mo1 C14 36.40(18) . . ? C11 Mo1 C14 59.77(18) . . ? C12 Mo1 C14 58.13(18) . . ? C3 Mo1 C13 86.8(2) . . ? C1 Mo1 C13 102.7(2) . . ? C2 Mo1 C13 103.8(2) . . ? N3 Mo1 C13 121.06(18) . . ? C15 Mo1 C13 59.70(19) . . ? C11 Mo1 C13 59.29(19) . . ? C12 Mo1 C13 34.89(18) . . ? C14 Mo1 C13 34.71(17) . . ? C3 Mo1 Cl1 126.64(16) . . ? C1 Mo1 Cl1 82.53(16) . . ? C2 Mo1 Cl1 79.32(15) . . ? N3 Mo1 Cl1 92.38(12) . . ? C15 Mo1 Cl1 89.32(14) . . ? C11 Mo1 Cl1 88.57(15) . . ? C12 Mo1 Cl1 120.09(15) . . ? C14 Mo1 Cl1 122.61(13) . . ? C13 Mo1 Cl1 146.53(14) . . ? C1 N1 C21 173.2(6) . . ? C2 N2 C41 172.5(5) . . ? N1 C1 Mo1 175.8(5) . . ? N2 C2 Mo1 168.9(5) . . ? C3 N3 C31 136.5(5) . . ? C3 N3 Mo1 67.7(3) . . ? C31 N3 Mo1 151.6(4) . . ? N3 C3 C4 132.3(5) . . ? N3 C3 Mo1 77.9(3) . . ? C4 C3 Mo1 149.6(4) . . ? C3 C4 Cl2 114.6(4) . . ? C12 C11 C15 108.2(5) . . ? C12 C11 C16 127.1(5) . . ? C15 C11 C16 124.4(5) . . ? C12 C11 Mo1 75.2(3) . . ? C15 C11 Mo1 71.6(3) . . ? C16 C11 Mo1 124.4(4) . . ? C11 C12 C13 109.1(5) . . ? C11 C12 C17 127.5(5) . . ? C13 C12 C17 123.0(5) . . ? C11 C12 Mo1 69.3(3) . . ? C13 C12 Mo1 73.9(3) . . ? C17 C12 Mo1 129.1(4) . . ? C14 C13 C12 107.6(5) . . ? C14 C13 C18 126.3(5) . . ? C12 C13 C18 125.1(5) . . ? C14 C13 Mo1 71.7(3) . . ? C12 C13 Mo1 71.2(3) . . ? C18 C13 Mo1 131.4(4) . . ? C13 C14 C15 108.1(5) . . ? C13 C14 C19 124.4(5) . . ? C15 C14 C19 126.8(5) . . ? C13 C14 Mo1 73.6(3) . . ? C15 C14 Mo1 68.3(3) . . ? C19 C14 Mo1 131.0(4) . . ? C11 C15 C14 107.0(5) . . ? C11 C15 C20 126.5(5) . . ? C14 C15 C20 125.7(5) . . ? C11 C15 Mo1 71.8(3) . . ? C14 C15 Mo1 75.3(3) . . ? C20 C15 Mo1 126.6(4) . . ? C22 C21 C26 124.2(6) . . ? C22 C21 N1 118.7(6) . . ? C26 C21 N1 117.1(6) . . ? C21 C22 C23 116.5(8) . . ? C21 C22 C27 122.0(6) . . ? C23 C22 C27 121.5(7) . . ? C24 C23 C22 120.3(8) . . ? C25 C24 C23 121.9(7) . . ? C24 C25 C26 120.8(8) . . ? C25 C26 C21 116.1(7) . . ? C25 C26 C28 122.1(7) . . ? C21 C26 C28 121.8(6) . . ? C36 C31 C32 123.0(5) . . ? C36 C31 N3 117.7(5) . . ? C32 C31 N3 119.2(5) . . ? C33 C32 C31 117.3(5) . . ? C33 C32 C38 119.1(5) . . ? C31 C32 C38 123.6(5) . . ? C34 C33 C32 121.6(6) . . ? C33 C34 C35 120.4(6) . . ? C34 C35 C36 121.1(6) . . ? C31 C36 C35 116.6(5) . . ? C31 C36 C37 123.5(5) . . ? C35 C36 C37 119.9(5) . . ? C42 C41 C46 123.6(5) . . ? C42 C41 N2 118.7(5) . . ? C46 C41 N2 117.7(5) . . ? C43 C42 C41 116.8(5) . . ? C43 C42 C48 121.3(5) . . ? C41 C42 C48 121.8(5) . . ? C44 C43 C42 121.0(6) . . ? C45 C44 C43 120.9(6) . . ? C44 C45 C46 121.3(6) . . ? C45 C46 C41 116.3(5) . . ? C45 C46 C47 121.8(6) . . ? C41 C46 C47 121.9(5) . . ? F3 B1 F2 111.2(6) . . ? F3 B1 F4 107.8(6) . . ? F2 B1 F4 108.3(6) . . ? F3 B1 F1 111.3(6) . . ? F2 B1 F1 110.3(6) . . ? F4 B1 F1 107.9(6) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.696 _refine_diff_density_min -0.757 _refine_diff_density_rms 0.099 #===END data_6 _database_code_CSD 155029 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C61 H64 B2 Cl2 F8 Mo N4' _chemical_formula_weight 1193.62 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' 'B' 'B' 0.0013 0.0007 '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' 'F' 'F' 0.0171 0.0103 '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 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 16.676(2) _cell_length_b 16.339(2) _cell_length_c 21.027(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.014(18) _cell_angle_gamma 90.00 _cell_volume 5725.5(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 154 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.001 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2464 _exptl_absorpt_coefficient_mu 0.391 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.743197 _exptl_absorpt_correction_T_max 0.918470 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Siemens CCD area detector' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 30322 _diffrn_reflns_av_R_equivalents 0.0567 _diffrn_reflns_av_sigmaI/netI 0.0770 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10066 _reflns_number_gt 6487 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0744P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10066 _refine_ls_number_parameters 707 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0888 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1323 _refine_ls_wR_factor_gt 0.1169 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.956 _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 0.31067(2) 0.691718(19) 0.356284(16) 0.02362(11) Uani 1 1 d . . . N1 N 0.2982(2) 0.4945(2) 0.37948(17) 0.0358(9) Uani 1 1 d . . . N2 N 0.4159(2) 0.7148(2) 0.48944(16) 0.0313(8) Uani 1 1 d . . . N3 N 0.1326(2) 0.6696(2) 0.28598(16) 0.0362(9) Uani 1 1 d . . . N4 N 0.2498(2) 0.8825(2) 0.37049(17) 0.0290(8) Uani 1 1 d . . . C1 C 0.4473(2) 0.6953(2) 0.32391(18) 0.0280(9) Uani 1 1 d . . . C2 C 0.4101(2) 0.6316(2) 0.28839(19) 0.0289(9) Uani 1 1 d . . . C3 C 0.3464(2) 0.6656(2) 0.25056(18) 0.0280(9) Uani 1 1 d . . . C4 C 0.3448(2) 0.7526(2) 0.26182(18) 0.0280(9) Uani 1 1 d . . . H4 H 0.280(2) 0.897(2) 0.3379(19) 0.032(12) Uiso 1 1 d . . . C5 C 0.4075(2) 0.7715(2) 0.30747(18) 0.0275(9) Uani 1 1 d . . . C6 C 0.5250(2) 0.6870(3) 0.3616(2) 0.0384(10) Uani 1 1 d . . . H6A H 0.5699 0.6915 0.3330 0.058 Uiso 1 1 calc R . . H6B H 0.5268 0.6336 0.3828 0.058 Uiso 1 1 calc R . . H6C H 0.5289 0.7305 0.3936 0.058 Uiso 1 1 calc R . . C7 C 0.4416(3) 0.5466(2) 0.2845(2) 0.0383(11) Uani 1 1 d . . . H7A H 0.4816 0.5438 0.2515 0.058 Uiso 1 1 calc R . . H7B H 0.3974 0.5090 0.2738 0.058 Uiso 1 1 calc R . . H7C H 0.4666 0.5311 0.3256 0.058 Uiso 1 1 calc R . . C8 C 0.3013(3) 0.6229(3) 0.19703(19) 0.0384(11) Uani 1 1 d . . . H8A H 0.3340 0.6226 0.1592 0.058 Uiso 1 1 calc R . . H8B H 0.2508 0.6517 0.1875 0.058 Uiso 1 1 calc R . . H8C H 0.2899 0.5664 0.2096 0.058 Uiso 1 1 calc R . . C9 C 0.2987(3) 0.8124(3) 0.2202(2) 0.0386(10) Uani 1 1 d . . . H9A H 0.3302 0.8263 0.1833 0.058 Uiso 1 1 calc R . . H9B H 0.2881 0.8622 0.2446 0.058 Uiso 1 1 calc R . . H9C H 0.2477 0.7877 0.2058 0.058 Uiso 1 1 calc R . . C10 C 0.4379(3) 0.8542(2) 0.3253(2) 0.0357(10) Uani 1 1 d . . . H10C H 0.4785 0.8713 0.2955 0.054 Uiso 1 1 calc R . . H10D H 0.4619 0.8525 0.3685 0.054 Uiso 1 1 calc R . . H10E H 0.3933 0.8933 0.3238 0.054 Uiso 1 1 calc R . . C11 C 0.3038(3) 0.5643(3) 0.37306(19) 0.0319(10) Uani 1 1 d . . . C12 C 0.2913(3) 0.4079(2) 0.3787(2) 0.0340(10) Uani 1 1 d . . . C13 C 0.2635(3) 0.3719(3) 0.3223(2) 0.0384(11) Uani 1 1 d . . . C14 C 0.2634(3) 0.2859(3) 0.3211(2) 0.0431(12) Uani 1 1 d . . . H14A H 0.2466 0.2579 0.2834 0.052 Uiso 1 1 calc R . . C15 C 0.2876(3) 0.2420(3) 0.3743(2) 0.0463(12) Uani 1 1 d . . . H15A H 0.2880 0.1840 0.3724 0.056 Uiso 1 1 calc R . . C16 C 0.3111(3) 0.2804(3) 0.4298(2) 0.0423(12) Uani 1 1 d . . . H16A H 0.3253 0.2484 0.4662 0.051 Uiso 1 1 calc R . . C17 C 0.3147(3) 0.3651(3) 0.4340(2) 0.0376(11) Uani 1 1 d . . . C18 C 0.3393(3) 0.4083(3) 0.4938(2) 0.0501(13) Uani 1 1 d . . . H18A H 0.3533 0.3680 0.5269 0.075 Uiso 1 1 calc R . . H18B H 0.2949 0.4424 0.5077 0.075 Uiso 1 1 calc R . . H18C H 0.3861 0.4428 0.4862 0.075 Uiso 1 1 calc R . . C19 C 0.2367(3) 0.4190(3) 0.2647(2) 0.0536(14) Uani 1 1 d . . . H19A H 0.2405 0.4778 0.2737 0.080 Uiso 1 1 calc R . . H19B H 0.1809 0.4049 0.2532 0.080 Uiso 1 1 calc R . . H19C H 0.2710 0.4054 0.2293 0.080 Uiso 1 1 calc R . . C20 C 0.3830(2) 0.7064(2) 0.4409(2) 0.0291(9) Uani 1 1 d . . . C21 C 0.4521(2) 0.7271(3) 0.55064(18) 0.0298(9) Uani 1 1 d . . . C22 C 0.4654(2) 0.6583(2) 0.58942(19) 0.0316(10) Uani 1 1 d . . . C23 C 0.4994(3) 0.6719(3) 0.6491(2) 0.0390(11) Uani 1 1 d . . . H23A H 0.5092 0.6270 0.6770 0.047 Uiso 1 1 calc R . . C24 C 0.5196(3) 0.7504(3) 0.6689(2) 0.0429(12) Uani 1 1 d . . . H24A H 0.5431 0.7586 0.7103 0.052 Uiso 1 1 calc R . . C25 C 0.5060(3) 0.8171(3) 0.6295(2) 0.0392(11) Uani 1 1 d . . . H25A H 0.5206 0.8703 0.6439 0.047 Uiso 1 1 calc R . . C26 C 0.4713(2) 0.8069(3) 0.5692(2) 0.0340(9) Uani 1 1 d . . . C27 C 0.4434(3) 0.5734(3) 0.5666(2) 0.0445(12) Uani 1 1 d . . . H27A H 0.4572 0.5336 0.6001 0.067 Uiso 1 1 calc R . . H27B H 0.4732 0.5606 0.5285 0.067 Uiso 1 1 calc R . . H27C H 0.3857 0.5709 0.5564 0.067 Uiso 1 1 calc R . . C28 C 0.4562(3) 0.8779(3) 0.5251(2) 0.0502(13) Uani 1 1 d . . . H28A H 0.4734 0.9287 0.5462 0.075 Uiso 1 1 calc R . . H28B H 0.3988 0.8812 0.5137 0.075 Uiso 1 1 calc R . . H28C H 0.4866 0.8702 0.4865 0.075 Uiso 1 1 calc R . . C29 C 0.1958(3) 0.6786(2) 0.30937(18) 0.0277(9) Uani 1 1 d . . . C30 C 0.0542(3) 0.6594(3) 0.2579(2) 0.0385(11) Uani 1 1 d . . . C31 C 0.0121(3) 0.5877(3) 0.2708(2) 0.0479(13) Uani 1 1 d . . . C32 C -0.0645(3) 0.5799(4) 0.2427(3) 0.0616(15) Uani 1 1 d . . . H32A H -0.0948 0.5318 0.2501 0.074 Uiso 1 1 calc R . . C33 C -0.0966(3) 0.6402(4) 0.2046(3) 0.0657(17) Uani 1 1 d . . . H33A H -0.1492 0.6339 0.1864 0.079 Uiso 1 1 calc R . . C34 C -0.0537(3) 0.7098(4) 0.1925(2) 0.0570(15) Uani 1 1 d . . . H34A H -0.0772 0.7513 0.1662 0.068 Uiso 1 1 calc R . . C35 C 0.0239(3) 0.7208(3) 0.2184(2) 0.0446(12) Uani 1 1 d . . . C36 C 0.0725(3) 0.7942(3) 0.2003(3) 0.0596(15) Uani 1 1 d . . . H36A H 0.1250 0.7922 0.2226 0.089 Uiso 1 1 calc R . . H36B H 0.0443 0.8442 0.2122 0.089 Uiso 1 1 calc R . . H36C H 0.0798 0.7939 0.1543 0.089 Uiso 1 1 calc R . . C37 C 0.0444(4) 0.5210(4) 0.3136(3) 0.0743(18) Uani 1 1 d . . . H37A H 0.0048 0.4769 0.3156 0.111 Uiso 1 1 calc R . . H37B H 0.0552 0.5431 0.3564 0.111 Uiso 1 1 calc R . . H37C H 0.0942 0.4995 0.2967 0.111 Uiso 1 1 calc R . . C38 C 0.2559(2) 0.8059(2) 0.38949(18) 0.0270(9) Uani 1 1 d . . . C39 C 0.2037(3) 0.9475(2) 0.39953(19) 0.0304(10) Uani 1 1 d . . . C40 C 0.1206(3) 0.9412(2) 0.40061(19) 0.0320(10) Uani 1 1 d . . . C41 C 0.0800(3) 0.9996(3) 0.4354(2) 0.0395(11) Uani 1 1 d . . . H41A H 0.0235 0.9959 0.4384 0.047 Uiso 1 1 calc R . . C42 C 0.1211(3) 1.0630(3) 0.4657(2) 0.0429(12) Uani 1 1 d . . . H42A H 0.0928 1.1018 0.4899 0.051 Uiso 1 1 calc R . . C43 C 0.2030(3) 1.0698(3) 0.4606(2) 0.0386(11) Uani 1 1 d . . . H43A H 0.2303 1.1147 0.4802 0.046 Uiso 1 1 calc R . . C44 C 0.2463(3) 1.0127(2) 0.42751(19) 0.0327(10) Uani 1 1 d . . . C45 C 0.3356(3) 1.0205(3) 0.4239(2) 0.0400(11) Uani 1 1 d . . . H45A H 0.3536 1.0701 0.4463 0.060 Uiso 1 1 calc R . . H45B H 0.3502 1.0239 0.3792 0.060 Uiso 1 1 calc R . . H45C H 0.3614 0.9726 0.4437 0.060 Uiso 1 1 calc R . . C46 C 0.0729(3) 0.8755(3) 0.3653(2) 0.0426(11) Uani 1 1 d . . . H46A H 0.1096 0.8393 0.3433 0.064 Uiso 1 1 calc R . . H46B H 0.0357 0.9011 0.3342 0.064 Uiso 1 1 calc R . . H46C H 0.0425 0.8436 0.3957 0.064 Uiso 1 1 calc R . . C47 C 0.2292(2) 0.6904(2) 0.43800(18) 0.0270(9) Uani 1 1 d . . . C48 C 0.2026(2) 0.6272(2) 0.48299(19) 0.0302(9) Uani 1 1 d . . . C49 C 0.1518(3) 0.5643(3) 0.4635(2) 0.0511(13) Uani 1 1 d . . . H49A H 0.1349 0.5604 0.4199 0.061 Uiso 1 1 calc R . . C50 C 0.1252(3) 0.5072(3) 0.5065(3) 0.0592(15) Uani 1 1 d . . . H50A H 0.0879 0.4663 0.4928 0.071 Uiso 1 1 calc R . . C51 C 0.1526(3) 0.5092(3) 0.5690(2) 0.0482(13) Uani 1 1 d . . . H51A H 0.1355 0.4690 0.5982 0.058 Uiso 1 1 calc R . . C52 C 0.2044(3) 0.5693(3) 0.5886(2) 0.0415(11) Uani 1 1 d . . . H52A H 0.2237 0.5708 0.6316 0.050 Uiso 1 1 calc R . . C53 C 0.2292(3) 0.6287(2) 0.54592(19) 0.0356(10) Uani 1 1 d . . . H53A H 0.2649 0.6707 0.5603 0.043 Uiso 1 1 calc R . . C54 C 0.2170(2) 0.7726(2) 0.44480(18) 0.0270(9) Uani 1 1 d . . . C55 C 0.1741(2) 0.8124(2) 0.49725(18) 0.0291(9) Uani 1 1 d . . . C56 C 0.0972(3) 0.7864(3) 0.5116(2) 0.0352(10) Uani 1 1 d . . . H56A H 0.0729 0.7428 0.4880 0.042 Uiso 1 1 calc R . . C57 C 0.0558(3) 0.8230(3) 0.5596(2) 0.0442(12) Uani 1 1 d . . . H57A H 0.0034 0.8050 0.5688 0.053 Uiso 1 1 calc R . . C58 C 0.0916(3) 0.8867(3) 0.5944(2) 0.0444(12) Uani 1 1 d . . . H58A H 0.0633 0.9122 0.6275 0.053 Uiso 1 1 calc R . . C59 C 0.1676(3) 0.9125(3) 0.5812(2) 0.0380(11) Uani 1 1 d . . . H59A H 0.1918 0.9560 0.6050 0.046 Uiso 1 1 calc R . . C60 C 0.2090(3) 0.8753(2) 0.53315(19) 0.0332(10) Uani 1 1 d . . . H60A H 0.2618 0.8930 0.5246 0.040 Uiso 1 1 calc R . . B1 B 0.6876(3) 0.9488(3) 0.7699(3) 0.0399(13) Uani 1 1 d . . . F1 F 0.6409(2) 0.8981(2) 0.73294(15) 0.0875(11) Uani 1 1 d . . . F2 F 0.7379(2) 0.9056(2) 0.80889(19) 0.1047(14) Uani 1 1 d . . . F3 F 0.63894(19) 0.99538(19) 0.80677(16) 0.0765(10) Uani 1 1 d . . . F4 F 0.73293(19) 1.00050(16) 0.73267(14) 0.0629(8) Uani 1 1 d . . . B101 B 0.3544(4) 1.1040(4) 0.6123(3) 0.0567(16) Uani 1 1 d . . . F101 F 0.4077(3) 1.0407(3) 0.6134(3) 0.1468(19) Uani 1 1 d . . . F102 F 0.3705(2) 1.1537(2) 0.56287(16) 0.0861(11) Uani 1 1 d . . . F103 F 0.2774(2) 1.0772(3) 0.60824(17) 0.1177(16) Uani 1 1 d . . . F104 F 0.36839(19) 1.1443(2) 0.66831(15) 0.0870(11) Uani 1 1 d . . . C100 C -0.1825(4) 0.7375(4) 0.4008(3) 0.093(2) Uani 1 1 d . . . H10A H -0.2153 0.6899 0.3868 0.112 Uiso 1 1 calc R . . H10B H -0.2187 0.7852 0.4044 0.112 Uiso 1 1 calc R . . Cl1 Cl -0.13671(15) 0.71663(11) 0.47577(11) 0.1141(7) Uani 1 1 d . . . Cl2 Cl -0.11170(14) 0.75797(19) 0.34486(11) 0.1429(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.02591(19) 0.02104(17) 0.02369(18) 0.00173(15) -0.00217(13) 0.00143(17) N1 0.044(2) 0.0213(19) 0.042(2) 0.0029(15) 0.0098(18) 0.0010(17) N2 0.0271(19) 0.041(2) 0.0257(19) 0.0017(15) -0.0019(16) 0.0013(16) N3 0.033(2) 0.042(2) 0.034(2) -0.0073(16) -0.0001(18) -0.0003(17) N4 0.031(2) 0.0267(19) 0.030(2) 0.0018(15) 0.0065(17) 0.0001(16) C1 0.026(2) 0.035(2) 0.023(2) 0.0039(18) 0.0014(16) -0.003(2) C2 0.029(2) 0.029(2) 0.029(2) -0.0012(17) 0.0037(18) 0.0018(18) C3 0.028(2) 0.032(2) 0.024(2) 0.0001(17) 0.0011(18) -0.0011(18) C4 0.028(2) 0.030(2) 0.026(2) 0.0038(17) 0.0025(18) 0.0022(18) C5 0.029(2) 0.029(2) 0.025(2) 0.0010(17) 0.0045(18) 0.0007(18) C6 0.028(2) 0.050(3) 0.037(2) -0.001(2) -0.0037(19) 0.001(2) C7 0.035(3) 0.034(2) 0.046(3) 0.001(2) 0.003(2) 0.008(2) C8 0.038(3) 0.045(3) 0.032(2) -0.005(2) -0.002(2) -0.002(2) C9 0.044(3) 0.035(2) 0.036(2) 0.014(2) -0.002(2) 0.003(2) C10 0.036(3) 0.030(2) 0.041(3) -0.0001(19) 0.007(2) -0.006(2) C11 0.034(2) 0.033(2) 0.029(2) 0.0006(18) 0.003(2) 0.001(2) C12 0.034(3) 0.020(2) 0.049(3) 0.0023(19) 0.011(2) 0.0008(18) C13 0.037(3) 0.032(2) 0.047(3) 0.000(2) 0.005(2) 0.002(2) C14 0.045(3) 0.035(3) 0.050(3) -0.007(2) 0.003(2) -0.003(2) C15 0.047(3) 0.025(2) 0.067(4) 0.003(2) 0.007(3) -0.002(2) C16 0.044(3) 0.029(2) 0.054(3) 0.011(2) 0.000(2) 0.000(2) C17 0.031(2) 0.033(2) 0.049(3) 0.007(2) 0.000(2) -0.002(2) C18 0.052(3) 0.042(3) 0.056(3) 0.009(2) -0.009(3) -0.003(2) C19 0.070(4) 0.043(3) 0.047(3) 0.001(2) 0.004(3) 0.004(3) C20 0.030(2) 0.026(2) 0.032(2) 0.0021(17) 0.0020(19) 0.0025(18) C21 0.026(2) 0.040(2) 0.023(2) -0.0046(18) -0.0015(18) 0.0025(19) C22 0.031(2) 0.038(2) 0.026(2) 0.0013(18) 0.0032(19) 0.0030(19) C23 0.040(3) 0.046(3) 0.031(2) 0.004(2) -0.001(2) 0.008(2) C24 0.040(3) 0.060(3) 0.029(2) -0.010(2) 0.000(2) 0.003(2) C25 0.034(2) 0.047(3) 0.036(2) -0.011(2) -0.001(2) -0.003(2) C26 0.028(2) 0.037(2) 0.037(2) -0.002(2) 0.0050(19) 0.003(2) C27 0.052(3) 0.037(2) 0.044(3) -0.001(2) -0.003(2) 0.006(2) C28 0.053(3) 0.040(3) 0.058(3) 0.003(2) -0.004(3) 0.004(2) C29 0.034(2) 0.023(2) 0.027(2) 0.0012(16) 0.0006(19) 0.0000(18) C30 0.024(2) 0.056(3) 0.035(3) -0.015(2) -0.003(2) 0.001(2) C31 0.036(3) 0.069(3) 0.038(3) -0.012(2) -0.001(2) -0.006(3) C32 0.041(3) 0.092(4) 0.053(3) -0.019(3) 0.008(3) -0.021(3) C33 0.028(3) 0.113(5) 0.056(4) -0.022(4) -0.001(3) 0.000(3) C34 0.037(3) 0.088(4) 0.046(3) -0.012(3) -0.004(2) 0.021(3) C35 0.034(3) 0.058(3) 0.041(3) -0.017(2) -0.003(2) 0.008(2) C36 0.067(4) 0.051(3) 0.059(3) -0.006(3) -0.021(3) 0.017(3) C37 0.068(4) 0.077(4) 0.076(4) 0.004(3) -0.013(3) -0.032(3) C38 0.026(2) 0.025(2) 0.029(2) 0.0032(18) -0.0058(17) -0.0012(19) C39 0.037(3) 0.026(2) 0.029(2) 0.0045(17) 0.0039(19) 0.0065(19) C40 0.038(3) 0.028(2) 0.029(2) 0.0087(18) -0.0003(19) 0.0054(19) C41 0.037(3) 0.044(3) 0.037(3) 0.006(2) 0.001(2) 0.015(2) C42 0.055(3) 0.033(2) 0.041(3) 0.005(2) 0.005(2) 0.014(2) C43 0.055(3) 0.026(2) 0.035(3) 0.0024(19) 0.003(2) 0.005(2) C44 0.040(3) 0.029(2) 0.029(2) 0.0084(18) 0.004(2) 0.002(2) C45 0.043(3) 0.030(2) 0.046(3) -0.001(2) 0.000(2) -0.001(2) C46 0.037(3) 0.048(3) 0.041(3) -0.006(2) -0.008(2) 0.007(2) C47 0.025(2) 0.029(2) 0.027(2) 0.0016(18) -0.0040(16) 0.0015(19) C48 0.028(2) 0.030(2) 0.032(2) 0.0053(18) 0.0030(19) 0.0011(19) C49 0.064(3) 0.052(3) 0.037(3) 0.009(2) -0.008(3) -0.022(3) C50 0.062(4) 0.057(3) 0.058(4) 0.010(3) -0.005(3) -0.030(3) C51 0.060(3) 0.039(3) 0.046(3) 0.013(2) 0.011(3) -0.006(2) C52 0.054(3) 0.040(3) 0.031(2) 0.006(2) 0.005(2) 0.007(2) C53 0.043(3) 0.029(2) 0.035(3) 0.0015(19) 0.001(2) -0.001(2) C54 0.023(2) 0.030(2) 0.027(2) 0.0047(17) -0.0008(18) 0.0004(18) C55 0.034(2) 0.029(2) 0.024(2) 0.0048(18) 0.0002(17) 0.007(2) C56 0.033(2) 0.039(3) 0.033(2) 0.0054(19) 0.003(2) 0.005(2) C57 0.036(3) 0.053(3) 0.044(3) 0.011(2) 0.011(2) 0.012(2) C58 0.051(3) 0.051(3) 0.032(3) 0.005(2) 0.010(2) 0.024(3) C59 0.050(3) 0.036(2) 0.027(2) 0.0025(19) -0.007(2) 0.013(2) C60 0.034(2) 0.033(2) 0.032(2) 0.0076(19) -0.002(2) 0.008(2) B1 0.044(3) 0.035(3) 0.041(3) -0.001(2) 0.001(3) -0.005(3) F1 0.125(3) 0.075(2) 0.062(2) -0.0243(18) 0.004(2) -0.040(2) F2 0.095(3) 0.099(3) 0.118(3) 0.057(2) -0.020(2) 0.017(2) F3 0.067(2) 0.068(2) 0.096(3) -0.0270(19) 0.0350(19) -0.0158(17) F4 0.077(2) 0.0451(16) 0.069(2) 0.0115(14) 0.0292(17) -0.0003(15) B101 0.057(4) 0.049(4) 0.064(4) -0.005(3) 0.009(3) -0.009(3) F101 0.177(5) 0.077(3) 0.185(5) -0.005(3) -0.003(4) 0.031(3) F102 0.112(3) 0.083(2) 0.063(2) 0.0143(18) 0.005(2) -0.037(2) F103 0.102(3) 0.182(4) 0.068(2) 0.002(2) -0.014(2) -0.094(3) F104 0.061(2) 0.142(3) 0.059(2) -0.023(2) 0.0077(17) -0.038(2) C100 0.058(4) 0.104(5) 0.119(6) -0.042(5) 0.019(4) -0.019(4) Cl1 0.157(2) 0.0695(11) 0.1173(16) -0.0113(11) 0.0259(15) -0.0180(12) Cl2 0.1091(17) 0.222(3) 0.1002(16) -0.0352(17) 0.0416(14) -0.0352(18) _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 C11 2.116(4) . ? Mo1 C20 2.128(4) . ? Mo1 C29 2.134(4) . ? Mo1 C38 2.202(4) . ? Mo1 C47 2.228(4) . ? Mo1 C4 2.310(4) . ? Mo1 C5 2.341(4) . ? Mo1 C3 2.361(4) . ? Mo1 C1 2.402(4) . ? Mo1 C2 2.433(4) . ? N1 C11 1.152(5) . ? N1 C12 1.420(5) . ? N2 C20 1.149(5) . ? N2 C21 1.416(5) . ? N3 C29 1.157(5) . ? N3 C30 1.425(5) . ? N4 C38 1.316(5) . ? N4 C39 1.457(5) . ? C1 C2 1.412(5) . ? C1 C5 1.447(5) . ? C1 C6 1.501(5) . ? C2 C3 1.418(5) . ? C2 C7 1.488(5) . ? C3 C4 1.442(5) . ? C3 C8 1.503(5) . ? C4 C5 1.429(5) . ? C4 C9 1.504(5) . ? C5 C10 1.486(5) . ? C12 C13 1.389(6) . ? C12 C17 1.400(6) . ? C13 C14 1.405(6) . ? C13 C19 1.490(6) . ? C14 C15 1.376(6) . ? C15 C16 1.370(6) . ? C16 C17 1.386(6) . ? C17 C18 1.488(6) . ? C21 C26 1.397(6) . ? C21 C22 1.401(5) . ? C22 C23 1.377(6) . ? C22 C27 1.508(6) . ? C23 C24 1.387(6) . ? C24 C25 1.383(6) . ? C25 C26 1.384(6) . ? C26 C28 1.501(6) . ? C30 C35 1.386(6) . ? C30 C31 1.397(6) . ? C31 C32 1.395(7) . ? C31 C37 1.501(7) . ? C32 C33 1.367(8) . ? C33 C34 1.372(8) . ? C34 C35 1.397(7) . ? C35 C36 1.504(7) . ? C38 C54 1.457(5) . ? C39 C40 1.389(6) . ? C39 C44 1.400(5) . ? C40 C41 1.392(6) . ? C40 C46 1.516(6) . ? C41 C42 1.384(6) . ? C42 C43 1.378(6) . ? C43 C44 1.381(6) . ? C44 C45 1.500(6) . ? C47 C54 1.367(5) . ? C47 C48 1.479(5) . ? C48 C53 1.381(5) . ? C48 C49 1.384(6) . ? C49 C50 1.384(6) . ? C50 C51 1.376(6) . ? C51 C52 1.362(6) . ? C52 C53 1.395(6) . ? C54 C55 1.485(6) . ? C55 C60 1.391(5) . ? C55 C56 1.394(6) . ? C56 C57 1.378(6) . ? C57 C58 1.394(6) . ? C58 C59 1.374(6) . ? C59 C60 1.384(6) . ? B1 F2 1.352(6) . ? B1 F1 1.362(6) . ? B1 F3 1.373(6) . ? B1 F4 1.392(6) . ? B101 F102 1.353(7) . ? B101 F103 1.356(7) . ? B101 F104 1.362(7) . ? B101 F101 1.365(8) . ? C100 Cl2 1.729(7) . ? C100 Cl1 1.760(8) . ? 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 Mo1 C20 90.23(14) . . ? C11 Mo1 C29 85.71(15) . . ? C20 Mo1 C29 150.57(16) . . ? C11 Mo1 C38 139.10(16) . . ? C20 Mo1 C38 82.44(14) . . ? C29 Mo1 C38 81.75(14) . . ? C11 Mo1 C47 79.86(15) . . ? C20 Mo1 C47 72.49(14) . . ? C29 Mo1 C47 78.10(14) . . ? C38 Mo1 C47 59.52(14) . . ? C11 Mo1 C4 125.69(14) . . ? C20 Mo1 C4 121.39(15) . . ? C29 Mo1 C4 83.69(14) . . ? C38 Mo1 C4 91.44(14) . . ? C47 Mo1 C4 147.41(14) . . ? C11 Mo1 C5 131.56(15) . . ? C20 Mo1 C5 85.66(14) . . ? C29 Mo1 C5 118.38(14) . . ? C38 Mo1 C5 88.12(14) . . ? C47 Mo1 C5 142.42(14) . . ? C4 Mo1 C5 35.77(13) . . ? C11 Mo1 C3 89.77(14) . . ? C20 Mo1 C3 130.80(15) . . ? C29 Mo1 C3 78.39(14) . . ? C38 Mo1 C3 124.96(14) . . ? C47 Mo1 C3 154.91(14) . . ? C4 Mo1 C3 35.93(13) . . ? C5 Mo1 C3 59.12(13) . . ? C11 Mo1 C1 97.39(15) . . ? C20 Mo1 C1 73.66(14) . . ? C29 Mo1 C1 135.76(14) . . ? C38 Mo1 C1 118.50(14) . . ? C47 Mo1 C1 146.02(13) . . ? C4 Mo1 C1 58.74(13) . . ? C5 Mo1 C1 35.50(13) . . ? C3 Mo1 C1 57.59(13) . . ? C11 Mo1 C2 75.08(15) . . ? C20 Mo1 C2 99.11(14) . . ? C29 Mo1 C2 107.90(14) . . ? C38 Mo1 C2 145.79(14) . . ? C47 Mo1 C2 153.57(13) . . ? C4 Mo1 C2 58.38(13) . . ? C5 Mo1 C2 58.16(14) . . ? C3 Mo1 C2 34.36(13) . . ? C1 Mo1 C2 33.96(13) . . ? C11 N1 C12 172.6(4) . . ? C20 N2 C21 176.6(4) . . ? C29 N3 C30 179.1(4) . . ? C38 N4 C39 127.0(4) . . ? C2 C1 C5 108.6(3) . . ? C2 C1 C6 124.6(4) . . ? C5 C1 C6 125.7(4) . . ? C2 C1 Mo1 74.2(2) . . ? C5 C1 Mo1 70.0(2) . . ? C6 C1 Mo1 131.1(3) . . ? C1 C2 C3 108.3(3) . . ? C1 C2 C7 124.6(4) . . ? C3 C2 C7 126.4(4) . . ? C1 C2 Mo1 71.8(2) . . ? C3 C2 Mo1 70.0(2) . . ? C7 C2 Mo1 131.2(3) . . ? C2 C3 C4 108.2(3) . . ? C2 C3 C8 125.7(4) . . ? C4 C3 C8 124.7(4) . . ? C2 C3 Mo1 75.6(2) . . ? C4 C3 Mo1 70.1(2) . . ? C8 C3 Mo1 130.8(3) . . ? C5 C4 C3 107.8(3) . . ? C5 C4 C9 126.7(3) . . ? C3 C4 C9 123.9(3) . . ? C5 C4 Mo1 73.3(2) . . ? C3 C4 Mo1 73.9(2) . . ? C9 C4 Mo1 130.0(3) . . ? C4 C5 C1 107.0(3) . . ? C4 C5 C10 127.0(4) . . ? C1 C5 C10 124.9(3) . . ? C4 C5 Mo1 71.0(2) . . ? C1 C5 Mo1 74.5(2) . . ? C10 C5 Mo1 129.0(3) . . ? N1 C11 Mo1 176.8(4) . . ? C13 C12 C17 124.9(4) . . ? C13 C12 N1 117.1(4) . . ? C17 C12 N1 117.9(4) . . ? C12 C13 C14 116.0(4) . . ? C12 C13 C19 123.8(4) . . ? C14 C13 C19 120.2(4) . . ? C15 C14 C13 120.5(4) . . ? C16 C15 C14 121.3(4) . . ? C15 C16 C17 121.4(4) . . ? C16 C17 C12 115.8(4) . . ? C16 C17 C18 122.5(4) . . ? C12 C17 C18 121.7(4) . . ? N2 C20 Mo1 174.0(4) . . ? C26 C21 C22 123.8(4) . . ? C26 C21 N2 118.2(4) . . ? C22 C21 N2 118.0(4) . . ? C23 C22 C21 116.9(4) . . ? C23 C22 C27 121.8(4) . . ? C21 C22 C27 121.3(4) . . ? C22 C23 C24 120.8(4) . . ? C25 C24 C23 121.0(4) . . ? C24 C25 C26 120.6(4) . . ? C25 C26 C21 116.9(4) . . ? C25 C26 C28 121.9(4) . . ? C21 C26 C28 121.1(4) . . ? N3 C29 Mo1 177.3(4) . . ? C35 C30 C31 123.2(4) . . ? C35 C30 N3 118.3(4) . . ? C31 C30 N3 118.5(4) . . ? C32 C31 C30 117.0(5) . . ? C32 C31 C37 119.4(5) . . ? C30 C31 C37 123.6(4) . . ? C33 C32 C31 121.1(5) . . ? C32 C33 C34 120.7(5) . . ? C33 C34 C35 121.0(5) . . ? C30 C35 C34 117.0(5) . . ? C30 C35 C36 122.6(4) . . ? C34 C35 C36 120.2(5) . . ? N4 C38 C54 124.4(4) . . ? N4 C38 Mo1 137.6(3) . . ? C54 C38 Mo1 97.9(2) . . ? C40 C39 C44 122.7(4) . . ? C40 C39 N4 119.6(4) . . ? C44 C39 N4 117.6(4) . . ? C39 C40 C41 117.5(4) . . ? C39 C40 C46 123.4(4) . . ? C41 C40 C46 119.1(4) . . ? C42 C41 C40 120.8(4) . . ? C43 C42 C41 120.0(4) . . ? C42 C43 C44 121.4(4) . . ? C43 C44 C39 117.4(4) . . ? C43 C44 C45 120.4(4) . . ? C39 C44 C45 122.2(4) . . ? C54 C47 C48 124.7(4) . . ? C54 C47 Mo1 99.7(3) . . ? C48 C47 Mo1 134.8(3) . . ? C53 C48 C49 118.0(4) . . ? C53 C48 C47 120.4(4) . . ? C49 C48 C47 121.5(4) . . ? C50 C49 C48 120.9(4) . . ? C51 C50 C49 120.3(5) . . ? C52 C51 C50 119.5(4) . . ? C51 C52 C53 120.4(4) . . ? C48 C53 C52 120.7(4) . . ? C47 C54 C38 102.2(4) . . ? C47 C54 C55 125.8(4) . . ? C38 C54 C55 132.0(3) . . ? C60 C55 C56 118.6(4) . . ? C60 C55 C54 121.5(4) . . ? C56 C55 C54 119.9(4) . . ? C57 C56 C55 120.9(4) . . ? C56 C57 C58 119.5(4) . . ? C59 C58 C57 120.2(4) . . ? C58 C59 C60 120.0(4) . . ? C59 C60 C55 120.7(4) . . ? F2 B1 F1 111.0(4) . . ? F2 B1 F3 108.3(5) . . ? F1 B1 F3 108.7(4) . . ? F2 B1 F4 108.7(4) . . ? F1 B1 F4 111.1(4) . . ? F3 B1 F4 109.0(4) . . ? F102 B101 F103 111.1(5) . . ? F102 B101 F104 110.0(5) . . ? F103 B101 F104 110.1(5) . . ? F102 B101 F101 108.7(6) . . ? F103 B101 F101 111.8(5) . . ? F104 B101 F101 105.0(5) . . ? Cl2 C100 Cl1 111.2(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.938 _refine_diff_density_min -0.946 _refine_diff_density_rms 0.072 #===END data_7(8) _database_code_CSD 155030 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37.09 H42.09 B Cl2.10 F4 Mo N3' _chemical_formula_weight 786.99 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' 'B' 'B' 0.0013 0.0007 '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' 'F' 'F' 0.0171 0.0103 '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 8.269(2) _cell_length_b 14.598(3) _cell_length_c 15.379(3) _cell_angle_alpha 103.043(18) _cell_angle_beta 90.989(19) _cell_angle_gamma 92.729(19) _cell_volume 1805.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 105 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 809 _exptl_absorpt_coefficient_mu 0.570 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.685690 _exptl_absorpt_correction_T_max 0.862083 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Siemens CCD area detector' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 15784 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_sigmaI/netI 0.0370 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6344 _reflns_number_gt 5052 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0580P)^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 6344 _refine_ls_number_parameters 506 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0439 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0887 _refine_ls_wR_factor_gt 0.0850 _refine_ls_goodness_of_fit_ref 0.962 _refine_ls_restrained_S_all 0.962 _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 0.23955(3) 0.309528(15) 0.296984(15) 0.03685(9) Uani 1 1 d . . . Cl1 Cl 0.49623(9) 0.39773(5) 0.35603(6) 0.0602(2) Uani 1 1 d . A . N1 N 0.2607(3) 0.45314(17) 0.16225(19) 0.0555(7) Uani 1 1 d . . . N2 N 0.4259(3) 0.15176(18) 0.37653(16) 0.0484(6) Uani 1 1 d . . . N3 N 0.0208(3) 0.15291(16) 0.15455(15) 0.0449(6) Uani 1 1 d . . . C1 C -0.0372(3) 0.29965(18) 0.34531(17) 0.0386(6) Uani 1 1 d . A . C2 C 0.0692(3) 0.2915(2) 0.41718(18) 0.0433(7) Uani 1 1 d . A . C3 C 0.1661(3) 0.3772(2) 0.4431(2) 0.0534(8) Uani 1 1 d . A . C4 C 0.1228(4) 0.4370(2) 0.3860(2) 0.0530(8) Uani 1 1 d . A . C5 C -0.0029(3) 0.38832(19) 0.3251(2) 0.0455(7) Uani 1 1 d . A . C6 C -0.1805(3) 0.2348(2) 0.3126(2) 0.0498(7) Uani 1 1 d . . . H6A H -0.2703 0.2512 0.3530 0.075 Uiso 1 1 calc R A . H6B H -0.1528 0.1698 0.3108 0.075 Uiso 1 1 calc R . . H6C H -0.2128 0.2405 0.2525 0.075 Uiso 1 1 calc R . . C7 C 0.0578(4) 0.2145(2) 0.4661(2) 0.0587(8) Uani 1 1 d . . . H7A H -0.0304 0.2255 0.5083 0.088 Uiso 1 1 calc R A . H7B H 0.1602 0.2131 0.4987 0.088 Uiso 1 1 calc R . . H7C H 0.0362 0.1541 0.4234 0.088 Uiso 1 1 calc R . . C8 C 0.2730(4) 0.4035(3) 0.5256(2) 0.0825(13) Uani 1 1 d . . . H8A H 0.3233 0.3473 0.5359 0.124 Uiso 1 1 calc R A . H8B H 0.2080 0.4303 0.5770 0.124 Uiso 1 1 calc R . . H8C H 0.3575 0.4502 0.5180 0.124 Uiso 1 1 calc R . . C9 C 0.1824(4) 0.5385(2) 0.3983(3) 0.0800(12) Uani 1 1 d . . . H9A H 0.1380 0.5760 0.4528 0.120 Uiso 1 1 calc R A . H9B H 0.1471 0.5624 0.3469 0.120 Uiso 1 1 calc R . . H9C H 0.3010 0.5430 0.4033 0.120 Uiso 1 1 calc R . . C10 C -0.1012(4) 0.4263(2) 0.2597(2) 0.0635(9) Uani 1 1 d . . . H10A H -0.2092 0.4394 0.2831 0.095 Uiso 1 1 calc R A . H10B H -0.1110 0.3798 0.2027 0.095 Uiso 1 1 calc R . . H10C H -0.0475 0.4846 0.2506 0.095 Uiso 1 1 calc R . . C11 C 0.2447(3) 0.4034(2) 0.2105(2) 0.0476(7) Uani 1 1 d . A . C12 C 0.2816(4) 0.5022(2) 0.0924(3) 0.0649(10) Uani 1 1 d . A . C13 C 0.3715(5) 0.5851(3) 0.1122(3) 0.0803(12) Uani 1 1 d . . . C14 C 0.4014(5) 0.6286(3) 0.0384(4) 0.0957(15) Uani 1 1 d . A . H14A H 0.4637 0.6864 0.0464 0.115 Uiso 1 1 calc R . . C15 C 0.3371(6) 0.5840(4) -0.0434(4) 0.0986(16) Uani 1 1 d . . . H15A H 0.3579 0.6126 -0.0920 0.118 Uiso 1 1 calc R A . C16 C 0.2458(5) 0.5019(3) -0.0604(3) 0.0844(12) Uani 1 1 d . A . H16A H 0.2045 0.4757 -0.1193 0.101 Uiso 1 1 calc R . . C17 C 0.2123(5) 0.4559(3) 0.0077(3) 0.0707(10) Uani 1 1 d . . . C18 C 0.1193(5) 0.3647(3) -0.0060(3) 0.0799(11) Uani 1 1 d . A . H18A H 0.0292 0.3705 0.0350 0.120 Uiso 1 1 calc R . . H18B H 0.1903 0.3166 0.0055 0.120 Uiso 1 1 calc R . . H18C H 0.0768 0.3464 -0.0677 0.120 Uiso 1 1 calc R . . C19 C 0.4407(5) 0.6269(3) 0.2028(4) 0.1030(16) Uani 1 1 d . A . H19A H 0.3541 0.6529 0.2421 0.155 Uiso 1 1 calc R . . H19B H 0.5217 0.6772 0.1996 0.155 Uiso 1 1 calc R . . H19C H 0.4921 0.5781 0.2265 0.155 Uiso 1 1 calc R . . C20 C 0.3463(3) 0.2033(2) 0.35138(18) 0.0439(7) Uani 1 1 d . A . C21 C 0.5400(3) 0.0926(2) 0.4024(2) 0.0513(7) Uani 1 1 d . A . C22 C 0.5753(4) 0.0108(2) 0.3396(3) 0.0639(9) Uani 1 1 d . . . C23 C 0.6950(4) -0.0427(3) 0.3650(3) 0.0771(11) Uani 1 1 d . A . H23A H 0.7245 -0.0985 0.3247 0.092 Uiso 1 1 calc R . . C24 C 0.7703(5) -0.0160(4) 0.4466(4) 0.0874(14) Uani 1 1 d . . . H24A H 0.8520 -0.0536 0.4620 0.105 Uiso 1 1 calc R A . C25 C 0.7323(5) 0.0629(4) 0.5072(3) 0.0810(13) Uani 1 1 d . A . H25A H 0.7857 0.0785 0.5642 0.097 Uiso 1 1 calc R . . C26 C 0.6144(4) 0.1219(3) 0.4860(2) 0.0635(9) Uani 1 1 d . . . C27 C 0.5751(5) 0.2114(3) 0.5485(3) 0.0854(12) Uani 1 1 d . A . H27A H 0.5889 0.2637 0.5185 0.128 Uiso 1 1 calc R . . H27B H 0.6478 0.2229 0.6013 0.128 Uiso 1 1 calc R . . H27C H 0.4626 0.2066 0.5668 0.128 Uiso 1 1 calc R . . C28 C 0.4926(6) -0.0172(3) 0.2507(3) 0.0994(15) Uani 1 1 d . A . H28A H 0.4898 0.0375 0.2238 0.149 Uiso 1 1 calc R . . H28B H 0.3818 -0.0410 0.2572 0.149 Uiso 1 1 calc R . . H28C H 0.5517 -0.0666 0.2122 0.149 Uiso 1 1 calc R . . C29 C 0.0998(3) 0.20903(19) 0.20444(18) 0.0398(6) Uani 1 1 d . A . C30 C -0.0789(3) 0.0742(2) 0.11041(19) 0.0447(7) Uani 1 1 d . A . C31 C -0.1843(4) 0.0833(2) 0.0419(2) 0.0538(8) Uani 1 1 d . . . C32 C -0.2805(4) 0.0021(3) 0.0012(2) 0.0649(10) Uani 1 1 d . A . H32A H -0.3540 0.0045 -0.0463 0.078 Uiso 1 1 calc R . . C33 C -0.2697(4) -0.0801(3) 0.0291(3) 0.0696(10) Uani 1 1 d . . . H33A H -0.3348 -0.1341 0.0003 0.084 Uiso 1 1 calc R A . C34 C -0.1669(4) -0.0854(2) 0.0978(2) 0.0659(9) Uani 1 1 d . A . H34A H -0.1630 -0.1429 0.1168 0.079 Uiso 1 1 calc R . . C35 C -0.0680(4) -0.0087(2) 0.1403(2) 0.0529(8) Uani 1 1 d . . . C36 C 0.0464(5) -0.0150(3) 0.2143(3) 0.0748(10) Uani 1 1 d . A . H36A H 0.0079 0.0217 0.2708 0.112 Uiso 1 1 calc R . . H36B H 0.1541 0.0101 0.2030 0.112 Uiso 1 1 calc R . . H36C H 0.0524 -0.0810 0.2177 0.112 Uiso 1 1 calc R . . C37 C -0.1952(5) 0.1733(3) 0.0142(3) 0.0780(11) Uani 1 1 d . A . H37A H -0.0874 0.1949 -0.0009 0.117 Uiso 1 1 calc R . . H37B H -0.2371 0.2206 0.0631 0.117 Uiso 1 1 calc R . . H37C H -0.2684 0.1643 -0.0382 0.117 Uiso 1 1 calc R . . Cl99 Cl 0.42751(12) 0.23695(6) 0.17967(7) 0.0444(3) Uani 0.906(2) 1 d P A 1 C99 C 0.458(7) 0.262(3) 0.191(4) 0.0444(3) Uani 0.094(2) 1 d P A 2 H99A H 0.5580 0.3051 0.2051 0.053 Uiso 0.094(2) 1 calc PR A 2 Cl3 Cl 0.4994(10) 0.1435(6) 0.1800(5) 0.057(3) Uani 0.094(2) 1 d P A 2 Cl2 Cl 0.3666(12) 0.2619(6) 0.0777(5) 0.064(3) Uani 0.094(2) 1 d P A 2 B1 B 1.024(3) 0.268(2) 0.7201(12) 0.071(4) Uani 0.549(6) 1 d P B 1 F1 F 0.9360(16) 0.2270(7) 0.6839(7) 0.177(5) Uani 0.549(6) 1 d P B 1 F2 F 0.9815(7) 0.3555(4) 0.7783(3) 0.0949(18) Uani 0.549(6) 1 d P B 1 F3 F 1.1468(11) 0.2411(5) 0.7840(4) 0.091(2) Uani 0.549(6) 1 d P B 1 F4 F 1.1604(8) 0.3142(6) 0.6748(3) 0.135(3) Uani 0.549(6) 1 d P B 1 B1' B 1.066(4) 0.277(3) 0.7421(17) 0.071(4) Uani 0.451(6) 1 d P B 2 F1' F 1.1609(15) 0.2458(10) 0.7463(16) 0.254(11) Uani 0.451(6) 1 d P B 2 F2' F 0.9804(13) 0.1838(6) 0.6617(4) 0.097(3) Uani 0.451(6) 1 d P B 2 F3' F 0.9145(9) 0.2456(5) 0.7906(5) 0.124(3) Uani 0.451(6) 1 d P B 2 F4' F 0.9890(17) 0.3313(8) 0.6969(13) 0.247(8) Uani 0.451(6) 1 d P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.03011(14) 0.03555(13) 0.04122(14) 0.00051(10) 0.00620(9) 0.00202(9) Cl1 0.0357(4) 0.0572(4) 0.0727(5) -0.0159(4) 0.0080(4) -0.0054(3) N1 0.0476(15) 0.0456(14) 0.0763(19) 0.0165(14) 0.0239(13) 0.0109(12) N2 0.0408(14) 0.0577(15) 0.0472(14) 0.0117(12) 0.0054(11) 0.0052(12) N3 0.0410(13) 0.0413(13) 0.0478(14) 0.0001(11) 0.0038(11) 0.0015(11) C1 0.0300(14) 0.0419(15) 0.0417(15) 0.0032(12) 0.0089(11) 0.0056(11) C2 0.0327(15) 0.0546(17) 0.0409(15) 0.0061(13) 0.0100(12) 0.0057(12) C3 0.0356(16) 0.066(2) 0.0458(17) -0.0136(15) 0.0114(13) -0.0026(14) C4 0.0436(17) 0.0411(16) 0.066(2) -0.0067(15) 0.0202(15) 0.0011(13) C5 0.0354(15) 0.0416(15) 0.0595(18) 0.0084(13) 0.0197(13) 0.0109(12) C6 0.0320(15) 0.0569(18) 0.0576(18) 0.0067(14) 0.0063(13) -0.0005(13) C7 0.0452(18) 0.083(2) 0.0556(19) 0.0295(17) 0.0081(14) 0.0074(16) C8 0.052(2) 0.121(3) 0.051(2) -0.027(2) -0.0001(16) -0.007(2) C9 0.062(2) 0.0398(18) 0.123(3) -0.0142(19) 0.032(2) -0.0027(15) C10 0.0493(19) 0.068(2) 0.085(2) 0.0359(19) 0.0242(17) 0.0263(16) C11 0.0365(16) 0.0399(16) 0.0636(19) 0.0045(15) 0.0128(14) 0.0051(12) C12 0.0503(19) 0.0514(19) 0.102(3) 0.030(2) 0.0314(19) 0.0214(15) C13 0.056(2) 0.059(2) 0.133(4) 0.031(2) 0.034(2) 0.0190(18) C14 0.065(3) 0.070(3) 0.171(5) 0.061(3) 0.035(3) 0.027(2) C15 0.070(3) 0.098(4) 0.156(5) 0.078(4) 0.040(3) 0.041(3) C16 0.073(3) 0.094(3) 0.107(3) 0.058(3) 0.024(2) 0.038(2) C17 0.070(2) 0.074(2) 0.081(3) 0.036(2) 0.025(2) 0.038(2) C18 0.089(3) 0.074(3) 0.081(3) 0.023(2) 0.007(2) 0.016(2) C19 0.069(3) 0.063(2) 0.169(5) 0.012(3) 0.029(3) -0.011(2) C20 0.0369(16) 0.0502(17) 0.0397(15) -0.0001(13) 0.0050(12) 0.0008(13) C21 0.0323(15) 0.066(2) 0.0632(19) 0.0314(16) 0.0045(14) 0.0018(14) C22 0.0433(18) 0.069(2) 0.085(3) 0.0275(19) 0.0046(17) 0.0142(16) C23 0.048(2) 0.076(2) 0.120(4) 0.048(2) 0.011(2) 0.0140(18) C24 0.049(2) 0.105(3) 0.136(4) 0.086(3) 0.000(3) 0.004(2) C25 0.048(2) 0.123(4) 0.090(3) 0.066(3) -0.015(2) -0.018(2) C26 0.0468(19) 0.085(2) 0.066(2) 0.036(2) -0.0058(16) -0.0177(17) C27 0.074(3) 0.114(3) 0.065(2) 0.020(2) -0.014(2) -0.021(2) C28 0.091(3) 0.107(3) 0.089(3) -0.011(3) -0.004(2) 0.053(3) C29 0.0385(15) 0.0384(15) 0.0425(15) 0.0071(13) 0.0089(12) 0.0076(12) C30 0.0328(15) 0.0476(16) 0.0473(16) -0.0026(13) 0.0035(12) 0.0014(12) C31 0.0456(17) 0.0601(19) 0.0519(18) 0.0023(15) 0.0047(14) 0.0122(14) C32 0.0392(18) 0.090(3) 0.0537(19) -0.0067(18) -0.0045(14) -0.0044(17) C33 0.060(2) 0.068(2) 0.070(2) -0.0030(19) 0.0088(18) -0.0193(18) C34 0.065(2) 0.0529(19) 0.076(2) 0.0085(17) 0.0128(19) -0.0122(16) C35 0.0462(18) 0.0471(17) 0.0614(19) 0.0049(15) 0.0092(15) -0.0038(13) C36 0.075(3) 0.069(2) 0.085(3) 0.029(2) -0.007(2) 0.0007(19) C37 0.088(3) 0.081(3) 0.067(2) 0.016(2) -0.006(2) 0.023(2) Cl99 0.0374(6) 0.0482(6) 0.0447(5) 0.0034(4) 0.0076(4) 0.0053(4) C99 0.0374(6) 0.0482(6) 0.0447(5) 0.0034(4) 0.0076(4) 0.0053(4) Cl3 0.058(5) 0.073(6) 0.038(4) -0.001(4) 0.006(3) 0.034(4) Cl2 0.091(7) 0.057(5) 0.046(5) 0.013(4) 0.031(4) 0.019(4) B1 0.105(15) 0.084(7) 0.029(10) 0.016(8) -0.024(6) 0.034(10) F1 0.179(10) 0.144(9) 0.167(9) -0.045(7) -0.047(7) -0.008(7) F2 0.121(4) 0.084(3) 0.079(3) 0.008(3) 0.002(3) 0.047(3) F3 0.148(7) 0.055(3) 0.069(3) 0.008(2) -0.023(3) 0.022(3) F4 0.136(6) 0.187(7) 0.090(4) 0.050(4) 0.016(3) -0.025(5) B1' 0.105(15) 0.084(7) 0.029(10) 0.016(8) -0.024(6) 0.034(10) F1' 0.070(6) 0.122(9) 0.57(3) 0.078(16) -0.006(13) 0.033(6) F2' 0.140(7) 0.102(6) 0.053(3) 0.030(4) -0.012(4) -0.009(5) F3' 0.155(7) 0.108(5) 0.116(5) 0.030(4) 0.049(5) 0.038(4) F4' 0.277(14) 0.134(8) 0.41(2) 0.194(12) 0.149(15) 0.112(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 C29 2.086(3) . ? Mo1 C11 2.114(3) . ? Mo1 C20 2.138(3) . ? Mo1 C4 2.310(3) . ? Mo1 C3 2.344(3) . ? Mo1 C5 2.357(3) . ? Mo1 C2 2.397(3) . ? Mo1 C1 2.426(3) . ? Mo1 Cl1 2.4764(10) . ? Mo1 C99 2.48(6) . ? Mo1 Cl99 2.4868(13) . ? N1 C11 1.154(4) . ? N1 C12 1.428(4) . ? N2 C20 1.148(4) . ? N2 C21 1.419(4) . ? N3 C29 1.155(3) . ? N3 C30 1.414(3) . ? C1 C5 1.415(4) . ? C1 C2 1.430(4) . ? C1 C6 1.487(4) . ? C2 C3 1.426(4) . ? C2 C7 1.488(4) . ? C3 C4 1.422(5) . ? C3 C8 1.500(4) . ? C4 C5 1.434(4) . ? C4 C9 1.509(4) . ? C5 C10 1.499(4) . ? C12 C13 1.361(5) . ? C12 C17 1.421(5) . ? C13 C14 1.438(6) . ? C13 C19 1.482(7) . ? C14 C15 1.365(7) . ? C15 C16 1.356(6) . ? C16 C17 1.392(5) . ? C17 C18 1.476(5) . ? C21 C26 1.384(4) . ? C21 C22 1.403(5) . ? C22 C23 1.393(5) . ? C22 C28 1.480(5) . ? C23 C24 1.358(6) . ? C24 C25 1.362(6) . ? C25 C26 1.412(5) . ? C26 C27 1.490(6) . ? C30 C31 1.390(4) . ? C30 C35 1.394(4) . ? C31 C32 1.410(4) . ? C31 C37 1.476(5) . ? C32 C33 1.368(5) . ? C33 C34 1.363(5) . ? C34 C35 1.384(4) . ? C35 C36 1.488(5) . ? C99 Cl3 1.75(5) . ? C99 Cl2 1.88(6) . ? B1 F1 1.00(2) . ? B1 F2 1.44(3) . ? B1 F3 1.531(16) . ? B1 F4 1.54(3) . ? B1' F1' 0.93(3) . ? B1' F4' 1.34(3) . ? B1' F3' 1.57(4) . ? B1' F2' 1.73(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 C29 Mo1 C11 91.49(11) . . ? C29 Mo1 C20 91.84(10) . . ? C11 Mo1 C20 151.15(11) . . ? C29 Mo1 C4 120.87(10) . . ? C11 Mo1 C4 79.87(12) . . ? C20 Mo1 C4 122.02(12) . . ? C29 Mo1 C3 125.52(10) . . ? C11 Mo1 C3 114.25(12) . . ? C20 Mo1 C3 86.58(12) . . ? C4 Mo1 C3 35.58(12) . . ? C29 Mo1 C5 85.23(10) . . ? C11 Mo1 C5 75.95(10) . . ? C20 Mo1 C5 132.89(10) . . ? C4 Mo1 C5 35.78(10) . . ? C3 Mo1 C5 58.86(11) . . ? C29 Mo1 C2 92.30(10) . . ? C11 Mo1 C2 133.22(10) . . ? C20 Mo1 C2 75.24(10) . . ? C4 Mo1 C2 58.59(11) . . ? C3 Mo1 C2 34.98(10) . . ? C5 Mo1 C2 57.98(10) . . ? C29 Mo1 C1 69.30(9) . . ? C11 Mo1 C1 106.53(10) . . ? C20 Mo1 C1 101.44(10) . . ? C4 Mo1 C1 58.18(9) . . ? C3 Mo1 C1 57.86(9) . . ? C5 Mo1 C1 34.37(9) . . ? C2 Mo1 C1 34.49(9) . . ? C29 Mo1 Cl1 153.67(7) . . ? C11 Mo1 Cl1 82.76(8) . . ? C20 Mo1 Cl1 81.64(8) . . ? C4 Mo1 Cl1 83.51(8) . . ? C3 Mo1 Cl1 79.76(7) . . ? C5 Mo1 Cl1 117.78(7) . . ? C2 Mo1 Cl1 110.36(7) . . ? C1 Mo1 Cl1 136.95(6) . . ? C29 Mo1 C99 83.5(11) . . ? C11 Mo1 C99 73.0(13) . . ? C20 Mo1 C99 79.0(13) . . ? C4 Mo1 C99 144.0(12) . . ? C3 Mo1 C99 148.2(12) . . ? C5 Mo1 C99 146.5(14) . . ? C2 Mo1 C99 153.7(13) . . ? C1 Mo1 C99 152.8(12) . . ? Cl1 Mo1 C99 70.2(11) . . ? C29 Mo1 Cl99 73.88(8) . . ? C11 Mo1 Cl99 76.91(8) . . ? C20 Mo1 Cl99 76.54(8) . . ? C4 Mo1 Cl99 152.85(8) . . ? C3 Mo1 Cl99 155.11(8) . . ? C5 Mo1 Cl99 145.05(8) . . ? C2 Mo1 Cl99 148.04(7) . . ? C1 Mo1 Cl99 143.05(6) . . ? Cl1 Mo1 Cl99 79.80(3) . . ? C99 Mo1 Cl99 10.1(11) . . ? C11 N1 C12 171.5(3) . . ? C20 N2 C21 173.0(3) . . ? C29 N3 C30 166.7(3) . . ? C5 C1 C2 108.2(2) . . ? C5 C1 C6 126.2(3) . . ? C2 C1 C6 124.4(3) . . ? C5 C1 Mo1 70.13(14) . . ? C2 C1 Mo1 71.62(14) . . ? C6 C1 Mo1 133.88(18) . . ? C3 C2 C1 107.9(3) . . ? C3 C2 C7 126.3(3) . . ? C1 C2 C7 125.0(3) . . ? C3 C2 Mo1 70.50(16) . . ? C1 C2 Mo1 73.89(15) . . ? C7 C2 Mo1 129.7(2) . . ? C4 C3 C2 108.0(3) . . ? C4 C3 C8 126.8(3) . . ? C2 C3 C8 124.5(3) . . ? C4 C3 Mo1 70.88(16) . . ? C2 C3 Mo1 74.51(15) . . ? C8 C3 Mo1 128.0(2) . . ? C3 C4 C5 107.9(3) . . ? C3 C4 C9 124.6(3) . . ? C5 C4 C9 126.8(3) . . ? C3 C4 Mo1 73.55(16) . . ? C5 C4 Mo1 73.90(15) . . ? C9 C4 Mo1 125.4(2) . . ? C1 C5 C4 108.0(3) . . ? C1 C5 C10 123.7(3) . . ? C4 C5 C10 127.8(3) . . ? C1 C5 Mo1 75.50(15) . . ? C4 C5 Mo1 70.32(15) . . ? C10 C5 Mo1 126.6(2) . . ? N1 C11 Mo1 174.4(2) . . ? C13 C12 C17 126.9(4) . . ? C13 C12 N1 117.3(4) . . ? C17 C12 N1 115.7(3) . . ? C12 C13 C14 115.7(5) . . ? C12 C13 C19 122.7(4) . . ? C14 C13 C19 121.5(4) . . ? C15 C14 C13 117.8(5) . . ? C16 C15 C14 124.9(5) . . ? C15 C16 C17 120.4(5) . . ? C16 C17 C12 114.3(4) . . ? C16 C17 C18 123.7(4) . . ? C12 C17 C18 122.0(3) . . ? N2 C20 Mo1 169.4(2) . . ? C26 C21 C22 124.5(3) . . ? C26 C21 N2 117.8(3) . . ? C22 C21 N2 117.6(3) . . ? C23 C22 C21 116.1(4) . . ? C23 C22 C28 121.4(4) . . ? C21 C22 C28 122.4(3) . . ? C24 C23 C22 120.8(4) . . ? C23 C24 C25 122.1(4) . . ? C24 C25 C26 120.6(4) . . ? C21 C26 C25 115.7(4) . . ? C21 C26 C27 121.8(3) . . ? C25 C26 C27 122.4(4) . . ? N3 C29 Mo1 178.7(2) . . ? C31 C30 C35 123.5(3) . . ? C31 C30 N3 119.2(3) . . ? C35 C30 N3 117.3(3) . . ? C30 C31 C32 116.1(3) . . ? C30 C31 C37 121.6(3) . . ? C32 C31 C37 122.2(3) . . ? C33 C32 C31 121.0(3) . . ? C34 C33 C32 120.9(3) . . ? C33 C34 C35 121.1(3) . . ? C34 C35 C30 117.3(3) . . ? C34 C35 C36 121.1(3) . . ? C30 C35 C36 121.6(3) . . ? Cl3 C99 Cl2 102(2) . . ? Cl3 C99 Mo1 111(3) . . ? Cl2 C99 Mo1 105(2) . . ? F1 B1 F2 119(2) . . ? F1 B1 F3 127(3) . . ? F2 B1 F3 96.8(9) . . ? F1 B1 F4 120.9(18) . . ? F2 B1 F4 94.6(18) . . ? F3 B1 F4 90.7(14) . . ? F1' B1' F4' 145(4) . . ? F1' B1' F3' 117(3) . . ? F4' B1' F3' 97(2) . . ? F1' B1' F2' 93(3) . . ? F4' B1' F2' 84.9(12) . . ? F3' B1' F2' 77.8(17) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.455 _refine_diff_density_min -0.476 _refine_diff_density_rms 0.055 #===END data_10 _database_code_CSD 155031 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H51 B2 F9 Mo N4' _chemical_formula_weight 948.47 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' 'B' 'B' 0.0013 0.0007 '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' 'F' 'F' 0.0171 0.0103 '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 20.315(3) _cell_length_b 13.973(2) _cell_length_c 16.0458(17) _cell_angle_alpha 90.00 _cell_angle_beta 100.087(8) _cell_angle_gamma 90.00 _cell_volume 4484.4(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 211 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 0.367 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.796 _exptl_absorpt_correction_T_max 0.915 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Siemens CCD Area Diffractometer' _diffrn_measurement_method '/w scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 23740 _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_sigmaI/netI 0.0264 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7896 _reflns_number_gt 6773 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0721P)^2^+8.8145P] 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 7896 _refine_ls_number_parameters 583 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.1310 _refine_ls_wR_factor_gt 0.1251 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.272796(13) 0.970140(18) 0.307563(16) 0.01991(11) Uani 1 1 d . . . N1 N 0.36993(14) 1.1399(2) 0.40014(17) 0.0282(6) Uani 1 1 d . . . N2 N 0.28079(14) 1.0545(2) 0.11785(18) 0.0278(6) Uani 1 1 d . . . N3 N 0.12075(14) 0.9092(2) 0.21776(17) 0.0270(6) Uani 1 1 d . . . N4 N 0.19378(15) 0.9942(2) 0.46722(18) 0.0279(6) Uani 1 1 d . . . C1 C 0.33927(16) 1.0774(2) 0.3657(2) 0.0252(7) Uani 1 1 d . . . C2 C 0.40622(17) 1.2150(2) 0.4445(2) 0.0287(7) Uani 1 1 d . . . C3 C 0.41211(18) 1.2162(3) 0.5326(2) 0.0325(8) Uani 1 1 d . . . C4 C 0.3794(2) 1.1418(3) 0.5782(2) 0.0440(10) Uani 1 1 d . . . H4A H 0.3760 1.1651 0.6349 0.066 Uiso 1 1 calc R . . H4B H 0.4063 1.0831 0.5831 0.066 Uiso 1 1 calc R . . H4C H 0.3346 1.1283 0.5467 0.066 Uiso 1 1 calc R . . C5 C 0.4494(2) 1.2901(3) 0.5744(2) 0.0425(9) Uani 1 1 d . . . H5A H 0.4546 1.2942 0.6343 0.051 Uiso 1 1 calc R . . C6 C 0.4794(2) 1.3582(3) 0.5308(3) 0.0522(11) Uani 1 1 d . . . H6A H 0.5062 1.4069 0.5610 0.063 Uiso 1 1 calc R . . C7 C 0.4706(2) 1.3556(3) 0.4433(3) 0.0535(12) Uani 1 1 d . . . H7A H 0.4898 1.4043 0.4139 0.064 Uiso 1 1 calc R . . C8 C 0.4340(2) 1.2831(3) 0.3982(2) 0.0402(9) Uani 1 1 d . . . C9 C 0.4226(3) 1.2802(4) 0.3028(3) 0.0643(15) Uani 1 1 d . . . H9A H 0.4375 1.3406 0.2812 0.096 Uiso 1 1 calc R . . H9B H 0.3749 1.2710 0.2810 0.096 Uiso 1 1 calc R . . H9C H 0.4481 1.2271 0.2843 0.096 Uiso 1 1 calc R . . C10 C 0.28395(17) 1.0206(2) 0.1838(2) 0.0252(7) Uani 1 1 d . . . C11 C 0.27015(18) 1.1031(2) 0.0396(2) 0.0290(7) Uani 1 1 d . . . C12 C 0.2920(2) 1.0606(3) -0.0297(2) 0.0359(8) Uani 1 1 d . . . C13 C 0.3261(3) 0.9657(3) -0.0230(3) 0.0498(11) Uani 1 1 d . . . H13A H 0.3407 0.9508 -0.0765 0.075 Uiso 1 1 calc R . . H13B H 0.2949 0.9163 -0.0107 0.075 Uiso 1 1 calc R . . H13C H 0.3649 0.9676 0.0228 0.075 Uiso 1 1 calc R . . C14 C 0.2788(2) 1.1108(3) -0.1063(2) 0.0422(10) Uani 1 1 d . . . H14A H 0.2926 1.0845 -0.1550 0.051 Uiso 1 1 calc R . . C15 C 0.2462(2) 1.1972(3) -0.1122(3) 0.0423(10) Uani 1 1 d . . . H15A H 0.2376 1.2298 -0.1650 0.051 Uiso 1 1 calc R . . C16 C 0.22573(19) 1.2372(3) -0.0425(3) 0.0398(9) Uani 1 1 d . . . H16A H 0.2035 1.2973 -0.0478 0.048 Uiso 1 1 calc R . . C17 C 0.23715(18) 1.1907(3) 0.0360(2) 0.0339(8) Uani 1 1 d . . . C18 C 0.2158(2) 1.2344(3) 0.1125(3) 0.0465(10) Uani 1 1 d . . . H18A H 0.2008 1.1838 0.1471 0.070 Uiso 1 1 calc R . . H18B H 0.1791 1.2793 0.0945 0.070 Uiso 1 1 calc R . . H18C H 0.2537 1.2685 0.1459 0.070 Uiso 1 1 calc R . . C19 C 0.17651(16) 0.9201(2) 0.2462(2) 0.0243(7) Uani 1 1 d . . . C20 C 0.05229(17) 0.9106(3) 0.1823(2) 0.0291(7) Uani 1 1 d . . . C21 C 0.02921(18) 0.9907(3) 0.1344(2) 0.0335(8) Uani 1 1 d . . . C22 C 0.0760(2) 1.0701(3) 0.1191(3) 0.0424(9) Uani 1 1 d . . . H22A H 0.0967 1.0980 0.1734 0.064 Uiso 1 1 calc R . . H22B H 0.0508 1.1196 0.0837 0.064 Uiso 1 1 calc R . . H22C H 0.1108 1.0443 0.0903 0.064 Uiso 1 1 calc R . . C23 C -0.03913(19) 0.9940(3) 0.1020(3) 0.0401(9) Uani 1 1 d . . . H23A H -0.0574 1.0478 0.0697 0.048 Uiso 1 1 calc R . . C24 C -0.08032(19) 0.9196(3) 0.1165(3) 0.0421(9) Uani 1 1 d . . . H24A H -0.1266 0.9223 0.0931 0.051 Uiso 1 1 calc R . . C25 C -0.05562(19) 0.8416(3) 0.1643(2) 0.0389(9) Uani 1 1 d . . . H25A H -0.0852 0.7916 0.1736 0.047 Uiso 1 1 calc R . . C26 C 0.01199(17) 0.8346(3) 0.1991(2) 0.0315(8) Uani 1 1 d . . . C27 C 0.04036(19) 0.7509(3) 0.2522(2) 0.0389(9) Uani 1 1 d . . . H27A H 0.0038 0.7103 0.2642 0.058 Uiso 1 1 calc R . . H27B H 0.0665 0.7741 0.3056 0.058 Uiso 1 1 calc R . . H27C H 0.0693 0.7137 0.2216 0.058 Uiso 1 1 calc R . . C28 C 0.22635(17) 0.9767(2) 0.4176(2) 0.0253(7) Uani 1 1 d . . . C29 C 0.14726(19) 1.0253(2) 0.5169(2) 0.0334(8) Uani 1 1 d . . . C30 C 0.0884(2) 1.0663(3) 0.4728(3) 0.0437(10) Uani 1 1 d . . . C31 C 0.0731(2) 1.0680(4) 0.3788(3) 0.0527(11) Uani 1 1 d . . . H31A H 0.0704 1.0023 0.3572 0.079 Uiso 1 1 calc R . . H31B H 0.1086 1.1024 0.3570 0.079 Uiso 1 1 calc R . . H31C H 0.0303 1.1005 0.3602 0.079 Uiso 1 1 calc R . . C32 C 0.0442(2) 1.1036(3) 0.5222(4) 0.0619(14) Uani 1 1 d . . . H32A H 0.0039 1.1330 0.4953 0.074 Uiso 1 1 calc R . . C33 C 0.0581(3) 1.0985(4) 0.6082(4) 0.0710(17) Uani 1 1 d . . . H33A H 0.0276 1.1253 0.6405 0.085 Uiso 1 1 calc R . . C34 C 0.1161(3) 1.0545(3) 0.6497(3) 0.0592(14) Uani 1 1 d . . . H34A H 0.1239 1.0498 0.7097 0.071 Uiso 1 1 calc R . . C35 C 0.1631(2) 1.0170(3) 0.6046(3) 0.0416(10) Uani 1 1 d . . . C36 C 0.2266(3) 0.9716(3) 0.6463(3) 0.0536(12) Uani 1 1 d . . . H36A H 0.2304 0.9764 0.7079 0.080 Uiso 1 1 calc R . . H36B H 0.2645 1.0044 0.6286 0.080 Uiso 1 1 calc R . . H36C H 0.2268 0.9040 0.6300 0.080 Uiso 1 1 calc R . . C37 C 0.31119(17) 0.8333(2) 0.2514(2) 0.0274(7) Uani 1 1 d . . . C38 C 0.2930(2) 0.7993(3) 0.1616(2) 0.0403(9) Uani 1 1 d . . . H38A H 0.3101 0.7343 0.1571 0.060 Uiso 1 1 calc R . . H38B H 0.3129 0.8421 0.1244 0.060 Uiso 1 1 calc R . . H38C H 0.2443 0.7994 0.1446 0.060 Uiso 1 1 calc R . . C39 C 0.36817(17) 0.8887(3) 0.2858(2) 0.0333(8) Uani 1 1 d . . . C40 C 0.4218(2) 0.9243(4) 0.2405(3) 0.0547(12) Uani 1 1 d . . . H40A H 0.4602 0.8807 0.2511 0.082 Uiso 1 1 calc R . . H40B H 0.4359 0.9884 0.2611 0.082 Uiso 1 1 calc R . . H40C H 0.4045 0.9271 0.1795 0.082 Uiso 1 1 calc R . . C41 C 0.37282(17) 0.8902(2) 0.3756(2) 0.0321(8) Uani 1 1 d . . . C42 C 0.4308(2) 0.9255(3) 0.4393(3) 0.0534(12) Uani 1 1 d . . . H42A H 0.4617 0.8725 0.4568 0.080 Uiso 1 1 calc R . . H42B H 0.4144 0.9510 0.4888 0.080 Uiso 1 1 calc R . . H42C H 0.4542 0.9762 0.4139 0.080 Uiso 1 1 calc R . . C43 C 0.31836(17) 0.8374(2) 0.3958(2) 0.0280(7) Uani 1 1 d . . . C44 C 0.3101(2) 0.8106(3) 0.4837(2) 0.0401(9) Uani 1 1 d . . . H44A H 0.3397 0.7568 0.5035 0.060 Uiso 1 1 calc R . . H44B H 0.2636 0.7920 0.4836 0.060 Uiso 1 1 calc R . . H44C H 0.3216 0.8655 0.5215 0.060 Uiso 1 1 calc R . . C45 C 0.28011(17) 0.8015(2) 0.3196(2) 0.0261(7) Uani 1 1 d . . . C46 C 0.22540(19) 0.7292(3) 0.3143(2) 0.0362(8) Uani 1 1 d . . . H46A H 0.2449 0.6652 0.3246 0.054 Uiso 1 1 calc R . . H46B H 0.1977 0.7313 0.2578 0.054 Uiso 1 1 calc R . . H46C H 0.1977 0.7436 0.3569 0.054 Uiso 1 1 calc R . . F1 F 0.21766(9) 1.08781(13) 0.29005(11) 0.0266(4) Uani 1 1 d . . . B1 B 0.58126(19) 1.4074(2) 0.75734(18) 0.0578(15) Uani 1 1 d . . . F3A F 0.5193(2) 1.4468(5) 0.73700(19) 0.323(17) Uani 0.517(11) 1 calc PR . . F4A F 0.5778(3) 1.3123(2) 0.7390(2) 0.082(3) Uani 0.517(11) 1 calc PR . . F5A F 0.6234(3) 1.4508(4) 0.71197(18) 0.347(18) Uani 0.517(11) 1 calc PR . . F3B F 0.6277(2) 1.3598(4) 0.7216(2) 0.150(7) Uani 0.483(11) 1 calc PR . . F4B F 0.5692(4) 1.4943(2) 0.71966(19) 0.198(9) Uani 0.483(11) 1 calc PR . . F5B F 0.5236(2) 1.3558(5) 0.74665(18) 0.60(4) Uani 0.483(11) 1 calc PR . . F2 F 0.6036(3) 1.4191(3) 0.8382(2) 0.1201(16) Uani 1 1 d . . . B2 B 0.1197(2) 0.7344(3) 0.5151(3) 0.0389(10) Uani 1 1 d . . . F6 F 0.05425(13) 0.7074(2) 0.4936(2) 0.0673(8) Uani 1 1 d . . . F7 F 0.13167(16) 0.7702(2) 0.59674(16) 0.0674(8) Uani 1 1 d . . . F8 F 0.16026(14) 0.6553(2) 0.5097(2) 0.0743(9) Uani 1 1 d . . . F9 F 0.13322(18) 0.8040(2) 0.45998(18) 0.0767(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.01828(16) 0.02103(16) 0.02009(16) -0.00195(10) 0.00247(11) 0.00038(10) N1 0.0241(14) 0.0331(16) 0.0272(15) -0.0035(13) 0.0040(12) -0.0018(13) N2 0.0305(16) 0.0258(14) 0.0273(16) -0.0007(12) 0.0052(12) -0.0006(12) N3 0.0255(16) 0.0273(15) 0.0277(14) -0.0038(12) 0.0028(12) -0.0008(12) N4 0.0321(16) 0.0235(14) 0.0301(15) 0.0022(12) 0.0108(13) 0.0012(12) C1 0.0237(17) 0.0292(18) 0.0229(16) -0.0015(14) 0.0047(13) -0.0009(14) C2 0.0256(17) 0.0316(18) 0.0273(17) -0.0083(14) 0.0004(14) -0.0056(14) C3 0.0327(19) 0.0361(19) 0.0275(17) -0.0034(15) 0.0024(15) -0.0013(16) C4 0.060(3) 0.045(2) 0.0276(19) -0.0006(17) 0.0075(18) -0.008(2) C5 0.050(2) 0.046(2) 0.0291(19) -0.0095(17) -0.0002(17) -0.0071(19) C6 0.056(3) 0.050(3) 0.047(2) -0.015(2) -0.002(2) -0.023(2) C7 0.061(3) 0.052(3) 0.048(2) -0.003(2) 0.010(2) -0.028(2) C8 0.043(2) 0.047(2) 0.0306(19) -0.0046(17) 0.0063(16) -0.0163(18) C9 0.076(3) 0.086(4) 0.032(2) -0.002(2) 0.012(2) -0.037(3) C10 0.0242(17) 0.0232(16) 0.0282(18) -0.0051(14) 0.0043(13) -0.0008(13) C11 0.0308(18) 0.0276(17) 0.0278(17) 0.0039(14) 0.0031(14) -0.0051(14) C12 0.044(2) 0.0350(19) 0.0286(18) 0.0040(15) 0.0049(16) -0.0057(17) C13 0.077(3) 0.042(2) 0.034(2) 0.0003(18) 0.022(2) 0.010(2) C14 0.053(2) 0.046(2) 0.0278(19) 0.0034(17) 0.0067(17) -0.0116(19) C15 0.046(2) 0.041(2) 0.037(2) 0.0147(18) -0.0004(18) -0.0121(19) C16 0.036(2) 0.0317(19) 0.050(2) 0.0134(17) 0.0011(18) -0.0027(16) C17 0.0315(19) 0.0288(18) 0.041(2) 0.0062(16) 0.0060(16) -0.0034(15) C18 0.057(3) 0.032(2) 0.056(3) 0.0052(18) 0.024(2) 0.0055(19) C19 0.0260(19) 0.0221(16) 0.0249(16) -0.0010(13) 0.0048(14) -0.0010(13) C20 0.0210(17) 0.0358(19) 0.0298(17) -0.0072(15) 0.0021(14) -0.0015(14) C21 0.0298(19) 0.037(2) 0.0320(19) -0.0025(16) 0.0020(15) -0.0018(16) C22 0.036(2) 0.042(2) 0.045(2) 0.0064(18) -0.0018(18) -0.0052(18) C23 0.030(2) 0.047(2) 0.040(2) 0.0006(18) -0.0041(16) 0.0018(17) C24 0.0246(19) 0.057(3) 0.042(2) -0.0022(19) -0.0005(16) -0.0017(18) C25 0.0275(19) 0.049(2) 0.041(2) -0.0072(18) 0.0064(16) -0.0081(17) C26 0.0281(18) 0.0369(19) 0.0293(18) -0.0068(15) 0.0040(14) -0.0051(15) C27 0.032(2) 0.042(2) 0.042(2) 0.0016(17) 0.0049(16) -0.0057(17) C28 0.0263(17) 0.0226(16) 0.0265(17) 0.0004(13) 0.0033(14) 0.0013(13) C29 0.039(2) 0.0248(18) 0.041(2) -0.0032(15) 0.0214(17) -0.0006(15) C30 0.039(2) 0.037(2) 0.060(3) -0.0032(19) 0.021(2) 0.0008(18) C31 0.035(2) 0.062(3) 0.062(3) 0.009(2) 0.008(2) 0.012(2) C32 0.047(3) 0.054(3) 0.094(4) -0.013(3) 0.038(3) 0.006(2) C33 0.065(3) 0.066(3) 0.098(4) -0.033(3) 0.060(3) -0.012(3) C34 0.085(4) 0.048(3) 0.056(3) -0.017(2) 0.047(3) -0.019(3) C35 0.060(3) 0.031(2) 0.040(2) -0.0037(16) 0.026(2) -0.0092(18) C36 0.081(4) 0.047(3) 0.033(2) 0.0058(18) 0.013(2) 0.002(2) C37 0.0331(18) 0.0257(17) 0.0241(16) -0.0014(13) 0.0070(14) 0.0114(14) C38 0.060(3) 0.036(2) 0.0252(18) -0.0047(16) 0.0073(17) 0.0133(19) C39 0.0239(18) 0.0348(19) 0.042(2) 0.0048(16) 0.0091(15) 0.0116(15) C40 0.030(2) 0.065(3) 0.073(3) 0.017(3) 0.021(2) 0.010(2) C41 0.0240(17) 0.0292(18) 0.039(2) -0.0019(15) -0.0051(15) 0.0080(14) C42 0.038(2) 0.047(2) 0.064(3) -0.003(2) -0.023(2) 0.0067(19) C43 0.0318(18) 0.0243(16) 0.0265(17) -0.0017(13) 0.0015(14) 0.0103(14) C44 0.056(3) 0.038(2) 0.0260(18) 0.0040(16) 0.0038(17) 0.0143(18) C45 0.0294(18) 0.0223(16) 0.0255(17) 0.0001(13) 0.0014(14) 0.0075(13) C46 0.039(2) 0.0254(18) 0.042(2) 0.0009(16) 0.0009(17) 0.0005(16) F1 0.0262(10) 0.0244(9) 0.0285(10) -0.0023(8) 0.0034(8) 0.0024(8) B1 0.055(3) 0.055(3) 0.052(3) -0.009(3) -0.025(3) 0.011(3) F3A 0.215(17) 0.224(16) 0.43(3) -0.209(18) -0.225(19) 0.155(14) F4A 0.083(5) 0.043(3) 0.101(5) -0.035(3) -0.037(4) 0.029(3) F5A 0.66(5) 0.28(3) 0.113(11) 0.041(13) 0.10(2) -0.16(3) F3B 0.164(11) 0.216(13) 0.090(6) 0.066(7) 0.076(7) 0.157(11) F4B 0.350(19) 0.209(11) 0.065(5) 0.089(7) 0.118(8) 0.251(13) F5B 0.164(17) 1.25(10) 0.35(3) -0.60(5) -0.091(19) 0.13(4) F2 0.214(5) 0.088(3) 0.0467(18) -0.0050(18) -0.008(2) 0.007(3) B2 0.036(2) 0.039(2) 0.042(2) -0.006(2) 0.0084(19) -0.0037(19) F6 0.0395(14) 0.0580(16) 0.101(2) -0.0114(15) 0.0038(14) -0.0054(12) F7 0.085(2) 0.0729(19) 0.0419(14) -0.0115(13) 0.0048(14) 0.0021(16) F8 0.0524(16) 0.0699(19) 0.093(2) -0.0300(17) -0.0088(15) 0.0184(14) F9 0.115(3) 0.0617(18) 0.0628(18) -0.0066(14) 0.0417(18) -0.0305(18) _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 F1 1.9816(18) . ? Mo1 C1 2.121(3) . ? Mo1 C28 2.145(3) . ? Mo1 C19 2.147(3) . ? Mo1 C10 2.156(3) . ? Mo1 C37 2.307(3) . ? Mo1 C39 2.325(3) . ? Mo1 C45 2.367(3) . ? Mo1 C41 2.406(3) . ? Mo1 C43 2.418(3) . ? N1 C1 1.155(4) . ? N1 C2 1.403(4) . ? N2 C10 1.151(4) . ? N2 C11 1.411(4) . ? N3 C19 1.155(4) . ? N3 C20 1.408(4) . ? N4 C28 1.147(4) . ? N4 C29 1.407(4) . ? C2 C8 1.388(5) . ? C2 C3 1.397(5) . ? C3 C5 1.384(5) . ? C3 C4 1.493(5) . ? C5 C6 1.384(6) . ? C6 C7 1.383(6) . ? C7 C8 1.384(6) . ? C8 C9 1.507(5) . ? C11 C17 1.393(5) . ? C11 C12 1.399(5) . ? C12 C14 1.399(5) . ? C12 C13 1.491(6) . ? C14 C15 1.373(6) . ? C15 C16 1.379(6) . ? C16 C17 1.400(5) . ? C17 C18 1.500(5) . ? C20 C21 1.392(5) . ? C20 C26 1.396(5) . ? C21 C23 1.395(5) . ? C21 C22 1.508(5) . ? C23 C24 1.380(6) . ? C24 C25 1.376(6) . ? C25 C26 1.393(5) . ? C26 C27 1.501(5) . ? C29 C35 1.392(6) . ? C29 C30 1.400(6) . ? C30 C32 1.399(6) . ? C30 C31 1.486(6) . ? C32 C33 1.362(8) . ? C33 C34 1.391(8) . ? C34 C35 1.397(6) . ? C35 C36 1.489(7) . ? C37 C39 1.421(5) . ? C37 C45 1.426(5) . ? C37 C38 1.501(5) . ? C39 C41 1.427(5) . ? C39 C40 1.497(5) . ? C41 C43 1.415(5) . ? C41 C42 1.501(5) . ? C43 C45 1.421(5) . ? C43 C44 1.496(5) . ? C45 C46 1.493(5) . ? B1 F2 1.308(4) . ? B2 F6 1.368(5) . ? B2 F9 1.374(5) . ? B2 F7 1.383(5) . ? B2 F8 1.390(5) . ? 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 F1 Mo1 C1 77.09(10) . . ? F1 Mo1 C28 76.22(10) . . ? C1 Mo1 C28 86.87(12) . . ? F1 Mo1 C19 76.00(10) . . ? C1 Mo1 C19 152.93(13) . . ? C28 Mo1 C19 83.97(12) . . ? F1 Mo1 C10 75.27(10) . . ? C1 Mo1 C10 90.71(12) . . ? C28 Mo1 C10 151.21(12) . . ? C19 Mo1 C10 85.31(12) . . ? F1 Mo1 C37 148.61(10) . . ? C1 Mo1 C37 121.65(13) . . ? C28 Mo1 C37 125.79(12) . . ? C19 Mo1 C37 83.93(12) . . ? C10 Mo1 C37 79.30(12) . . ? F1 Mo1 C39 148.20(11) . . ? C1 Mo1 C39 85.92(13) . . ? C28 Mo1 C39 130.00(13) . . ? C19 Mo1 C39 119.21(13) . . ? C10 Mo1 C39 78.31(13) . . ? C37 Mo1 C39 35.73(13) . . ? F1 Mo1 C45 149.71(10) . . ? C1 Mo1 C45 129.92(12) . . ? C28 Mo1 C45 90.36(12) . . ? C19 Mo1 C45 75.67(12) . . ? C10 Mo1 C45 112.67(11) . . ? C37 Mo1 C45 35.50(12) . . ? C39 Mo1 C45 58.86(12) . . ? F1 Mo1 C41 149.40(10) . . ? C1 Mo1 C41 72.92(12) . . ? C28 Mo1 C41 96.01(13) . . ? C19 Mo1 C41 133.33(12) . . ? C10 Mo1 C41 110.67(13) . . ? C37 Mo1 C41 58.41(12) . . ? C39 Mo1 C41 35.06(13) . . ? C45 Mo1 C41 57.67(12) . . ? F1 Mo1 C43 150.30(10) . . ? C1 Mo1 C43 97.79(12) . . ? C28 Mo1 C43 74.28(12) . . ? C19 Mo1 C43 104.10(12) . . ? C10 Mo1 C43 134.38(12) . . ? C37 Mo1 C43 58.13(11) . . ? C39 Mo1 C43 57.92(12) . . ? C45 Mo1 C43 34.54(11) . . ? C41 Mo1 C43 34.10(12) . . ? C1 N1 C2 178.0(3) . . ? C10 N2 C11 172.7(3) . . ? C19 N3 C20 171.6(3) . . ? C28 N4 C29 170.0(3) . . ? N1 C1 Mo1 173.1(3) . . ? C8 C2 C3 124.2(3) . . ? C8 C2 N1 117.9(3) . . ? C3 C2 N1 117.8(3) . . ? C5 C3 C2 116.3(3) . . ? C5 C3 C4 122.3(3) . . ? C2 C3 C4 121.4(3) . . ? C3 C5 C6 121.3(4) . . ? C7 C6 C5 120.4(4) . . ? C6 C7 C8 120.8(4) . . ? C7 C8 C2 116.9(3) . . ? C7 C8 C9 121.7(4) . . ? C2 C8 C9 121.4(3) . . ? N2 C10 Mo1 169.6(3) . . ? C17 C11 C12 123.9(3) . . ? C17 C11 N2 117.2(3) . . ? C12 C11 N2 118.9(3) . . ? C14 C12 C11 116.5(4) . . ? C14 C12 C13 121.6(4) . . ? C11 C12 C13 121.8(3) . . ? C15 C14 C12 121.2(4) . . ? C14 C15 C16 120.7(4) . . ? C15 C16 C17 121.1(4) . . ? C11 C17 C16 116.6(4) . . ? C11 C17 C18 122.0(3) . . ? C16 C17 C18 121.4(3) . . ? N3 C19 Mo1 167.5(3) . . ? C21 C20 C26 124.5(3) . . ? C21 C20 N3 116.6(3) . . ? C26 C20 N3 118.8(3) . . ? C20 C21 C23 116.7(3) . . ? C20 C21 C22 121.4(3) . . ? C23 C21 C22 121.9(4) . . ? C24 C23 C21 120.3(4) . . ? C25 C24 C23 121.2(4) . . ? C24 C25 C26 121.2(4) . . ? C25 C26 C20 116.0(3) . . ? C25 C26 C27 122.4(3) . . ? C20 C26 C27 121.5(3) . . ? N4 C28 Mo1 166.2(3) . . ? C35 C29 C30 124.8(4) . . ? C35 C29 N4 119.2(4) . . ? C30 C29 N4 116.0(3) . . ? C32 C30 C29 116.3(4) . . ? C32 C30 C31 121.9(4) . . ? C29 C30 C31 121.9(4) . . ? C33 C32 C30 121.0(5) . . ? C32 C33 C34 121.0(4) . . ? C33 C34 C35 121.1(5) . . ? C29 C35 C34 115.8(4) . . ? C29 C35 C36 121.2(4) . . ? C34 C35 C36 123.0(4) . . ? C39 C37 C45 108.2(3) . . ? C39 C37 C38 126.3(3) . . ? C45 C37 C38 124.7(3) . . ? C39 C37 Mo1 72.85(19) . . ? C45 C37 Mo1 74.57(18) . . ? C38 C37 Mo1 126.5(2) . . ? C37 C39 C41 107.8(3) . . ? C37 C39 C40 127.2(4) . . ? C41 C39 C40 124.1(4) . . ? C37 C39 Mo1 71.42(19) . . ? C41 C39 Mo1 75.6(2) . . ? C40 C39 Mo1 127.3(3) . . ? C43 C41 C39 107.9(3) . . ? C43 C41 C42 124.5(4) . . ? C39 C41 C42 126.7(4) . . ? C43 C41 Mo1 73.40(19) . . ? C39 C41 Mo1 69.38(19) . . ? C42 C41 Mo1 131.0(3) . . ? C41 C43 C45 108.5(3) . . ? C41 C43 C44 124.6(3) . . ? C45 C43 C44 126.0(3) . . ? C41 C43 Mo1 72.50(19) . . ? C45 C43 Mo1 70.79(18) . . ? C44 C43 Mo1 130.5(2) . . ? C43 C45 C37 107.5(3) . . ? C43 C45 C46 125.2(3) . . ? C37 C45 C46 126.3(3) . . ? C43 C45 Mo1 74.67(19) . . ? C37 C45 Mo1 69.93(18) . . ? C46 C45 Mo1 129.3(2) . . ? F6 B2 F9 109.1(4) . . ? F6 B2 F7 109.9(4) . . ? F9 B2 F7 109.4(4) . . ? F6 B2 F8 109.0(4) . . ? F9 B2 F8 109.6(4) . . ? F7 B2 F8 109.8(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.593 _refine_diff_density_min -0.972 _refine_diff_density_rms 0.081 #===END