Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jason Lynam' _publ_contact_author_address ;Department of Chemistry University of York Heslington York YO10 5DD UK ; _publ_contact_author_email jml12@york.ac.uk _publ_contact_author_phone +44(0)1904432534 _publ_contact_author_fax +44(0)1904432516 loop_ _publ_author_name _publ_author_address J.M.Lynam ;Department of Chemistry University of York Heslington York YO10 5DD UK ; M.Cowley ;Department of Chemistry University of York Heslington York YO10 5DD UK ; A.C.Whitwood ;Department of Chemistry University of York Heslington York YO10 5DD UK ; _publ_section_title ; Transition Metal Vinylidene Complexes as Supramolecular Building Blocks: Nucleobase-Mediated Self-Assembly of Crystals with Hexagonal Symmetry. ; data_jml0534m _database_code_depnum_ccdc_archive 'CCDC 628686' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H35 Mo N2 O2 P2, 0.5(C H2 Cl2), B F4' _chemical_formula_sum 'C39.50 H36 B Cl F4 Mo N2 O2 P2' _chemical_formula_weight 850.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 13.3618(8) _cell_length_b 11.6388(7) _cell_length_c 23.6419(15) _cell_angle_alpha 90.00 _cell_angle_beta 100.4780(10) _cell_angle_gamma 90.00 _cell_volume 3615.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 7245 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 22.55 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1732 _exptl_absorpt_coefficient_mu 0.585 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.873 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS v2.03;(Sheldrick)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22244 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0296 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 22.55 _reflns_number_total 4758 _reflns_number_gt 4027 _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, 1997)' _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^)+(0.0401P)^2^+3.7487P] 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 4758 _refine_ls_number_parameters 486 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0388 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0755 _refine_ls_wR_factor_gt 0.0711 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 C1 C 0.1841(2) 0.1837(3) 0.15461(14) 0.0186(7) Uani 1 1 d . . . C2 C 0.1983(2) 0.2437(3) 0.11029(13) 0.0188(7) Uani 1 1 d . . . H2 H 0.2588 0.2881 0.1143 0.023 Uiso 1 1 calc R . . C3 C -0.0063(2) 0.1801(3) 0.22270(14) 0.0208(8) Uani 1 1 d . . . H3 H -0.0405 0.2504 0.2116 0.025 Uiso 1 1 calc R . . C4 C 0.0430(2) 0.1713(3) 0.28030(14) 0.0217(8) Uani 1 1 d . . . H4 H 0.0421 0.2390 0.3027 0.026 Uiso 1 1 calc R . . C5 C 0.0936(2) 0.0765(3) 0.30969(14) 0.0218(8) Uani 1 1 d . . . H5 H 0.1124 0.0849 0.3502 0.026 Uiso 1 1 calc R . . C6 C 0.1199(2) -0.0278(3) 0.28746(14) 0.0204(8) Uani 1 1 d . . . H6 H 0.1588 -0.0789 0.3141 0.024 Uiso 1 1 calc R . . C7 C 0.0952(2) -0.0665(3) 0.22984(14) 0.0208(8) Uani 1 1 d . . . H7 H 0.1251 -0.1374 0.2220 0.025 Uiso 1 1 calc R . . C8 C 0.0328(2) -0.0144(3) 0.18288(14) 0.0207(8) Uani 1 1 d . . . H8 H 0.0177 -0.0592 0.1488 0.025 Uiso 1 1 calc R . . C9 C -0.0104(2) 0.0965(3) 0.17994(14) 0.0218(8) Uani 1 1 d . . . H9 H -0.0480 0.1175 0.1433 0.026 Uiso 1 1 calc R . . C10 C 0.1284(2) 0.2486(3) 0.05437(13) 0.0177(7) Uani 1 1 d . . . C11 C 0.0690(2) 0.1479(3) 0.03387(13) 0.0197(7) Uani 1 1 d . . . C12 C 0.0024(2) 0.2513(3) -0.05629(14) 0.0181(7) Uani 1 1 d . . . C13 C 0.1177(2) 0.3427(3) 0.02078(13) 0.0203(8) Uani 1 1 d . . . H13 H 0.1543 0.4102 0.0343 0.024 Uiso 1 1 calc R . . C14 C 0.4237(2) 0.1331(3) 0.23981(13) 0.0185(7) Uani 1 1 d . . . H14A H 0.4894 0.0940 0.2535 0.022 Uiso 1 1 calc R . . H14B H 0.4301 0.1770 0.2048 0.022 Uiso 1 1 calc R . . C15 C 0.4032(2) 0.2165(3) 0.28588(13) 0.0168(7) Uani 1 1 d . . . H15A H 0.4500 0.2828 0.2873 0.020 Uiso 1 1 calc R . . H15B H 0.4176 0.1778 0.3238 0.020 Uiso 1 1 calc R . . C16 C 0.3567(2) -0.0956(3) 0.27131(13) 0.0181(7) Uani 1 1 d . . . C17 C 0.3339(2) -0.2078(3) 0.25268(15) 0.0236(8) Uani 1 1 d . . . H17 H 0.3119 -0.2226 0.2129 0.028 Uiso 1 1 calc R . . C18 C 0.3428(3) -0.2967(3) 0.29107(14) 0.0255(8) Uani 1 1 d . . . H18 H 0.3255 -0.3724 0.2777 0.031 Uiso 1 1 calc R . . C19 C 0.3766(3) -0.2780(3) 0.34878(15) 0.0284(9) Uani 1 1 d . . . H19 H 0.3834 -0.3404 0.3751 0.034 Uiso 1 1 calc R . . C20 C 0.4003(3) -0.1685(3) 0.36803(15) 0.0325(9) Uani 1 1 d . . . H20 H 0.4243 -0.1549 0.4078 0.039 Uiso 1 1 calc R . . C21 C 0.3892(3) -0.0776(3) 0.32953(15) 0.0273(8) Uani 1 1 d . . . H21 H 0.4043 -0.0018 0.3434 0.033 Uiso 1 1 calc R . . C22 C 0.3477(2) -0.0349(3) 0.15341(13) 0.0191(7) Uani 1 1 d . . . C23 C 0.4445(3) -0.0346(3) 0.13987(15) 0.0257(8) Uani 1 1 d . . . H23 H 0.4996 -0.0009 0.1656 0.031 Uiso 1 1 calc R . . C24 C 0.4609(3) -0.0833(3) 0.08895(15) 0.0320(9) Uani 1 1 d . . . H24 H 0.5271 -0.0820 0.0797 0.038 Uiso 1 1 calc R . . C25 C 0.3820(3) -0.1337(3) 0.05153(15) 0.0311(9) Uani 1 1 d . . . H25 H 0.3938 -0.1672 0.0167 0.037 Uiso 1 1 calc R . . C26 C 0.2854(3) -0.1354(3) 0.06494(14) 0.0271(8) Uani 1 1 d . . . H26 H 0.2310 -0.1714 0.0397 0.033 Uiso 1 1 calc R . . C27 C 0.2682(3) -0.0848(3) 0.11514(14) 0.0222(8) Uani 1 1 d . . . H27 H 0.2013 -0.0841 0.1236 0.027 Uiso 1 1 calc R . . C28 C 0.2617(2) 0.3248(3) 0.34405(13) 0.0179(7) Uani 1 1 d . . . C29 C 0.2797(2) 0.2489(3) 0.39042(14) 0.0232(8) Uani 1 1 d . . . H29 H 0.2929 0.1702 0.3840 0.028 Uiso 1 1 calc R . . C30 C 0.2784(3) 0.2875(3) 0.44572(14) 0.0273(8) Uani 1 1 d . . . H30 H 0.2923 0.2355 0.4772 0.033 Uiso 1 1 calc R . . C31 C 0.2573(3) 0.4004(3) 0.45521(15) 0.0282(9) Uani 1 1 d . . . H31 H 0.2570 0.4265 0.4932 0.034 Uiso 1 1 calc R . . C32 C 0.2368(2) 0.4759(3) 0.40997(15) 0.0261(8) Uani 1 1 d . . . H32 H 0.2209 0.5537 0.4167 0.031 Uiso 1 1 calc R . . C33 C 0.2391(2) 0.4388(3) 0.35438(14) 0.0214(8) Uani 1 1 d . . . H33 H 0.2252 0.4915 0.3233 0.026 Uiso 1 1 calc R . . C34 C 0.2694(2) 0.3949(3) 0.22672(13) 0.0166(7) Uani 1 1 d . . . C35 C 0.3534(3) 0.4282(3) 0.20363(14) 0.0208(8) Uani 1 1 d . . . H35 H 0.4173 0.3918 0.2159 0.025 Uiso 1 1 calc R . . C36 C 0.3439(3) 0.5151(3) 0.16256(14) 0.0249(8) Uani 1 1 d . . . H36 H 0.4012 0.5371 0.1465 0.030 Uiso 1 1 calc R . . C37 C 0.2517(3) 0.5694(3) 0.14495(14) 0.0264(8) Uani 1 1 d . . . H37 H 0.2455 0.6285 0.1168 0.032 Uiso 1 1 calc R . . C38 C 0.1683(3) 0.5373(3) 0.16853(14) 0.0238(8) Uani 1 1 d . . . H38 H 0.1052 0.5760 0.1573 0.029 Uiso 1 1 calc R . . C39 C 0.1765(2) 0.4496(3) 0.20812(13) 0.0195(7) Uani 1 1 d . . . H39 H 0.1182 0.4262 0.2229 0.023 Uiso 1 1 calc R . . Mo1 Mo 0.15694(2) 0.11360(2) 0.224470(11) 0.01378(10) Uani 1 1 d . . . N1 N 0.0112(2) 0.1575(2) -0.02048(11) 0.0193(6) Uani 1 1 d . . . H1 H -0.019(2) 0.098(3) -0.0329(13) 0.014(9) Uiso 1 1 d . . . N2 N 0.0562(2) 0.3446(3) -0.03211(12) 0.0217(7) Uani 1 1 d . . . H2A H 0.048(2) 0.403(3) -0.0502(13) 0.008(9) Uiso 1 1 d . . . O1 O 0.06909(17) 0.05740(19) 0.06060(9) 0.0255(5) Uani 1 1 d . . . O2 O -0.04777(18) 0.25023(18) -0.10425(10) 0.0253(5) Uani 1 1 d . . . P1 P 0.32389(6) 0.02422(7) 0.22109(3) 0.0159(2) Uani 1 1 d . . . P2 P 0.27108(6) 0.26905(7) 0.27269(3) 0.0156(2) Uani 1 1 d . . . B1 B 0.1571(3) 0.8829(4) 0.44260(18) 0.0316(10) Uani 1 1 d . . . F1 F 0.1620(2) 0.7778(2) 0.41848(12) 0.0673(8) Uani 1 1 d . . . F2 F 0.22768(16) 0.9576(2) 0.42620(10) 0.0514(6) Uani 1 1 d . . . F3 F 0.1729(2) 0.8769(2) 0.50136(9) 0.0587(7) Uani 1 1 d . . . F4 F 0.06066(15) 0.93124(17) 0.42287(9) 0.0369(5) Uani 1 1 d . . . C40 C 0.4261(6) 0.4810(7) 0.0115(3) 0.044(2) Uani 0.50 1 d P . . H40A H 0.3592 0.5051 -0.0106 0.053 Uiso 0.50 1 calc PR . . H40B H 0.4147 0.4311 0.0436 0.053 Uiso 0.50 1 calc PR . . Cl1 Cl 0.49733(10) 0.59855(10) 0.03709(5) 0.0623(3) 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 C1 0.0151(17) 0.0132(17) 0.0239(19) -0.0072(15) -0.0059(14) 0.0001(14) C2 0.0219(18) 0.0188(18) 0.0152(18) -0.0063(14) 0.0021(14) -0.0036(15) C3 0.0104(17) 0.0219(18) 0.031(2) 0.0024(16) 0.0072(15) 0.0044(14) C4 0.0197(18) 0.0203(18) 0.028(2) -0.0071(15) 0.0132(15) -0.0029(15) C5 0.0237(19) 0.029(2) 0.0155(18) 0.0008(15) 0.0110(15) -0.0070(16) C6 0.0184(18) 0.0178(18) 0.0253(19) 0.0082(15) 0.0047(14) -0.0066(14) C7 0.0208(18) 0.0122(17) 0.033(2) 0.0003(15) 0.0140(16) -0.0044(14) C8 0.0180(17) 0.0203(18) 0.0236(19) -0.0071(15) 0.0033(14) -0.0104(15) C9 0.0116(17) 0.028(2) 0.0244(19) 0.0001(15) -0.0013(14) -0.0037(15) C10 0.0242(19) 0.0144(17) 0.0158(17) -0.0017(14) 0.0072(14) 0.0007(14) C11 0.0230(18) 0.0209(19) 0.0158(18) -0.0017(15) 0.0054(14) 0.0008(15) C12 0.0213(18) 0.0143(18) 0.020(2) -0.0002(15) 0.0058(15) 0.0026(15) C13 0.0247(19) 0.0193(18) 0.0174(18) -0.0020(15) 0.0054(15) -0.0017(15) C14 0.0169(17) 0.0175(18) 0.0207(18) 0.0012(14) 0.0028(14) 0.0008(14) C15 0.0171(17) 0.0128(17) 0.0195(18) 0.0024(13) 0.0002(14) 0.0016(14) C16 0.0178(17) 0.0171(18) 0.0202(18) 0.0009(14) 0.0059(14) 0.0034(14) C17 0.0259(19) 0.0214(19) 0.0240(19) -0.0005(15) 0.0057(15) 0.0042(15) C18 0.032(2) 0.0161(18) 0.030(2) 0.0004(15) 0.0115(16) 0.0010(16) C19 0.035(2) 0.019(2) 0.033(2) 0.0087(16) 0.0141(17) 0.0066(16) C20 0.046(2) 0.029(2) 0.022(2) 0.0051(17) 0.0027(17) 0.0023(18) C21 0.036(2) 0.0167(19) 0.028(2) -0.0012(15) 0.0045(17) -0.0007(16) C22 0.0237(19) 0.0128(17) 0.0203(18) 0.0020(14) 0.0028(15) 0.0027(15) C23 0.027(2) 0.0211(19) 0.029(2) -0.0034(16) 0.0053(16) 0.0019(16) C24 0.033(2) 0.034(2) 0.032(2) -0.0023(17) 0.0148(18) 0.0056(18) C25 0.045(2) 0.029(2) 0.0213(19) -0.0039(16) 0.0111(17) 0.0087(18) C26 0.040(2) 0.0185(19) 0.022(2) -0.0036(15) 0.0037(16) -0.0005(16) C27 0.0269(19) 0.0171(18) 0.0232(19) 0.0000(15) 0.0067(15) 0.0000(15) C28 0.0147(17) 0.0186(18) 0.0213(18) -0.0028(14) 0.0053(13) -0.0035(14) C29 0.0259(19) 0.0208(19) 0.023(2) -0.0013(15) 0.0049(15) -0.0052(15) C30 0.030(2) 0.033(2) 0.0202(19) -0.0009(16) 0.0088(15) -0.0064(17) C31 0.027(2) 0.037(2) 0.022(2) -0.0093(17) 0.0102(16) -0.0099(17) C32 0.0232(19) 0.024(2) 0.032(2) -0.0111(17) 0.0071(16) -0.0013(16) C33 0.0179(18) 0.0213(19) 0.0250(19) -0.0005(15) 0.0036(15) -0.0018(15) C34 0.0229(18) 0.0100(16) 0.0167(17) -0.0040(13) 0.0030(14) -0.0019(14) C35 0.0222(19) 0.0168(18) 0.0232(19) -0.0031(15) 0.0036(15) -0.0030(15) C36 0.030(2) 0.0234(19) 0.0226(19) -0.0018(16) 0.0085(16) -0.0101(17) C37 0.042(2) 0.0162(18) 0.0198(19) 0.0025(15) 0.0026(16) -0.0013(17) C38 0.027(2) 0.0170(19) 0.026(2) 0.0009(15) 0.0005(15) 0.0050(15) C39 0.0227(19) 0.0140(18) 0.0221(18) -0.0030(14) 0.0052(14) -0.0008(15) Mo1 0.01577(16) 0.01103(16) 0.01473(16) -0.00057(11) 0.00330(11) -0.00033(12) N1 0.0256(16) 0.0141(16) 0.0167(16) -0.0009(13) 0.0002(12) -0.0037(14) N2 0.0333(18) 0.0123(16) 0.0192(16) 0.0059(14) 0.0042(13) 0.0006(14) O1 0.0390(15) 0.0168(13) 0.0182(12) 0.0035(10) -0.0014(10) -0.0062(11) O2 0.0359(14) 0.0185(13) 0.0195(14) 0.0011(10) 0.0001(11) 0.0012(11) P1 0.0175(4) 0.0131(4) 0.0174(5) -0.0009(3) 0.0040(3) 0.0007(4) P2 0.0177(5) 0.0123(4) 0.0167(4) -0.0015(3) 0.0032(3) -0.0007(4) B1 0.042(3) 0.027(2) 0.027(2) 0.0034(19) 0.010(2) 0.005(2) F1 0.0818(19) 0.0336(14) 0.085(2) -0.0239(14) 0.0105(15) 0.0157(13) F2 0.0370(13) 0.0622(16) 0.0544(15) 0.0156(12) 0.0068(11) -0.0042(12) F3 0.091(2) 0.0564(16) 0.0292(13) 0.0137(11) 0.0120(12) 0.0181(14) F4 0.0393(13) 0.0281(12) 0.0449(13) -0.0020(10) 0.0115(10) 0.0008(10) C40 0.048(5) 0.044(5) 0.036(5) 0.000(4) -0.003(4) 0.004(4) Cl1 0.0733(8) 0.0469(7) 0.0593(8) 0.0056(6) -0.0077(6) 0.0002(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 C1 C2 1.301(4) . ? C1 Mo1 1.935(3) . ? C2 C10 1.474(4) . ? C2 H2 0.9500 . ? C3 C9 1.397(5) . ? C3 C4 1.405(5) . ? C3 Mo1 2.308(3) . ? C3 H3 0.9500 . ? C4 C5 1.409(5) . ? C4 Mo1 2.290(3) . ? C4 H4 0.9500 . ? C5 C6 1.393(5) . ? C5 Mo1 2.363(3) . ? C5 H5 0.9500 . ? C6 C7 1.416(5) . ? C6 Mo1 2.332(3) . ? C6 H6 0.9500 . ? C7 C8 1.400(5) . ? C7 Mo1 2.265(3) . ? C7 H7 0.9500 . ? C8 C9 1.410(5) . ? C8 Mo1 2.312(3) . ? C8 H8 0.9500 . ? C9 Mo1 2.300(3) . ? C9 H9 0.9500 . ? C10 C13 1.345(4) . ? C10 C11 1.448(4) . ? C11 O1 1.229(4) . ? C11 N1 1.378(4) . ? C12 O2 1.208(4) . ? C12 N2 1.369(4) . ? C12 N1 1.373(4) . ? C13 N2 1.366(4) . ? C13 H13 0.9500 . ? C14 C15 1.520(4) . ? C14 P1 1.834(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 P2 1.840(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C21 1.382(5) . ? C16 C17 1.394(4) . ? C16 P1 1.832(3) . ? C17 C18 1.368(5) . ? C17 H17 0.9500 . ? C18 C19 1.374(5) . ? C18 H18 0.9500 . ? C19 C20 1.371(5) . ? C19 H19 0.9500 . ? C20 C21 1.386(5) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.388(5) . ? C22 C27 1.391(5) . ? C22 P1 1.822(3) . ? C23 C24 1.383(5) . ? C23 H23 0.9500 . ? C24 C25 1.378(5) . ? C24 H24 0.9500 . ? C25 C26 1.384(5) . ? C25 H25 0.9500 . ? C26 C27 1.381(5) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C33 1.392(5) . ? C28 C29 1.394(4) . ? C28 P2 1.833(3) . ? C29 C30 1.385(5) . ? C29 H29 0.9500 . ? C30 C31 1.371(5) . ? C30 H30 0.9500 . ? C31 C32 1.373(5) . ? C31 H31 0.9500 . ? C32 C33 1.389(5) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.391(4) . ? C34 C39 1.393(4) . ? C34 P2 1.821(3) . ? C35 C36 1.391(5) . ? C35 H35 0.9500 . ? C36 C37 1.380(5) . ? C36 H36 0.9500 . ? C37 C38 1.385(5) . ? C37 H37 0.9500 . ? C38 C39 1.376(5) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? Mo1 P1 2.4759(9) . ? Mo1 P2 2.5032(8) . ? N1 H1 0.82(3) . ? N2 H2A 0.81(3) . ? B1 F1 1.356(5) . ? B1 F3 1.369(5) . ? B1 F2 1.388(5) . ? B1 F4 1.406(5) . ? C40 Cl1 1.713(8) . ? C40 Cl1 1.910(8) 3_665 ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? Cl1 C40 1.910(8) 3_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 Mo1 172.3(3) . . ? C1 C2 C10 125.6(3) . . ? C1 C2 H2 117.2 . . ? C10 C2 H2 117.2 . . ? C9 C3 C4 126.9(3) . . ? C9 C3 Mo1 72.06(18) . . ? C4 C3 Mo1 71.50(18) . . ? C9 C3 H3 116.6 . . ? C4 C3 H3 116.6 . . ? Mo1 C3 H3 134.4 . . ? C3 C4 C5 129.3(3) . . ? C3 C4 Mo1 72.92(18) . . ? C5 C4 Mo1 75.22(18) . . ? C3 C4 H4 115.3 . . ? C5 C4 H4 115.3 . . ? Mo1 C4 H4 129.9 . . ? C6 C5 C4 128.9(3) . . ? C6 C5 Mo1 71.55(18) . . ? C4 C5 Mo1 69.56(17) . . ? C6 C5 H5 115.6 . . ? C4 C5 H5 115.6 . . ? Mo1 C5 H5 140.5 . . ? C5 C6 C7 127.6(3) . . ? C5 C6 Mo1 73.94(18) . . ? C7 C6 Mo1 69.48(17) . . ? C5 C6 H6 116.2 . . ? C7 C6 H6 116.2 . . ? Mo1 C6 H6 135.3 . . ? C8 C7 C6 128.7(3) . . ? C8 C7 Mo1 74.04(18) . . ? C6 C7 Mo1 74.68(18) . . ? C8 C7 H7 115.6 . . ? C6 C7 H7 115.6 . . ? Mo1 C7 H7 128.5 . . ? C7 C8 C9 128.0(3) . . ? C7 C8 Mo1 70.35(18) . . ? C9 C8 Mo1 71.75(18) . . ? C7 C8 H8 116.0 . . ? C9 C8 H8 116.0 . . ? Mo1 C8 H8 137.7 . . ? C3 C9 C8 129.8(3) . . ? C3 C9 Mo1 72.64(17) . . ? C8 C9 Mo1 72.65(18) . . ? C3 C9 H9 115.1 . . ? C8 C9 H9 115.1 . . ? Mo1 C9 H9 134.7 . . ? C13 C10 C11 117.9(3) . . ? C13 C10 C2 122.9(3) . . ? C11 C10 C2 119.2(3) . . ? O1 C11 N1 119.8(3) . . ? O1 C11 C10 124.9(3) . . ? N1 C11 C10 115.3(3) . . ? O2 C12 N2 124.0(3) . . ? O2 C12 N1 122.8(3) . . ? N2 C12 N1 113.1(3) . . ? C10 C13 N2 122.4(3) . . ? C10 C13 H13 118.8 . . ? N2 C13 H13 118.8 . . ? C15 C14 P1 113.3(2) . . ? C15 C14 H14A 108.9 . . ? P1 C14 H14A 108.9 . . ? C15 C14 H14B 108.9 . . ? P1 C14 H14B 108.9 . . ? H14A C14 H14B 107.7 . . ? C14 C15 P2 112.5(2) . . ? C14 C15 H15A 109.1 . . ? P2 C15 H15A 109.1 . . ? C14 C15 H15B 109.1 . . ? P2 C15 H15B 109.1 . . ? H15A C15 H15B 107.8 . . ? C21 C16 C17 117.9(3) . . ? C21 C16 P1 121.7(2) . . ? C17 C16 P1 119.7(2) . . ? C18 C17 C16 120.8(3) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C17 C18 C19 120.8(3) . . ? C17 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? C20 C19 C18 119.4(3) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C19 C20 C21 120.1(3) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C16 C21 C20 121.0(3) . . ? C16 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? C23 C22 C27 119.0(3) . . ? C23 C22 P1 121.4(2) . . ? C27 C22 P1 119.6(2) . . ? C24 C23 C22 120.0(3) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C25 C24 C23 120.7(3) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C24 C25 C26 119.7(3) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? C27 C26 C25 119.9(3) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C26 C27 C22 120.7(3) . . ? C26 C27 H27 119.7 . . ? C22 C27 H27 119.7 . . ? C33 C28 C29 118.5(3) . . ? C33 C28 P2 123.5(2) . . ? C29 C28 P2 118.0(2) . . ? C30 C29 C28 120.5(3) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C31 C30 C29 120.2(3) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C30 C31 C32 120.3(3) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C31 C32 C33 120.2(3) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? C32 C33 C28 120.3(3) . . ? C32 C33 H33 119.8 . . ? C28 C33 H33 119.8 . . ? C35 C34 C39 119.0(3) . . ? C35 C34 P2 122.4(2) . . ? C39 C34 P2 118.0(2) . . ? C34 C35 C36 119.9(3) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C37 C36 C35 120.5(3) . . ? C37 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? C36 C37 C38 119.6(3) . . ? C36 C37 H37 120.2 . . ? C38 C37 H37 120.2 . . ? C39 C38 C37 120.3(3) . . ? C39 C38 H38 119.9 . . ? C37 C38 H38 119.9 . . ? C38 C39 C34 120.7(3) . . ? C38 C39 H39 119.7 . . ? C34 C39 H39 119.7 . . ? C1 Mo1 C7 124.41(12) . . ? C1 Mo1 C4 128.02(12) . . ? C7 Mo1 C4 87.26(12) . . ? C1 Mo1 C9 87.92(12) . . ? C7 Mo1 C9 67.16(12) . . ? C4 Mo1 C9 66.20(12) . . ? C1 Mo1 C3 99.58(12) . . ? C7 Mo1 C3 87.65(12) . . ? C4 Mo1 C3 35.58(11) . . ? C9 Mo1 C3 35.31(11) . . ? C1 Mo1 C8 98.07(12) . . ? C7 Mo1 C8 35.60(12) . . ? C4 Mo1 C8 86.18(12) . . ? C9 Mo1 C8 35.60(11) . . ? C3 Mo1 C8 66.78(11) . . ? C1 Mo1 C6 159.61(12) . . ? C7 Mo1 C6 35.84(11) . . ? C4 Mo1 C6 66.30(12) . . ? C9 Mo1 C6 85.95(11) . . ? C3 Mo1 C6 86.47(11) . . ? C8 Mo1 C6 66.27(11) . . ? C1 Mo1 C5 163.10(12) . . ? C7 Mo1 C5 65.96(11) . . ? C4 Mo1 C5 35.22(12) . . ? C9 Mo1 C5 84.57(12) . . ? C3 Mo1 C5 65.97(11) . . ? C8 Mo1 C5 84.52(11) . . ? C6 Mo1 C5 34.51(11) . . ? C1 Mo1 P1 80.78(9) . . ? C7 Mo1 P1 87.26(8) . . ? C4 Mo1 P1 147.07(9) . . ? C9 Mo1 P1 139.05(8) . . ? C3 Mo1 P1 174.02(8) . . ? C8 Mo1 P1 107.25(8) . . ? C6 Mo1 P1 91.23(8) . . ? C5 Mo1 P1 114.54(8) . . ? C1 Mo1 P2 83.71(9) . . ? C7 Mo1 P2 147.29(9) . . ? C4 Mo1 P2 86.52(8) . . ? C9 Mo1 P2 137.06(8) . . ? C3 Mo1 P2 105.15(8) . . ? C8 Mo1 P2 171.90(8) . . ? C6 Mo1 P2 113.68(8) . . ? C5 Mo1 P2 91.53(8) . . ? P1 Mo1 P2 80.82(3) . . ? C12 N1 C11 127.6(3) . . ? C12 N1 H1 118(2) . . ? C11 N1 H1 115(2) . . ? C13 N2 C12 123.6(3) . . ? C13 N2 H2A 120(2) . . ? C12 N2 H2A 116(2) . . ? C22 P1 C16 102.85(14) . . ? C22 P1 C14 103.73(14) . . ? C16 P1 C14 106.96(14) . . ? C22 P1 Mo1 119.29(10) . . ? C16 P1 Mo1 114.18(10) . . ? C14 P1 Mo1 108.76(10) . . ? C34 P2 C28 105.61(14) . . ? C34 P2 C15 106.03(14) . . ? C28 P2 C15 100.72(14) . . ? C34 P2 Mo1 111.64(10) . . ? C28 P2 Mo1 122.46(10) . . ? C15 P2 Mo1 108.85(10) . . ? F1 B1 F3 111.7(3) . . ? F1 B1 F2 111.1(3) . . ? F3 B1 F2 109.1(3) . . ? F1 B1 F4 109.5(3) . . ? F3 B1 F4 108.7(3) . . ? F2 B1 F4 106.5(3) . . ? Cl1 C40 Cl1 106.0(4) . 3_665 ? Cl1 C40 H40A 110.5 . . ? Cl1 C40 H40A 110.5 3_665 . ? Cl1 C40 H40B 110.5 . . ? Cl1 C40 H40B 110.5 3_665 . ? H40A C40 H40B 108.7 . . ? C40 Cl1 C40 74.0(4) . 3_665 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 C3 C4 C5 -4.5(5) . . . . ? Mo1 C3 C4 C5 -53.4(3) . . . . ? C9 C3 C4 Mo1 48.9(3) . . . . ? C3 C4 C5 C6 9.7(6) . . . . ? Mo1 C4 C5 C6 -42.8(3) . . . . ? C3 C4 C5 Mo1 52.5(3) . . . . ? C4 C5 C6 C7 -4.8(5) . . . . ? Mo1 C5 C6 C7 -47.0(3) . . . . ? C4 C5 C6 Mo1 42.1(3) . . . . ? C5 C6 C7 C8 -5.6(5) . . . . ? Mo1 C6 C7 C8 -54.2(3) . . . . ? C5 C6 C7 Mo1 48.6(3) . . . . ? C6 C7 C8 C9 8.9(5) . . . . ? Mo1 C7 C8 C9 -45.6(3) . . . . ? C6 C7 C8 Mo1 54.4(3) . . . . ? C4 C3 C9 C8 -0.6(5) . . . . ? Mo1 C3 C9 C8 48.1(3) . . . . ? C4 C3 C9 Mo1 -48.7(3) . . . . ? C7 C8 C9 C3 -3.1(6) . . . . ? Mo1 C8 C9 C3 -48.1(3) . . . . ? C7 C8 C9 Mo1 45.1(3) . . . . ? C1 C2 C10 C13 148.3(3) . . . . ? C1 C2 C10 C11 -32.4(5) . . . . ? C13 C10 C11 O1 -178.0(3) . . . . ? C2 C10 C11 O1 2.7(5) . . . . ? C13 C10 C11 N1 3.7(4) . . . . ? C2 C10 C11 N1 -175.7(3) . . . . ? C11 C10 C13 N2 -2.3(5) . . . . ? C2 C10 C13 N2 177.0(3) . . . . ? P1 C14 C15 P2 -45.4(3) . . . . ? C21 C16 C17 C18 0.5(5) . . . . ? P1 C16 C17 C18 -169.8(3) . . . . ? C16 C17 C18 C19 -1.4(5) . . . . ? C17 C18 C19 C20 0.8(5) . . . . ? C18 C19 C20 C21 0.6(5) . . . . ? C17 C16 C21 C20 0.9(5) . . . . ? P1 C16 C21 C20 171.0(3) . . . . ? C19 C20 C21 C16 -1.5(5) . . . . ? C27 C22 C23 C24 0.1(5) . . . . ? P1 C22 C23 C24 178.0(3) . . . . ? C22 C23 C24 C25 -0.8(5) . . . . ? C23 C24 C25 C26 0.2(5) . . . . ? C24 C25 C26 C27 1.2(5) . . . . ? C25 C26 C27 C22 -1.9(5) . . . . ? C23 C22 C27 C26 1.3(5) . . . . ? P1 C22 C27 C26 -176.6(2) . . . . ? C33 C28 C29 C30 -2.2(5) . . . . ? P2 C28 C29 C30 176.9(3) . . . . ? C28 C29 C30 C31 1.4(5) . . . . ? C29 C30 C31 C32 0.3(5) . . . . ? C30 C31 C32 C33 -1.2(5) . . . . ? C31 C32 C33 C28 0.4(5) . . . . ? C29 C28 C33 C32 1.3(5) . . . . ? P2 C28 C33 C32 -177.7(2) . . . . ? C39 C34 C35 C36 0.0(4) . . . . ? P2 C34 C35 C36 171.1(2) . . . . ? C34 C35 C36 C37 0.7(5) . . . . ? C35 C36 C37 C38 0.2(5) . . . . ? C36 C37 C38 C39 -1.8(5) . . . . ? C37 C38 C39 C34 2.5(5) . . . . ? C35 C34 C39 C38 -1.5(5) . . . . ? P2 C34 C39 C38 -173.0(2) . . . . ? C8 C7 Mo1 C1 -48.4(2) . . . . ? C6 C7 Mo1 C1 172.77(18) . . . . ? C8 C7 Mo1 C4 87.3(2) . . . . ? C6 C7 Mo1 C4 -51.61(19) . . . . ? C8 C7 Mo1 C9 21.99(18) . . . . ? C6 C7 Mo1 C9 -116.9(2) . . . . ? C8 C7 Mo1 C3 51.6(2) . . . . ? C6 C7 Mo1 C3 -87.22(19) . . . . ? C6 C7 Mo1 C8 -138.9(3) . . . . ? C8 C7 Mo1 C6 138.9(3) . . . . ? C8 C7 Mo1 C5 116.3(2) . . . . ? C6 C7 Mo1 C5 -22.56(18) . . . . ? C8 C7 Mo1 P1 -125.22(18) . . . . ? C6 C7 Mo1 P1 95.91(18) . . . . ? C8 C7 Mo1 P2 166.49(14) . . . . ? C6 C7 Mo1 P2 27.6(3) . . . . ? C3 C4 Mo1 C1 43.1(2) . . . . ? C5 C4 Mo1 C1 -176.84(18) . . . . ? C3 C4 Mo1 C7 -89.8(2) . . . . ? C5 C4 Mo1 C7 50.3(2) . . . . ? C3 C4 Mo1 C9 -23.59(18) . . . . ? C5 C4 Mo1 C9 116.4(2) . . . . ? C5 C4 Mo1 C3 140.0(3) . . . . ? C3 C4 Mo1 C8 -54.14(19) . . . . ? C5 C4 Mo1 C8 85.9(2) . . . . ? C3 C4 Mo1 C6 -119.9(2) . . . . ? C5 C4 Mo1 C6 20.18(18) . . . . ? C3 C4 Mo1 C5 -140.0(3) . . . . ? C3 C4 Mo1 P1 -170.47(15) . . . . ? C5 C4 Mo1 P1 -30.4(3) . . . . ? C3 C4 Mo1 P2 122.35(18) . . . . ? C5 C4 Mo1 P2 -97.61(18) . . . . ? C3 C9 Mo1 C1 -109.8(2) . . . . ? C8 C9 Mo1 C1 107.0(2) . . . . ? C3 C9 Mo1 C7 121.2(2) . . . . ? C8 C9 Mo1 C7 -21.99(18) . . . . ? C3 C9 Mo1 C4 23.76(18) . . . . ? C8 C9 Mo1 C4 -119.4(2) . . . . ? C8 C9 Mo1 C3 -143.2(3) . . . . ? C3 C9 Mo1 C8 143.2(3) . . . . ? C3 C9 Mo1 C6 89.6(2) . . . . ? C8 C9 Mo1 C6 -53.56(19) . . . . ? C3 C9 Mo1 C5 55.0(2) . . . . ? C8 C9 Mo1 C5 -88.2(2) . . . . ? C3 C9 Mo1 P1 176.81(14) . . . . ? C8 C9 Mo1 P1 33.6(2) . . . . ? C3 C9 Mo1 P2 -31.4(2) . . . . ? C8 C9 Mo1 P2 -174.56(14) . . . . ? C9 C3 Mo1 C1 72.4(2) . . . . ? C4 C3 Mo1 C1 -146.90(19) . . . . ? C9 C3 Mo1 C7 -52.1(2) . . . . ? C4 C3 Mo1 C7 88.6(2) . . . . ? C9 C3 Mo1 C4 -140.7(3) . . . . ? C4 C3 Mo1 C9 140.7(3) . . . . ? C9 C3 Mo1 C8 -22.32(19) . . . . ? C4 C3 Mo1 C8 118.4(2) . . . . ? C9 C3 Mo1 C6 -88.0(2) . . . . ? C4 C3 Mo1 C6 52.7(2) . . . . ? C9 C3 Mo1 C5 -116.8(2) . . . . ? C4 C3 Mo1 C5 23.93(18) . . . . ? C9 C3 Mo1 P2 158.43(17) . . . . ? C4 C3 Mo1 P2 -60.88(19) . . . . ? C7 C8 Mo1 C1 141.5(2) . . . . ? C9 C8 Mo1 C1 -74.9(2) . . . . ? C9 C8 Mo1 C7 143.7(3) . . . . ? C7 C8 Mo1 C4 -90.6(2) . . . . ? C9 C8 Mo1 C4 53.0(2) . . . . ? C7 C8 Mo1 C9 -143.7(3) . . . . ? C7 C8 Mo1 C3 -121.5(2) . . . . ? C9 C8 Mo1 C3 22.15(18) . . . . ? C7 C8 Mo1 C6 -24.88(18) . . . . ? C9 C8 Mo1 C6 118.8(2) . . . . ? C7 C8 Mo1 C5 -55.3(2) . . . . ? C9 C8 Mo1 C5 88.3(2) . . . . ? C7 C8 Mo1 P1 58.69(19) . . . . ? C9 C8 Mo1 P1 -157.65(17) . . . . ? C5 C6 Mo1 C1 -159.1(3) . . . . ? C7 C6 Mo1 C1 -17.3(4) . . . . ? C5 C6 Mo1 C7 -141.8(3) . . . . ? C5 C6 Mo1 C4 -20.55(19) . . . . ? C7 C6 Mo1 C4 121.2(2) . . . . ? C5 C6 Mo1 C9 -86.3(2) . . . . ? C7 C6 Mo1 C9 55.49(19) . . . . ? C5 C6 Mo1 C3 -50.9(2) . . . . ? C7 C6 Mo1 C3 90.9(2) . . . . ? C5 C6 Mo1 C8 -117.1(2) . . . . ? C7 C6 Mo1 C8 24.73(18) . . . . ? C7 C6 Mo1 C5 141.8(3) . . . . ? C5 C6 Mo1 P1 134.60(18) . . . . ? C7 C6 Mo1 P1 -83.61(18) . . . . ? C5 C6 Mo1 P2 54.1(2) . . . . ? C7 C6 Mo1 P2 -164.12(16) . . . . ? C6 C5 Mo1 C1 154.7(4) . . . . ? C4 C5 Mo1 C1 8.6(5) . . . . ? C6 C5 Mo1 C7 23.36(19) . . . . ? C4 C5 Mo1 C7 -122.8(2) . . . . ? C6 C5 Mo1 C4 146.1(3) . . . . ? C6 C5 Mo1 C9 90.7(2) . . . . ? C4 C5 Mo1 C9 -55.38(19) . . . . ? C6 C5 Mo1 C3 122.0(2) . . . . ? C4 C5 Mo1 C3 -24.15(18) . . . . ? C6 C5 Mo1 C8 55.0(2) . . . . ? C4 C5 Mo1 C8 -91.1(2) . . . . ? C4 C5 Mo1 C6 -146.1(3) . . . . ? C6 C5 Mo1 P1 -51.5(2) . . . . ? C4 C5 Mo1 P1 162.38(16) . . . . ? C6 C5 Mo1 P2 -132.10(18) . . . . ? C4 C5 Mo1 P2 81.78(18) . . . . ? O2 C12 N1 C11 177.4(3) . . . . ? N2 C12 N1 C11 -2.4(5) . . . . ? O1 C11 N1 C12 -179.8(3) . . . . ? C10 C11 N1 C12 -1.3(5) . . . . ? C10 C13 N2 C12 -1.7(5) . . . . ? O2 C12 N2 C13 -175.8(3) . . . . ? N1 C12 N2 C13 3.9(4) . . . . ? C23 C22 P1 C16 -84.0(3) . . . . ? C27 C22 P1 C16 93.9(3) . . . . ? C23 C22 P1 C14 27.4(3) . . . . ? C27 C22 P1 C14 -154.8(3) . . . . ? C23 C22 P1 Mo1 148.5(2) . . . . ? C27 C22 P1 Mo1 -33.6(3) . . . . ? C21 C16 P1 C22 153.3(3) . . . . ? C17 C16 P1 C22 -36.8(3) . . . . ? C21 C16 P1 C14 44.4(3) . . . . ? C17 C16 P1 C14 -145.7(3) . . . . ? C21 C16 P1 Mo1 -75.9(3) . . . . ? C17 C16 P1 Mo1 93.9(3) . . . . ? C15 C14 P1 C22 164.4(2) . . . . ? C15 C14 P1 C16 -87.3(2) . . . . ? C15 C14 P1 Mo1 36.4(2) . . . . ? C1 Mo1 P1 C22 -45.65(15) . . . . ? C7 Mo1 P1 C22 79.86(14) . . . . ? C4 Mo1 P1 C22 160.55(19) . . . . ? C9 Mo1 P1 C22 30.26(18) . . . . ? C8 Mo1 P1 C22 50.00(15) . . . . ? C6 Mo1 P1 C22 115.49(14) . . . . ? C5 Mo1 P1 C22 141.82(14) . . . . ? P2 Mo1 P1 C22 -130.71(12) . . . . ? C1 Mo1 P1 C16 -167.75(14) . . . . ? C7 Mo1 P1 C16 -42.23(14) . . . . ? C4 Mo1 P1 C16 38.45(19) . . . . ? C9 Mo1 P1 C16 -91.84(17) . . . . ? C8 Mo1 P1 C16 -72.10(14) . . . . ? C6 Mo1 P1 C16 -6.60(14) . . . . ? C5 Mo1 P1 C16 19.72(14) . . . . ? P2 Mo1 P1 C16 107.20(11) . . . . ? C1 Mo1 P1 C14 72.89(14) . . . . ? C7 Mo1 P1 C14 -161.59(14) . . . . ? C4 Mo1 P1 C14 -80.90(19) . . . . ? C9 Mo1 P1 C14 148.81(16) . . . . ? C8 Mo1 P1 C14 168.54(14) . . . . ? C6 Mo1 P1 C14 -125.96(13) . . . . ? C5 Mo1 P1 C14 -99.63(14) . . . . ? P2 Mo1 P1 C14 -12.16(11) . . . . ? C35 C34 P2 C28 112.7(3) . . . . ? C39 C34 P2 C28 -76.1(3) . . . . ? C35 C34 P2 C15 6.4(3) . . . . ? C39 C34 P2 C15 177.6(2) . . . . ? C35 C34 P2 Mo1 -112.0(2) . . . . ? C39 C34 P2 Mo1 59.2(3) . . . . ? C33 C28 P2 C34 10.4(3) . . . . ? C29 C28 P2 C34 -168.6(2) . . . . ? C33 C28 P2 C15 120.5(3) . . . . ? C29 C28 P2 C15 -58.5(3) . . . . ? C33 C28 P2 Mo1 -118.8(2) . . . . ? C29 C28 P2 Mo1 62.2(3) . . . . ? C14 C15 P2 C34 -87.7(2) . . . . ? C14 C15 P2 C28 162.5(2) . . . . ? C14 C15 P2 Mo1 32.5(2) . . . . ? C1 Mo1 P2 C34 26.87(14) . . . . ? C7 Mo1 P2 C34 178.56(18) . . . . ? C4 Mo1 P2 C34 -102.00(14) . . . . ? C9 Mo1 P2 C34 -53.21(17) . . . . ? C3 Mo1 P2 C34 -71.38(14) . . . . ? C6 Mo1 P2 C34 -164.20(14) . . . . ? C5 Mo1 P2 C34 -136.88(14) . . . . ? P1 Mo1 P2 C34 108.50(11) . . . . ? C1 Mo1 P2 C28 153.42(15) . . . . ? C7 Mo1 P2 C28 -54.9(2) . . . . ? C4 Mo1 P2 C28 24.55(15) . . . . ? C9 Mo1 P2 C28 73.34(18) . . . . ? C3 Mo1 P2 C28 55.16(15) . . . . ? C6 Mo1 P2 C28 -37.65(15) . . . . ? C5 Mo1 P2 C28 -10.33(15) . . . . ? P1 Mo1 P2 C28 -124.95(13) . . . . ? C1 Mo1 P2 C15 -89.83(14) . . . . ? C7 Mo1 P2 C15 61.85(19) . . . . ? C4 Mo1 P2 C15 141.30(14) . . . . ? C9 Mo1 P2 C15 -169.91(16) . . . . ? C3 Mo1 P2 C15 171.91(13) . . . . ? C6 Mo1 P2 C15 79.10(14) . . . . ? C5 Mo1 P2 C15 106.42(13) . . . . ? P1 Mo1 P2 C15 -8.20(11) . . . . ? Cl1 C40 Cl1 C40 0.0 3_665 . . 3_665 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2A F4 0.81(3) 2.04(3) 2.823(4) 163(3) 4_575 N1 H1 O1 0.82(3) 2.00(3) 2.818(4) 171(3) 3 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 22.55 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.555 _refine_diff_density_min -0.438 _refine_diff_density_rms 0.065 data_Ruuracilvinylidene _database_code_depnum_ccdc_archive 'CCDC 628687' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C47 H39 N2 O2 P2 Ru, F6 P' _chemical_formula_sum 'C47 H39 F6 N2 O2 P3 Ru' _chemical_formula_weight 971.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6(3)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' _cell_length_a 28.3109(11) _cell_length_b 28.3109(11) _cell_length_c 24.9373(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 17309.6(16) _cell_formula_units_Z 12 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7669 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 21.81 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.119 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5928 _exptl_absorpt_coefficient_mu 0.405 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.867 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS v2.03; (Sheldrick)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 110577 _diffrn_reflns_av_R_equivalents 0.0633 _diffrn_reflns_av_sigmaI/netI 0.0260 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 0.83 _diffrn_reflns_theta_max 22.51 _reflns_number_total 7777 _reflns_number_gt 6088 _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, 1997)' _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. The PF6- anions occupied two special positions within the asymmetric unit of equal occupancy; the geometry of one anion was restrained by fixing the PF bond lengths and FPF angles to 1.56 A and 90%, respectively (using DFIX and DANG). The disordered solvent was modelled using the SQUEEZE procedure within Platon. ; _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^)+(0.1126P)^2^+22.6269P] 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 7777 _refine_ls_number_parameters 559 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0767 _refine_ls_R_factor_gt 0.0611 _refine_ls_wR_factor_ref 0.1860 _refine_ls_wR_factor_gt 0.1760 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.057 _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 Ru1 Ru 0.377728(19) 0.298822(17) 0.606503(16) 0.0460(2) Uani 1 1 d . . . C1 C 0.4067(4) 0.3456(3) 0.6831(2) 0.078(2) Uani 1 1 d . . . H1 H 0.4259 0.3844 0.6836 0.093 Uiso 1 1 calc R . . C2 C 0.3506(4) 0.3129(3) 0.6858(2) 0.079(2) Uani 1 1 d . . . H2 H 0.3249 0.3250 0.6877 0.094 Uiso 1 1 calc R . . C3 C 0.3386(3) 0.2581(3) 0.6852(2) 0.0726(18) Uani 1 1 d . . . H3 H 0.3033 0.2267 0.6873 0.087 Uiso 1 1 calc R . . C4 C 0.3876(3) 0.2582(3) 0.6808(2) 0.076(2) Uani 1 1 d . . . H4 H 0.3913 0.2267 0.6791 0.091 Uiso 1 1 calc R . . C5 C 0.4310(3) 0.3127(3) 0.6793(2) 0.079(2) Uani 1 1 d . . . H5 H 0.4688 0.3247 0.6765 0.095 Uiso 1 1 calc R . . C6 C 0.3675(2) 0.2208(2) 0.4844(2) 0.0468(13) Uani 1 1 d . . . C7 C 0.3201(2) 0.2203(2) 0.4689(2) 0.0514(13) Uani 1 1 d . . . H7 H 0.3037 0.2342 0.4926 0.062 Uiso 1 1 calc R . . C8 C 0.2964(3) 0.1998(2) 0.4195(3) 0.0675(17) Uani 1 1 d . . . H8 H 0.2646 0.2008 0.4094 0.081 Uiso 1 1 calc R . . C9 C 0.3179(4) 0.1786(3) 0.3856(3) 0.088(2) Uani 1 1 d . . . H9 H 0.3011 0.1645 0.3519 0.106 Uiso 1 1 calc R . . C10 C 0.3639(4) 0.1773(3) 0.3998(3) 0.088(2) Uani 1 1 d . . . H10 H 0.3789 0.1620 0.3760 0.106 Uiso 1 1 calc R . . C11 C 0.3889(3) 0.1981(2) 0.4489(2) 0.0631(16) Uani 1 1 d . . . H11 H 0.4207 0.1969 0.4584 0.076 Uiso 1 1 calc R . . C12 C 0.3679(2) 0.1721(2) 0.5804(2) 0.0476(13) Uani 1 1 d . . . C13 C 0.3193(3) 0.1479(2) 0.6082(2) 0.0595(16) Uani 1 1 d . . . H13 H 0.3019 0.1684 0.6158 0.071 Uiso 1 1 calc R . . C14 C 0.2954(3) 0.0944(2) 0.6252(3) 0.0753(19) Uani 1 1 d . . . H14 H 0.2618 0.0785 0.6442 0.090 Uiso 1 1 calc R . . C15 C 0.3202(3) 0.0637(3) 0.6148(3) 0.0752(19) Uani 1 1 d . . . H15 H 0.3039 0.0268 0.6264 0.090 Uiso 1 1 calc R . . C16 C 0.3690(3) 0.0878(2) 0.5873(3) 0.0685(17) Uani 1 1 d . . . H16 H 0.3866 0.0674 0.5802 0.082 Uiso 1 1 calc R . . C17 C 0.3929(2) 0.1413(2) 0.5698(2) 0.0528(14) Uani 1 1 d . . . H17 H 0.4263 0.1571 0.5506 0.063 Uiso 1 1 calc R . . C18 C 0.4676(2) 0.2651(2) 0.5461(3) 0.0622(17) Uani 1 1 d . . . C19 C 0.4954(3) 0.2611(3) 0.5892(4) 0.088(2) Uani 1 1 d . . . H19 H 0.4757 0.2421 0.6203 0.106 Uiso 1 1 calc R . . C20 C 0.5517(4) 0.2841(4) 0.5883(6) 0.142(5) Uani 1 1 d . . . H20 H 0.5710 0.2806 0.6177 0.171 Uiso 1 1 calc R . . C21 C 0.5790(4) 0.3131(4) 0.5416(8) 0.182(7) Uani 1 1 d . . . H21 H 0.6177 0.3306 0.5407 0.218 Uiso 1 1 calc R . . C22 C 0.5523(3) 0.3173(3) 0.4973(6) 0.143(5) Uani 1 1 d . . . H22 H 0.5720 0.3361 0.4662 0.172 Uiso 1 1 calc R . . C23 C 0.4955(3) 0.2932(2) 0.4992(3) 0.081(2) Uani 1 1 d . . . H23 H 0.4760 0.2958 0.4695 0.098 Uiso 1 1 calc R . . C24 C 0.3945(2) 0.42114(19) 0.5554(2) 0.0450(12) Uani 1 1 d . . . C25 C 0.3674(2) 0.4250(2) 0.5997(2) 0.0584(15) Uani 1 1 d . . . H25 H 0.3651 0.4052 0.6313 0.070 Uiso 1 1 calc R . . C26 C 0.3433(3) 0.4576(2) 0.5984(3) 0.0654(17) Uani 1 1 d . . . H26 H 0.3250 0.4602 0.6292 0.079 Uiso 1 1 calc R . . C27 C 0.3462(2) 0.4859(2) 0.5528(3) 0.0607(16) Uani 1 1 d . . . H27 H 0.3299 0.5081 0.5516 0.073 Uiso 1 1 calc R . . C28 C 0.3728(2) 0.4816(2) 0.5089(3) 0.0544(15) Uani 1 1 d . . . H28 H 0.3744 0.5008 0.4771 0.065 Uiso 1 1 calc R . . C29 C 0.3971(2) 0.45020(19) 0.5099(2) 0.0448(12) Uani 1 1 d . . . H29 H 0.4158 0.4484 0.4791 0.054 Uiso 1 1 calc R . . C30 C 0.44381(19) 0.37677(19) 0.4873(2) 0.0413(12) Uani 1 1 d . . . C31 C 0.4012(2) 0.34593(19) 0.4523(2) 0.0428(12) Uani 1 1 d . . . H31 H 0.3647 0.3273 0.4650 0.051 Uiso 1 1 calc R . . C32 C 0.4120(2) 0.3423(2) 0.3987(2) 0.0519(14) Uani 1 1 d . . . H32 H 0.3828 0.3211 0.3749 0.062 Uiso 1 1 calc R . . C33 C 0.4643(2) 0.3689(2) 0.3799(2) 0.0590(15) Uani 1 1 d . . . H33 H 0.4716 0.3655 0.3434 0.071 Uiso 1 1 calc R . . C34 C 0.5066(2) 0.4010(2) 0.4146(2) 0.0582(15) Uani 1 1 d . . . H34 H 0.5429 0.4204 0.4013 0.070 Uiso 1 1 calc R . . C35 C 0.4970(2) 0.4051(2) 0.4678(2) 0.0518(14) Uani 1 1 d . . . H35 H 0.5264 0.4271 0.4912 0.062 Uiso 1 1 calc R . . C36 C 0.4940(2) 0.4246(2) 0.5889(2) 0.0520(14) Uani 1 1 d . . . C37 C 0.5291(3) 0.4052(3) 0.5988(3) 0.0748(19) Uani 1 1 d . . . H37 H 0.5192 0.3692 0.5883 0.090 Uiso 1 1 calc R . . C38 C 0.5791(3) 0.4380(3) 0.6243(3) 0.082(2) Uani 1 1 d . . . H38 H 0.6033 0.4245 0.6306 0.099 Uiso 1 1 calc R . . C39 C 0.5932(3) 0.4903(3) 0.6402(3) 0.083(2) Uani 1 1 d . . . H39 H 0.6270 0.5128 0.6578 0.100 Uiso 1 1 calc R . . C40 C 0.5583(3) 0.5092(3) 0.6306(2) 0.0716(18) Uani 1 1 d . . . H40 H 0.5679 0.5449 0.6419 0.086 Uiso 1 1 calc R . . C41 C 0.5094(2) 0.4778(2) 0.60486(19) 0.0527(14) Uani 1 1 d . . . H41 H 0.4861 0.4922 0.5979 0.063 Uiso 1 1 calc R . . C42 C 0.3157(2) 0.2906(2) 0.5731(2) 0.0476(13) Uani 1 1 d . . . C43 C 0.2746(2) 0.2942(2) 0.5542(2) 0.0519(14) Uani 1 1 d . . . H43 H 0.2798 0.3300 0.5530 0.062 Uiso 1 1 calc R . . C44 C 0.2212(2) 0.2508(2) 0.5343(3) 0.0587(15) Uani 1 1 d . . . C47 C 0.1869(2) 0.2623(2) 0.5080(3) 0.0677(18) Uani 1 1 d . . . H47 H 0.1964 0.2993 0.5034 0.081 Uiso 1 1 calc R . . C48 C 0.1225(3) 0.1692(3) 0.4929(5) 0.112(3) Uani 1 1 d . . . C49 C 0.2059(2) 0.1948(2) 0.5428(3) 0.076(2) Uani 1 1 d . . . F1 F 0.3429(4) 0.0925(3) 0.2964(3) 0.193(3) Uani 1 1 d . . . F2 F 0.3996(4) 0.0784(4) 0.2500 0.181(4) Uani 1 2 d S . . F3 F 0.4271(3) 0.1586(3) 0.2925(3) 0.185(3) Uani 1 1 d . . . F4 F 0.3602(5) 0.1634(4) 0.2500 0.182(4) Uani 1 2 d S . . F5 F 0.4759(3) 0.2453(2) 0.7500 0.167(4) Uani 1 2 d SD . . F6 F 0.4266(4) 0.1694(3) 0.7045(3) 0.301(7) Uani 1 1 d D . . F7 F 0.5159(4) 0.2079(3) 0.7063(3) 0.335(8) Uani 1 1 d D . . F8 F 0.4653(5) 0.1309(3) 0.7500 0.375(14) Uani 1 2 d SD . . N1 N 0.1382(2) 0.2219(2) 0.4875(3) 0.0863(19) Uani 1 1 d . . . H1A H 0.1168 0.2311 0.4703 0.104 Uiso 1 1 calc R . . N2 N 0.1565(2) 0.1574(2) 0.5213(3) 0.108(3) Uani 1 1 d . . . H2A H 0.1458 0.1227 0.5262 0.130 Uiso 1 1 calc R . . O1 O 0.0797(2) 0.1321(2) 0.4724(4) 0.155(3) Uani 1 1 d . . . O2 O 0.23361(17) 0.17890(16) 0.5655(2) 0.0821(15) Uani 1 1 d . . . P2 P 0.42767(5) 0.37888(5) 0.55781(5) 0.0433(4) Uani 1 1 d . . . P3 P 0.39483(5) 0.24082(5) 0.55209(5) 0.0418(3) Uani 1 1 d . . . P4 P 0.3820(2) 0.12268(17) 0.2500 0.1186(13) Uani 1 2 d S . . P5 P 0.4699(3) 0.1876(2) 0.7500 0.251(4) Uani 1 2 d SD . . 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 Ru1 0.0645(3) 0.0509(3) 0.0366(3) 0.00075(19) 0.00130(19) 0.0394(2) C1 0.136(7) 0.090(5) 0.031(3) -0.016(3) -0.019(4) 0.074(5) C2 0.141(7) 0.090(5) 0.040(3) 0.007(3) 0.011(4) 0.085(5) C3 0.108(5) 0.091(5) 0.041(3) 0.015(3) 0.021(3) 0.067(5) C4 0.138(7) 0.072(5) 0.036(3) 0.007(3) -0.012(4) 0.066(5) C5 0.129(6) 0.095(5) 0.045(4) -0.011(3) -0.026(4) 0.080(5) C6 0.059(3) 0.038(3) 0.052(3) 0.001(2) 0.007(3) 0.031(3) C7 0.056(3) 0.040(3) 0.057(3) -0.008(3) -0.005(3) 0.023(3) C8 0.089(5) 0.050(3) 0.073(4) -0.010(3) -0.017(4) 0.041(3) C9 0.153(8) 0.081(5) 0.060(4) -0.017(4) -0.026(4) 0.081(5) C10 0.154(7) 0.104(6) 0.046(4) -0.012(4) 0.003(4) 0.094(6) C11 0.092(4) 0.070(4) 0.052(4) 0.003(3) 0.011(3) 0.058(4) C12 0.057(3) 0.046(3) 0.050(3) 0.007(2) 0.007(3) 0.033(3) C13 0.076(4) 0.055(4) 0.064(4) 0.016(3) 0.017(3) 0.046(3) C14 0.077(4) 0.062(4) 0.102(5) 0.026(4) 0.029(4) 0.046(4) C15 0.090(5) 0.057(4) 0.091(5) 0.029(4) 0.026(4) 0.046(4) C16 0.087(5) 0.061(4) 0.080(4) 0.005(3) 0.009(4) 0.053(4) C17 0.062(3) 0.049(3) 0.058(3) 0.006(3) 0.012(3) 0.035(3) C18 0.042(3) 0.041(3) 0.110(5) 0.006(3) 0.011(3) 0.025(3) C19 0.070(5) 0.059(4) 0.154(7) -0.012(4) -0.032(5) 0.046(4) C20 0.073(6) 0.064(5) 0.298(15) -0.008(7) -0.057(8) 0.040(5) C21 0.044(5) 0.072(6) 0.43(2) 0.045(10) 0.012(9) 0.032(5) C22 0.065(5) 0.078(6) 0.305(16) 0.053(7) 0.068(8) 0.049(5) C23 0.061(4) 0.054(4) 0.143(7) 0.013(4) 0.033(4) 0.039(3) C24 0.050(3) 0.039(3) 0.052(3) -0.013(2) -0.013(3) 0.026(2) C25 0.078(4) 0.048(3) 0.059(4) -0.003(3) 0.003(3) 0.039(3) C26 0.071(4) 0.052(3) 0.085(5) -0.010(3) 0.008(3) 0.039(3) C27 0.047(3) 0.035(3) 0.100(5) -0.007(3) -0.009(3) 0.021(3) C28 0.040(3) 0.038(3) 0.080(4) -0.003(3) -0.019(3) 0.016(3) C29 0.041(3) 0.040(3) 0.055(3) -0.003(2) -0.012(2) 0.021(2) C30 0.042(3) 0.036(3) 0.051(3) 0.001(2) -0.003(2) 0.023(2) C31 0.041(3) 0.039(3) 0.047(3) 0.000(2) -0.003(2) 0.019(2) C32 0.055(3) 0.052(3) 0.041(3) -0.002(3) -0.002(3) 0.021(3) C33 0.071(4) 0.054(3) 0.052(3) 0.002(3) 0.013(3) 0.031(3) C34 0.049(3) 0.052(3) 0.068(4) 0.005(3) 0.013(3) 0.021(3) C35 0.044(3) 0.041(3) 0.065(4) -0.008(3) -0.008(3) 0.017(3) C36 0.061(3) 0.049(3) 0.050(3) -0.005(3) -0.019(3) 0.031(3) C37 0.077(4) 0.056(4) 0.095(5) -0.010(3) -0.036(4) 0.036(4) C38 0.064(4) 0.068(4) 0.111(6) 0.000(4) -0.045(4) 0.030(4) C39 0.084(5) 0.067(4) 0.075(5) 0.000(4) -0.042(4) 0.021(4) C40 0.087(5) 0.056(4) 0.055(4) -0.007(3) -0.028(4) 0.024(4) C41 0.064(4) 0.052(3) 0.040(3) -0.004(3) -0.015(3) 0.028(3) C42 0.055(3) 0.042(3) 0.055(3) 0.004(2) 0.016(3) 0.031(3) C43 0.064(4) 0.045(3) 0.057(3) 0.007(3) 0.009(3) 0.035(3) C44 0.046(3) 0.048(3) 0.094(4) 0.007(3) 0.018(3) 0.031(3) C47 0.033(3) 0.053(3) 0.117(5) -0.005(3) 0.005(3) 0.022(3) C48 0.038(4) 0.049(4) 0.252(11) -0.026(5) -0.011(5) 0.024(3) C49 0.040(3) 0.055(4) 0.144(6) 0.001(4) 0.015(4) 0.031(3) F1 0.283(9) 0.135(5) 0.154(5) 0.061(4) 0.076(6) 0.099(6) F2 0.186(9) 0.130(7) 0.265(12) 0.000 0.000 0.108(7) F3 0.218(7) 0.216(7) 0.105(4) -0.025(4) -0.043(5) 0.097(6) F4 0.258(11) 0.178(8) 0.193(9) 0.000 0.000 0.171(9) F5 0.223(9) 0.196(9) 0.186(8) 0.000 0.000 0.183(8) F6 0.56(2) 0.282(10) 0.207(8) -0.060(7) -0.199(11) 0.321(13) F7 0.69(3) 0.434(17) 0.103(5) -0.010(8) 0.039(10) 0.45(2) F8 0.92(4) 0.56(3) 0.068(5) 0.000 0.000 0.69(3) N1 0.051(3) 0.057(3) 0.161(6) -0.007(3) -0.006(3) 0.034(3) N2 0.040(3) 0.046(3) 0.250(9) 0.000(4) 0.012(4) 0.029(3) O1 0.059(3) 0.068(3) 0.347(11) -0.058(5) -0.046(5) 0.038(3) O2 0.065(3) 0.055(2) 0.144(4) 0.021(3) 0.024(3) 0.043(2) P2 0.0503(8) 0.0432(8) 0.0430(8) -0.0068(6) -0.0101(6) 0.0284(7) P3 0.0460(8) 0.0412(7) 0.0465(8) 0.0027(6) 0.0048(6) 0.0280(6) P4 0.196(4) 0.134(3) 0.0640(19) 0.000 0.000 0.112(3) P5 0.573(13) 0.402(9) 0.058(2) 0.000 0.000 0.454(11) _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 Ru1 C42 1.850(6) . ? Ru1 C2 2.228(6) . ? Ru1 C1 2.233(6) . ? Ru1 C3 2.264(6) . ? Ru1 C5 2.267(6) . ? Ru1 C4 2.270(5) . ? Ru1 P2 2.3250(14) . ? Ru1 P3 2.3595(13) . ? C1 C2 1.383(10) . ? C1 C5 1.413(9) . ? C1 H1 0.9500 . ? C2 C3 1.412(9) . ? C2 H2 0.9500 . ? C3 C4 1.390(9) . ? C3 H3 0.9500 . ? C4 C5 1.411(10) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.389(7) . ? C6 C11 1.397(7) . ? C6 P3 1.824(5) . ? C7 C8 1.384(8) . ? C7 H7 0.9500 . ? C8 C9 1.346(9) . ? C8 H8 0.9500 . ? C9 C10 1.370(10) . ? C9 H9 0.9500 . ? C10 C11 1.388(9) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.379(8) . ? C12 C17 1.394(7) . ? C12 P3 1.839(5) . ? C13 C14 1.381(8) . ? C13 H13 0.9500 . ? C14 C15 1.388(8) . ? C14 H14 0.9500 . ? C15 C16 1.380(9) . ? C15 H15 0.9500 . ? C16 C17 1.384(8) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.367(10) . ? C18 C23 1.413(9) . ? C18 P3 1.824(5) . ? C19 C20 1.389(11) . ? C19 H19 0.9500 . ? C20 C21 1.412(18) . ? C20 H20 0.9500 . ? C21 C22 1.376(18) . ? C21 H21 0.9500 . ? C22 C23 1.399(10) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C25 1.381(8) . ? C24 C29 1.381(7) . ? C24 P2 1.855(5) . ? C25 C26 1.396(8) . ? C25 H25 0.9500 . ? C26 C27 1.370(9) . ? C26 H26 0.9500 . ? C27 C28 1.366(8) . ? C27 H27 0.9500 . ? C28 C29 1.370(7) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 C31 1.389(7) . ? C30 C35 1.393(7) . ? C30 P2 1.824(5) . ? C31 C32 1.384(7) . ? C31 H31 0.9500 . ? C32 C33 1.365(8) . ? C32 H32 0.9500 . ? C33 C34 1.385(8) . ? C33 H33 0.9500 . ? C34 C35 1.372(8) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C37 1.377(8) . ? C36 C41 1.399(7) . ? C36 P2 1.836(5) . ? C37 C38 1.399(9) . ? C37 H37 0.9500 . ? C38 C39 1.384(9) . ? C38 H38 0.9500 . ? C39 C40 1.361(9) . ? C39 H39 0.9500 . ? C40 C41 1.373(8) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 C43 1.306(7) . ? C43 C44 1.477(8) . ? C43 H43 0.9500 . ? C44 C47 1.338(8) . ? C44 C49 1.438(8) . ? C47 N1 1.377(8) . ? C47 H47 0.9500 . ? C48 O1 1.248(8) . ? C48 N1 1.333(8) . ? C48 N2 1.364(10) . ? C49 O2 1.220(7) . ? C49 N2 1.373(8) . ? F1 P4 1.532(7) . ? F2 P4 1.562(9) . ? F3 P4 1.578(7) . ? F4 P4 1.556(8) . ? F5 P5 1.556(4) . ? F6 P5 1.557(11) . ? F7 P5 1.570(11) . ? F8 P5 1.544(11) . ? N1 H1A 0.8800 . ? N2 H2A 0.8800 . ? P4 F1 1.532(7) 10_556 ? P4 F3 1.578(7) 10_556 ? P5 F6 1.557(11) 10_557 ? P5 F7 1.570(11) 10_557 ? 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 C42 Ru1 C2 91.8(3) . . ? C42 Ru1 C1 120.2(2) . . ? C2 Ru1 C1 36.1(3) . . ? C42 Ru1 C3 97.7(2) . . ? C2 Ru1 C3 36.6(2) . . ? C1 Ru1 C3 60.2(3) . . ? C42 Ru1 C5 152.9(2) . . ? C2 Ru1 C5 61.1(3) . . ? C1 Ru1 C5 36.6(2) . . ? C3 Ru1 C5 60.5(3) . . ? C42 Ru1 C4 130.8(3) . . ? C2 Ru1 C4 60.5(3) . . ? C1 Ru1 C4 60.1(3) . . ? C3 Ru1 C4 35.7(2) . . ? C5 Ru1 C4 36.3(2) . . ? C42 Ru1 P2 87.93(16) . . ? C2 Ru1 P2 112.67(19) . . ? C1 Ru1 P2 90.3(2) . . ? C3 Ru1 P2 148.55(18) . . ? C5 Ru1 P2 102.8(2) . . ? C4 Ru1 P2 138.7(2) . . ? C42 Ru1 P3 99.52(15) . . ? C2 Ru1 P3 147.53(17) . . ? C1 Ru1 P3 139.67(19) . . ? C3 Ru1 P3 111.22(17) . . ? C5 Ru1 P3 103.33(17) . . ? C4 Ru1 P3 89.81(18) . . ? P2 Ru1 P3 98.15(5) . . ? C2 C1 C5 109.6(7) . . ? C2 C1 Ru1 71.7(4) . . ? C5 C1 Ru1 73.0(3) . . ? C2 C1 H1 125.2 . . ? C5 C1 H1 125.2 . . ? Ru1 C1 H1 121.7 . . ? C1 C2 C3 107.5(7) . . ? C1 C2 Ru1 72.2(4) . . ? C3 C2 Ru1 73.1(3) . . ? C1 C2 H2 126.3 . . ? C3 C2 H2 126.3 . . ? Ru1 C2 H2 120.3 . . ? C4 C3 C2 107.8(7) . . ? C4 C3 Ru1 72.4(3) . . ? C2 C3 Ru1 70.3(3) . . ? C4 C3 H3 126.1 . . ? C2 C3 H3 126.1 . . ? Ru1 C3 H3 122.9 . . ? C3 C4 C5 109.1(6) . . ? C3 C4 Ru1 71.9(3) . . ? C5 C4 Ru1 71.7(3) . . ? C3 C4 H4 125.4 . . ? C5 C4 H4 125.4 . . ? Ru1 C4 H4 122.6 . . ? C4 C5 C1 105.9(7) . . ? C4 C5 Ru1 72.0(4) . . ? C1 C5 Ru1 70.4(3) . . ? C4 C5 H5 127.1 . . ? C1 C5 H5 127.1 . . ? Ru1 C5 H5 122.3 . . ? C7 C6 C11 117.1(5) . . ? C7 C6 P3 121.2(4) . . ? C11 C6 P3 121.1(4) . . ? C8 C7 C6 121.0(5) . . ? C8 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C9 C8 C7 121.0(6) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C8 C9 C10 119.8(6) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C9 C10 C11 120.4(6) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C10 C11 C6 120.7(6) . . ? C10 C11 H11 119.7 . . ? C6 C11 H11 119.7 . . ? C13 C12 C17 118.5(5) . . ? C13 C12 P3 120.1(4) . . ? C17 C12 P3 121.1(4) . . ? C12 C13 C14 121.2(5) . . ? C12 C13 H13 119.4 . . ? C14 C13 H13 119.4 . . ? C13 C14 C15 120.4(6) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C16 C15 C14 118.5(6) . . ? C16 C15 H15 120.7 . . ? C14 C15 H15 120.7 . . ? C15 C16 C17 121.2(5) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C16 C17 C12 120.1(5) . . ? C16 C17 H17 120.0 . . ? C12 C17 H17 120.0 . . ? C19 C18 C23 121.0(6) . . ? C19 C18 P3 119.5(6) . . ? C23 C18 P3 119.1(5) . . ? C18 C19 C20 121.3(9) . . ? C18 C19 H19 119.3 . . ? C20 C19 H19 119.3 . . ? C19 C20 C21 116.9(10) . . ? C19 C20 H20 121.5 . . ? C21 C20 H20 121.5 . . ? C22 C21 C20 123.1(8) . . ? C22 C21 H21 118.4 . . ? C20 C21 H21 118.4 . . ? C21 C22 C23 118.6(10) . . ? C21 C22 H22 120.7 . . ? C23 C22 H22 120.7 . . ? C22 C23 C18 119.0(8) . . ? C22 C23 H23 120.5 . . ? C18 C23 H23 120.5 . . ? C25 C24 C29 118.4(5) . . ? C25 C24 P2 120.4(4) . . ? C29 C24 P2 121.2(4) . . ? C24 C25 C26 120.5(6) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C27 C26 C25 120.0(6) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C28 C27 C26 119.2(5) . . ? C28 C27 H27 120.4 . . ? C26 C27 H27 120.4 . . ? C27 C28 C29 121.4(6) . . ? C27 C28 H28 119.3 . . ? C29 C28 H28 119.3 . . ? C28 C29 C24 120.5(5) . . ? C28 C29 H29 119.7 . . ? C24 C29 H29 119.7 . . ? C31 C30 C35 119.4(5) . . ? C31 C30 P2 118.3(4) . . ? C35 C30 P2 122.3(4) . . ? C32 C31 C30 120.0(5) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C33 C32 C31 120.6(5) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C32 C33 C34 119.4(5) . . ? C32 C33 H33 120.3 . . ? C34 C33 H33 120.3 . . ? C35 C34 C33 121.1(5) . . ? C35 C34 H34 119.5 . . ? C33 C34 H34 119.5 . . ? C34 C35 C30 119.5(5) . . ? C34 C35 H35 120.3 . . ? C30 C35 H35 120.3 . . ? C37 C36 C41 118.6(5) . . ? C37 C36 P2 118.8(4) . . ? C41 C36 P2 122.6(4) . . ? C36 C37 C38 120.6(6) . . ? C36 C37 H37 119.7 . . ? C38 C37 H37 119.7 . . ? C39 C38 C37 119.7(6) . . ? C39 C38 H38 120.1 . . ? C37 C38 H38 120.1 . . ? C40 C39 C38 119.4(6) . . ? C40 C39 H39 120.3 . . ? C38 C39 H39 120.3 . . ? C39 C40 C41 121.6(6) . . ? C39 C40 H40 119.2 . . ? C41 C40 H40 119.2 . . ? C40 C41 C36 120.1(6) . . ? C40 C41 H41 120.0 . . ? C36 C41 H41 120.0 . . ? C43 C42 Ru1 168.4(4) . . ? C42 C43 C44 129.8(5) . . ? C42 C43 H43 115.1 . . ? C44 C43 H43 115.1 . . ? C47 C44 C49 119.1(6) . . ? C47 C44 C43 121.9(5) . . ? C49 C44 C43 119.0(5) . . ? C44 C47 N1 121.7(6) . . ? C44 C47 H47 119.1 . . ? N1 C47 H47 119.1 . . ? O1 C48 N1 122.7(8) . . ? O1 C48 N2 120.9(6) . . ? N1 C48 N2 116.4(6) . . ? O2 C49 N2 119.6(6) . . ? O2 C49 C44 125.6(6) . . ? N2 C49 C44 114.8(6) . . ? C48 N1 C47 121.9(6) . . ? C48 N1 H1A 119.0 . . ? C47 N1 H1A 119.0 . . ? C48 N2 C49 126.0(5) . . ? C48 N2 H2A 117.0 . . ? C49 N2 H2A 117.0 . . ? C30 P2 C36 104.2(2) . . ? C30 P2 C24 101.9(2) . . ? C36 P2 C24 103.1(2) . . ? C30 P2 Ru1 120.76(16) . . ? C36 P2 Ru1 112.09(18) . . ? C24 P2 Ru1 112.87(18) . . ? C18 P3 C6 105.4(3) . . ? C18 P3 C12 102.8(2) . . ? C6 P3 C12 98.0(2) . . ? C18 P3 Ru1 111.8(2) . . ? C6 P3 Ru1 123.05(16) . . ? C12 P3 Ru1 113.25(17) . . ? F1 P4 F1 98.1(7) 10_556 . ? F1 P4 F4 88.3(4) 10_556 . ? F1 P4 F4 88.3(4) . . ? F1 P4 F2 89.0(4) 10_556 . ? F1 P4 F2 89.0(4) . . ? F4 P4 F2 176.0(7) . . ? F1 P4 F3 173.1(5) 10_556 . ? F1 P4 F3 88.8(4) . . ? F4 P4 F3 90.8(5) . . ? F2 P4 F3 92.1(4) . . ? F1 P4 F3 88.8(4) 10_556 10_556 ? F1 P4 F3 173.1(5) . 10_556 ? F4 P4 F3 90.8(5) . 10_556 ? F2 P4 F3 92.1(4) . 10_556 ? F3 P4 F3 84.4(6) . 10_556 ? F8 P5 F6 90.7(3) . . ? F8 P5 F6 90.7(3) . 10_557 ? F6 P5 F6 93.6(8) . 10_557 ? F8 P5 F5 178.8(5) . . ? F6 P5 F5 90.1(5) . . ? F6 P5 F5 90.2(2) 10_557 . ? F8 P5 F7 90.3(3) . 10_557 ? F6 P5 F7 177.0(7) . 10_557 ? F6 P5 F7 89.2(3) 10_557 10_557 ? F5 P5 F7 88.8(3) . 10_557 ? F8 P5 F7 90.3(3) . . ? F6 P5 F7 89.2(3) . . ? F6 P5 F7 177.0(7) 10_557 . ? F5 P5 F7 88.8(3) . . ? F7 P5 F7 87.9(7) 10_557 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C42 Ru1 C1 C2 42.6(5) . . . . ? C3 Ru1 C1 C2 -38.4(4) . . . . ? C5 Ru1 C1 C2 -118.1(6) . . . . ? C4 Ru1 C1 C2 -79.9(5) . . . . ? P2 Ru1 C1 C2 130.4(4) . . . . ? P3 Ru1 C1 C2 -126.7(4) . . . . ? C42 Ru1 C1 C5 160.7(4) . . . . ? C2 Ru1 C1 C5 118.1(6) . . . . ? C3 Ru1 C1 C5 79.7(5) . . . . ? C4 Ru1 C1 C5 38.2(5) . . . . ? P2 Ru1 C1 C5 -111.5(5) . . . . ? P3 Ru1 C1 C5 -8.6(7) . . . . ? C5 C1 C2 C3 1.5(7) . . . . ? Ru1 C1 C2 C3 65.0(4) . . . . ? C5 C1 C2 Ru1 -63.6(4) . . . . ? C42 Ru1 C2 C1 -144.2(4) . . . . ? C3 Ru1 C2 C1 115.3(6) . . . . ? C5 Ru1 C2 C1 36.9(4) . . . . ? C4 Ru1 C2 C1 78.7(5) . . . . ? P2 Ru1 C2 C1 -55.6(4) . . . . ? P3 Ru1 C2 C1 104.8(5) . . . . ? C42 Ru1 C2 C3 100.5(5) . . . . ? C1 Ru1 C2 C3 -115.3(6) . . . . ? C5 Ru1 C2 C3 -78.4(5) . . . . ? C4 Ru1 C2 C3 -36.7(4) . . . . ? P2 Ru1 C2 C3 -171.0(4) . . . . ? P3 Ru1 C2 C3 -10.5(8) . . . . ? C1 C2 C3 C4 -1.4(7) . . . . ? Ru1 C2 C3 C4 63.1(4) . . . . ? C1 C2 C3 Ru1 -64.4(4) . . . . ? C42 Ru1 C3 C4 160.3(4) . . . . ? C2 Ru1 C3 C4 -117.1(7) . . . . ? C1 Ru1 C3 C4 -79.2(5) . . . . ? C5 Ru1 C3 C4 -36.8(4) . . . . ? P2 Ru1 C3 C4 -101.0(4) . . . . ? P3 Ru1 C3 C4 56.9(4) . . . . ? C42 Ru1 C3 C2 -82.6(5) . . . . ? C1 Ru1 C3 C2 37.9(4) . . . . ? C5 Ru1 C3 C2 80.3(5) . . . . ? C4 Ru1 C3 C2 117.1(7) . . . . ? P2 Ru1 C3 C2 16.1(7) . . . . ? P3 Ru1 C3 C2 174.0(4) . . . . ? C2 C3 C4 C5 0.8(7) . . . . ? Ru1 C3 C4 C5 62.5(4) . . . . ? C2 C3 C4 Ru1 -61.7(4) . . . . ? C42 Ru1 C4 C3 -26.2(5) . . . . ? C2 Ru1 C4 C3 37.6(4) . . . . ? C1 Ru1 C4 C3 79.5(5) . . . . ? C5 Ru1 C4 C3 118.1(6) . . . . ? P2 Ru1 C4 C3 129.2(4) . . . . ? P3 Ru1 C4 C3 -128.7(4) . . . . ? C42 Ru1 C4 C5 -144.3(4) . . . . ? C2 Ru1 C4 C5 -80.4(5) . . . . ? C1 Ru1 C4 C5 -38.6(4) . . . . ? C3 Ru1 C4 C5 -118.1(6) . . . . ? P2 Ru1 C4 C5 11.1(6) . . . . ? P3 Ru1 C4 C5 113.2(4) . . . . ? C3 C4 C5 C1 0.1(7) . . . . ? Ru1 C4 C5 C1 62.7(4) . . . . ? C3 C4 C5 Ru1 -62.6(4) . . . . ? C2 C1 C5 C4 -1.0(7) . . . . ? Ru1 C1 C5 C4 -63.8(4) . . . . ? C2 C1 C5 Ru1 62.8(4) . . . . ? C42 Ru1 C5 C4 76.1(6) . . . . ? C2 Ru1 C5 C4 78.5(5) . . . . ? C1 Ru1 C5 C4 114.9(7) . . . . ? C3 Ru1 C5 C4 36.3(4) . . . . ? P2 Ru1 C5 C4 -172.5(4) . . . . ? P3 Ru1 C5 C4 -70.8(4) . . . . ? C42 Ru1 C5 C1 -38.8(8) . . . . ? C2 Ru1 C5 C1 -36.4(4) . . . . ? C3 Ru1 C5 C1 -78.6(5) . . . . ? C4 Ru1 C5 C1 -114.9(7) . . . . ? P2 Ru1 C5 C1 72.6(5) . . . . ? P3 Ru1 C5 C1 174.3(4) . . . . ? C11 C6 C7 C8 -2.2(8) . . . . ? P3 C6 C7 C8 -173.3(4) . . . . ? C6 C7 C8 C9 1.7(9) . . . . ? C7 C8 C9 C10 -0.3(11) . . . . ? C8 C9 C10 C11 -0.4(12) . . . . ? C9 C10 C11 C6 -0.2(11) . . . . ? C7 C6 C11 C10 1.4(9) . . . . ? P3 C6 C11 C10 172.6(5) . . . . ? C17 C12 C13 C14 -0.2(9) . . . . ? P3 C12 C13 C14 173.4(5) . . . . ? C12 C13 C14 C15 0.3(11) . . . . ? C13 C14 C15 C16 0.1(11) . . . . ? C14 C15 C16 C17 -0.5(11) . . . . ? C15 C16 C17 C12 0.7(10) . . . . ? C13 C12 C17 C16 -0.3(9) . . . . ? P3 C12 C17 C16 -173.8(5) . . . . ? C23 C18 C19 C20 -0.4(10) . . . . ? P3 C18 C19 C20 -173.1(6) . . . . ? C18 C19 C20 C21 1.7(13) . . . . ? C19 C20 C21 C22 -2.6(16) . . . . ? C20 C21 C22 C23 2.2(16) . . . . ? C21 C22 C23 C18 -0.7(12) . . . . ? C19 C18 C23 C22 -0.2(9) . . . . ? P3 C18 C23 C22 172.6(5) . . . . ? C29 C24 C25 C26 -0.2(8) . . . . ? P2 C24 C25 C26 178.7(4) . . . . ? C24 C25 C26 C27 0.5(9) . . . . ? C25 C26 C27 C28 0.0(9) . . . . ? C26 C27 C28 C29 -0.7(8) . . . . ? C27 C28 C29 C24 1.0(8) . . . . ? C25 C24 C29 C28 -0.6(7) . . . . ? P2 C24 C29 C28 -179.4(4) . . . . ? C35 C30 C31 C32 1.9(7) . . . . ? P2 C30 C31 C32 -178.5(4) . . . . ? C30 C31 C32 C33 -0.2(8) . . . . ? C31 C32 C33 C34 -1.8(9) . . . . ? C32 C33 C34 C35 2.0(9) . . . . ? C33 C34 C35 C30 -0.2(8) . . . . ? C31 C30 C35 C34 -1.7(7) . . . . ? P2 C30 C35 C34 178.7(4) . . . . ? C41 C36 C37 C38 -0.1(10) . . . . ? P2 C36 C37 C38 -177.6(6) . . . . ? C36 C37 C38 C39 0.8(12) . . . . ? C37 C38 C39 C40 -0.5(11) . . . . ? C38 C39 C40 C41 -0.7(11) . . . . ? C39 C40 C41 C36 1.4(10) . . . . ? C37 C36 C41 C40 -1.0(9) . . . . ? P2 C36 C41 C40 176.4(5) . . . . ? C2 Ru1 C42 C43 52(2) . . . . ? C1 Ru1 C42 C43 28(2) . . . . ? C3 Ru1 C42 C43 88(2) . . . . ? C5 Ru1 C42 C43 54(2) . . . . ? C4 Ru1 C42 C43 103(2) . . . . ? P2 Ru1 C42 C43 -61(2) . . . . ? P3 Ru1 C42 C43 -159(2) . . . . ? Ru1 C42 C43 C44 -157.4(19) . . . . ? C42 C43 C44 C47 -168.7(6) . . . . ? C42 C43 C44 C49 10.4(9) . . . . ? C49 C44 C47 N1 -2.0(10) . . . . ? C43 C44 C47 N1 177.1(6) . . . . ? C47 C44 C49 O2 179.2(7) . . . . ? C43 C44 C49 O2 0.1(10) . . . . ? C47 C44 C49 N2 1.3(10) . . . . ? C43 C44 C49 N2 -177.8(6) . . . . ? O1 C48 N1 C47 -176.6(9) . . . . ? N2 C48 N1 C47 1.9(12) . . . . ? C44 C47 N1 C48 0.3(11) . . . . ? O1 C48 N2 C49 175.9(9) . . . . ? N1 C48 N2 C49 -2.6(14) . . . . ? O2 C49 N2 C48 -177.0(8) . . . . ? C44 C49 N2 C48 1.0(12) . . . . ? C31 C30 P2 C36 -178.6(4) . . . . ? C35 C30 P2 C36 1.1(5) . . . . ? C31 C30 P2 C24 -71.5(4) . . . . ? C35 C30 P2 C24 108.1(4) . . . . ? C31 C30 P2 Ru1 54.4(4) . . . . ? C35 C30 P2 Ru1 -125.9(4) . . . . ? C37 C36 P2 C30 -76.3(5) . . . . ? C41 C36 P2 C30 106.2(5) . . . . ? C37 C36 P2 C24 177.6(5) . . . . ? C41 C36 P2 C24 0.2(5) . . . . ? C37 C36 P2 Ru1 55.9(6) . . . . ? C41 C36 P2 Ru1 -121.5(4) . . . . ? C25 C24 P2 C30 168.7(4) . . . . ? C29 C24 P2 C30 -12.5(5) . . . . ? C25 C24 P2 C36 -83.5(5) . . . . ? C29 C24 P2 C36 95.4(4) . . . . ? C25 C24 P2 Ru1 37.7(5) . . . . ? C29 C24 P2 Ru1 -143.4(4) . . . . ? C42 Ru1 P2 C30 -77.8(2) . . . . ? C2 Ru1 P2 C30 -168.9(3) . . . . ? C1 Ru1 P2 C30 162.0(3) . . . . ? C3 Ru1 P2 C30 -179.2(4) . . . . ? C5 Ru1 P2 C30 127.3(3) . . . . ? C4 Ru1 P2 C30 120.6(3) . . . . ? P3 Ru1 P2 C30 21.57(19) . . . . ? C42 Ru1 P2 C36 158.9(2) . . . . ? C2 Ru1 P2 C36 67.8(3) . . . . ? C1 Ru1 P2 C36 38.6(3) . . . . ? C3 Ru1 P2 C36 57.5(4) . . . . ? C5 Ru1 P2 C36 4.0(3) . . . . ? C4 Ru1 P2 C36 -2.7(3) . . . . ? P3 Ru1 P2 C36 -101.8(2) . . . . ? C42 Ru1 P2 C24 42.9(2) . . . . ? C2 Ru1 P2 C24 -48.2(3) . . . . ? C1 Ru1 P2 C24 -77.3(3) . . . . ? C3 Ru1 P2 C24 -58.5(4) . . . . ? C5 Ru1 P2 C24 -112.0(2) . . . . ? C4 Ru1 P2 C24 -118.7(3) . . . . ? P3 Ru1 P2 C24 142.27(17) . . . . ? C19 C18 P3 C6 -152.0(5) . . . . ? C23 C18 P3 C6 35.1(5) . . . . ? C19 C18 P3 C12 -49.8(5) . . . . ? C23 C18 P3 C12 137.3(5) . . . . ? C19 C18 P3 Ru1 72.0(5) . . . . ? C23 C18 P3 Ru1 -100.9(5) . . . . ? C7 C6 P3 C18 -155.0(4) . . . . ? C11 C6 P3 C18 34.2(5) . . . . ? C7 C6 P3 C12 99.3(4) . . . . ? C11 C6 P3 C12 -71.5(5) . . . . ? C7 C6 P3 Ru1 -25.3(5) . . . . ? C11 C6 P3 Ru1 163.9(4) . . . . ? C13 C12 P3 C18 156.9(5) . . . . ? C17 C12 P3 C18 -29.7(5) . . . . ? C13 C12 P3 C6 -95.2(5) . . . . ? C17 C12 P3 C6 78.2(5) . . . . ? C13 C12 P3 Ru1 36.1(5) . . . . ? C17 C12 P3 Ru1 -150.5(4) . . . . ? C42 Ru1 P3 C18 147.5(3) . . . . ? C2 Ru1 P3 C18 -103.6(5) . . . . ? C1 Ru1 P3 C18 -41.9(4) . . . . ? C3 Ru1 P3 C18 -110.3(3) . . . . ? C5 Ru1 P3 C18 -47.1(3) . . . . ? C4 Ru1 P3 C18 -81.1(3) . . . . ? P2 Ru1 P3 C18 58.2(2) . . . . ? C42 Ru1 P3 C6 20.5(3) . . . . ? C2 Ru1 P3 C6 129.4(5) . . . . ? C1 Ru1 P3 C6 -168.9(4) . . . . ? C3 Ru1 P3 C6 122.7(3) . . . . ? C5 Ru1 P3 C6 -174.1(3) . . . . ? C4 Ru1 P3 C6 152.0(3) . . . . ? P2 Ru1 P3 C6 -68.8(2) . . . . ? C42 Ru1 P3 C12 -96.9(2) . . . . ? C2 Ru1 P3 C12 12.0(5) . . . . ? C1 Ru1 P3 C12 73.7(4) . . . . ? C3 Ru1 P3 C12 5.3(3) . . . . ? C5 Ru1 P3 C12 68.5(3) . . . . ? C4 Ru1 P3 C12 34.5(3) . . . . ? P2 Ru1 P3 C12 173.81(19) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2A O1 0.88 1.83 2.699(7) 170.1 8_556 N1 H1A O2 0.88 2.01 2.868(7) 166.4 9_556 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 22.51 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.105 _refine_diff_density_min -1.666 _refine_diff_density_rms 0.085 # SQUEEZE RESULTS loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.009 -0.009 0.000 6141.0 1367.4 _platon_squeeze_details ; ;