Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Michael Ward' 'Zoe R. Bell' 'Timothy L. Easun' 'Ramune Rutkaite' 'Nail M. Shavaleev' 'Linda Swanson' _publ_contact_author_name 'Prof Michael Ward' _publ_contact_author_address ; Departmet of Chemistry University of Sheffield Dainton Building Brook Hill Sheffield S3 7HF UNITED KINGDOM ; _publ_contact_author_email M.D.WARD@SHEFFIELD.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Complexes of substituted derivatives of 2-(2-pyridyl)benzimidazole with Re(I), Ru(II) and Pt(II): structures, redox and luminescence properties ; data_test_1 _database_code_depnum_ccdc_archive 'CCDC 245715' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H10 Cl F5 N3 O3 Re' _chemical_formula_sum 'C22 H10 Cl F5 N3 O3 Re' _chemical_formula_weight 680.98 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3838(15) _cell_length_b 12.105(2) _cell_length_c 12.532(2) _cell_angle_alpha 99.044(15) _cell_angle_beta 111.359(17) _cell_angle_gamma 91.924(17) _cell_volume 1302.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 110 _cell_measurement_theta_min 0.43 _cell_measurement_theta_max 0.62 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.736 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 4.828 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.33 _exptl_absorpt_correction_T_max 0.62 _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 'CCD area detector' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean 8.2 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 13700 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5904 _reflns_number_gt 5269 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1998)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1998)' _computing_data_reduction 'Bruker SHELXTL (Bruker, 1998)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 1998)' _computing_structure_refinement 'Bruker SHELXTL (Bruker, 1998)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1998)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1998)' _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^)+(0.0227P)^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 5904 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0267 _refine_ls_R_factor_gt 0.0223 _refine_ls_wR_factor_ref 0.0514 _refine_ls_wR_factor_gt 0.0505 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.232559(13) 0.154302(10) 0.003083(11) 0.02091(4) Uani 1 1 d . . . Cl1 Cl 0.35267(9) 0.16034(6) -0.14411(7) 0.02920(17) Uani 1 1 d . . . F32 F 0.8611(2) 0.58392(19) 0.38524(17) 0.0439(5) Uani 1 1 d . . . F33 F 0.8923(3) 0.6207(2) 0.60993(18) 0.0582(7) Uani 1 1 d . . . F34 F 0.6423(3) 0.6540(2) 0.66795(18) 0.0643(7) Uani 1 1 d . . . F35 F 0.3620(3) 0.6541(2) 0.4984(2) 0.0620(7) Uani 1 1 d . . . F36 F 0.3286(2) 0.61702(19) 0.27393(18) 0.0452(5) Uani 1 1 d . . . O41 O 0.1036(3) 0.1567(2) 0.1952(2) 0.0370(6) Uani 1 1 d . . . O51 O -0.0964(3) 0.1268(2) -0.1813(2) 0.0438(6) Uani 1 1 d . . . O61 O 0.2276(3) -0.10122(19) -0.0149(2) 0.0377(6) Uani 1 1 d . . . N11 N 0.4684(3) 0.1901(2) 0.1313(2) 0.0227(5) Uani 1 1 d . . . N21 N 0.2857(3) 0.33434(19) 0.0337(2) 0.0196(5) Uani 1 1 d . . . N23 N 0.4460(3) 0.4902(2) 0.1195(2) 0.0217(5) Uani 1 1 d . . . C12 C 0.5302(3) 0.2995(2) 0.1693(3) 0.0211(6) Uani 1 1 d . . . C13 C 0.6776(3) 0.3269(3) 0.2514(3) 0.0275(7) Uani 1 1 d . . . H13A H 0.7197 0.4032 0.2774 0.033 Uiso 1 1 calc R . . C14 C 0.7640(4) 0.2413(3) 0.2959(3) 0.0312(7) Uani 1 1 d . . . H14A H 0.8653 0.2590 0.3528 0.037 Uiso 1 1 calc R . . C15 C 0.7019(4) 0.1326(3) 0.2573(3) 0.0331(8) Uani 1 1 d . . . H15A H 0.7595 0.0735 0.2867 0.040 Uiso 1 1 calc R . . C16 C 0.5543(4) 0.1090(3) 0.1752(3) 0.0298(7) Uani 1 1 d . . . H16A H 0.5116 0.0329 0.1486 0.036 Uiso 1 1 calc R . . C22 C 0.4232(3) 0.3769(2) 0.1110(2) 0.0198(6) Uani 1 1 d . . . C23 C 0.5774(3) 0.5712(3) 0.1949(3) 0.0236(6) Uani 1 1 d . . . H23A H 0.5669 0.6424 0.1645 0.028 Uiso 1 1 calc R . . H23B H 0.6728 0.5416 0.1910 0.028 Uiso 1 1 calc R . . C24 C 0.3112(3) 0.5204(3) 0.0393(3) 0.0222(6) Uani 1 1 d . . . C25 C 0.2719(4) 0.6255(3) 0.0094(3) 0.0264(7) Uani 1 1 d . . . H25A H 0.3382 0.6926 0.0472 0.032 Uiso 1 1 calc R . . C26 C 0.1302(4) 0.6246(3) -0.0786(3) 0.0295(7) Uani 1 1 d . . . H26A H 0.0985 0.6935 -0.1024 0.035 Uiso 1 1 calc R . . C27 C 0.0318(4) 0.5261(3) -0.1340(3) 0.0290(7) Uani 1 1 d . . . H27A H -0.0644 0.5299 -0.1942 0.035 Uiso 1 1 calc R . . C28 C 0.0713(3) 0.4232(3) -0.1032(3) 0.0250(6) Uani 1 1 d . . . H28A H 0.0049 0.3560 -0.1409 0.030 Uiso 1 1 calc R . . C29 C 0.2138(3) 0.4232(2) -0.0138(3) 0.0204(6) Uani 1 1 d . . . C31 C 0.5933(4) 0.5960(2) 0.3214(3) 0.0251(7) Uani 1 1 d . . . C32 C 0.7342(4) 0.6015(3) 0.4103(3) 0.0318(7) Uani 1 1 d . . . C33 C 0.7537(4) 0.6215(3) 0.5269(3) 0.0405(9) Uani 1 1 d . . . C34 C 0.6273(5) 0.6386(3) 0.5561(3) 0.0436(10) Uani 1 1 d . . . C35 C 0.4853(4) 0.6370(3) 0.4700(3) 0.0405(9) Uani 1 1 d . . . C36 C 0.4708(4) 0.6166(3) 0.3554(3) 0.0318(7) Uani 1 1 d . . . C41 C 0.1516(3) 0.1568(3) 0.1220(3) 0.0269(7) Uani 1 1 d . . . C51 C 0.0272(4) 0.1364(3) -0.1131(3) 0.0286(7) Uani 1 1 d . . . C61 C 0.2257(3) -0.0054(3) -0.0112(3) 0.0264(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 Re1 0.02117(7) 0.01580(7) 0.02490(7) 0.00350(5) 0.00791(5) -0.00077(4) Cl1 0.0377(4) 0.0205(4) 0.0345(4) 0.0042(3) 0.0198(4) 0.0015(3) F32 0.0295(10) 0.0588(14) 0.0381(12) -0.0019(11) 0.0115(9) -0.0042(10) F33 0.0473(13) 0.0824(19) 0.0286(12) 0.0019(12) 0.0004(10) -0.0140(12) F34 0.0753(17) 0.087(2) 0.0246(11) -0.0105(12) 0.0237(12) -0.0295(14) F35 0.0554(14) 0.0835(19) 0.0529(15) -0.0142(13) 0.0394(13) -0.0104(13) F36 0.0334(11) 0.0587(15) 0.0404(12) -0.0059(11) 0.0167(10) 0.0033(10) O41 0.0396(14) 0.0422(15) 0.0345(14) 0.0089(12) 0.0195(12) 0.0028(11) O51 0.0303(13) 0.0467(17) 0.0410(15) 0.0087(13) -0.0018(12) -0.0060(11) O61 0.0377(13) 0.0202(13) 0.0553(17) 0.0087(11) 0.0172(12) -0.0001(10) N11 0.0227(13) 0.0202(13) 0.0258(14) 0.0056(11) 0.0091(11) 0.0027(10) N21 0.0212(12) 0.0162(13) 0.0217(12) 0.0028(10) 0.0086(10) 0.0018(10) N23 0.0261(13) 0.0154(13) 0.0232(13) 0.0014(10) 0.0098(11) -0.0005(10) C12 0.0214(14) 0.0214(16) 0.0226(15) 0.0049(13) 0.0104(12) 0.0015(12) C13 0.0269(16) 0.0259(17) 0.0273(17) 0.0020(14) 0.0090(14) -0.0027(13) C14 0.0237(16) 0.0348(19) 0.0301(18) 0.0059(15) 0.0045(14) 0.0020(14) C15 0.0314(18) 0.0302(19) 0.037(2) 0.0098(16) 0.0097(15) 0.0090(14) C16 0.0312(17) 0.0216(17) 0.0356(19) 0.0094(15) 0.0099(15) 0.0026(13) C22 0.0231(14) 0.0179(15) 0.0206(15) 0.0030(12) 0.0110(12) -0.0006(11) C23 0.0281(16) 0.0193(15) 0.0232(16) 0.0004(13) 0.0115(13) -0.0055(12) C24 0.0277(16) 0.0218(16) 0.0212(15) 0.0051(13) 0.0134(13) 0.0029(12) C25 0.0327(17) 0.0196(16) 0.0304(18) 0.0038(14) 0.0160(14) 0.0038(13) C26 0.0350(18) 0.0244(17) 0.0362(19) 0.0124(15) 0.0185(16) 0.0099(14) C27 0.0272(16) 0.0318(19) 0.0308(18) 0.0105(15) 0.0117(14) 0.0083(14) C28 0.0237(15) 0.0249(17) 0.0251(16) 0.0016(13) 0.0090(13) 0.0009(12) C29 0.0247(15) 0.0178(15) 0.0226(15) 0.0060(12) 0.0123(13) 0.0042(12) C31 0.0307(16) 0.0188(16) 0.0243(16) -0.0022(13) 0.0120(13) -0.0074(12) C32 0.0322(17) 0.0314(19) 0.0286(18) -0.0028(15) 0.0120(15) -0.0083(14) C33 0.044(2) 0.046(2) 0.0219(18) -0.0043(16) 0.0071(16) -0.0166(17) C34 0.055(2) 0.045(2) 0.0277(19) -0.0083(17) 0.0199(18) -0.0181(19) C35 0.045(2) 0.041(2) 0.038(2) -0.0082(17) 0.0250(18) -0.0114(17) C36 0.0321(18) 0.0311(19) 0.0287(18) -0.0045(15) 0.0123(15) -0.0071(14) C41 0.0223(15) 0.0201(16) 0.0355(19) 0.0056(14) 0.0076(14) 0.0005(12) C51 0.0318(18) 0.0238(17) 0.0288(18) 0.0038(14) 0.0106(15) -0.0036(14) C61 0.0243(15) 0.0228(17) 0.0311(18) 0.0038(14) 0.0100(14) -0.0024(13) _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 Re1 C41 1.901(3) . ? Re1 C61 1.910(3) . ? Re1 C51 1.926(3) . ? Re1 N21 2.161(2) . ? Re1 N11 2.189(3) . ? Re1 Cl1 2.4960(8) . ? F32 C32 1.353(4) . ? F33 C33 1.339(4) . ? F34 C34 1.339(4) . ? F35 C35 1.342(4) . ? F36 C36 1.354(4) . ? O41 C41 1.159(4) . ? O51 C51 1.152(4) . ? O61 C61 1.154(4) . ? N11 C16 1.348(4) . ? N11 C12 1.366(4) . ? N21 C22 1.325(4) . ? N21 C29 1.387(4) . ? N23 C22 1.362(3) . ? N23 C24 1.402(4) . ? N23 C23 1.468(4) . ? C12 C13 1.381(4) . ? C12 C22 1.471(4) . ? C13 C14 1.396(4) . ? C13 H13A 0.9500 . ? C14 C15 1.360(5) . ? C14 H14A 0.9500 . ? C15 C16 1.379(4) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C23 C31 1.517(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C29 1.379(4) . ? C24 C25 1.405(4) . ? C25 C26 1.383(4) . ? C25 H25A 0.9500 . ? C26 C27 1.398(4) . ? C26 H26A 0.9500 . ? C27 C28 1.385(4) . ? C27 H27A 0.9500 . ? C28 C29 1.398(4) . ? C28 H28A 0.9500 . ? C31 C32 1.375(4) . ? C31 C36 1.381(4) . ? C32 C33 1.386(4) . ? C33 C34 1.376(5) . ? C34 C35 1.373(5) . ? C35 C36 1.372(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 C41 Re1 C61 88.23(13) . . ? C41 Re1 C51 90.22(13) . . ? C61 Re1 C51 88.90(13) . . ? C41 Re1 N21 95.05(11) . . ? C61 Re1 N21 169.41(10) . . ? C51 Re1 N21 101.13(12) . . ? C41 Re1 N11 91.82(11) . . ? C61 Re1 N11 96.06(11) . . ? C51 Re1 N11 174.70(11) . . ? N21 Re1 N11 73.82(9) . . ? C41 Re1 Cl1 176.26(9) . . ? C61 Re1 Cl1 94.06(9) . . ? C51 Re1 Cl1 92.78(9) . . ? N21 Re1 Cl1 82.18(6) . . ? N11 Re1 Cl1 85.00(7) . . ? C16 N11 C12 118.7(3) . . ? C16 N11 Re1 122.8(2) . . ? C12 N11 Re1 118.47(19) . . ? C22 N21 C29 106.6(2) . . ? C22 N21 Re1 117.37(19) . . ? C29 N21 Re1 135.9(2) . . ? C22 N23 C24 105.8(2) . . ? C22 N23 C23 130.7(3) . . ? C24 N23 C23 123.5(2) . . ? N11 C12 C13 120.8(3) . . ? N11 C12 C22 111.8(3) . . ? C13 C12 C22 127.3(3) . . ? C12 C13 C14 119.4(3) . . ? C12 C13 H13A 120.3 . . ? C14 C13 H13A 120.3 . . ? C15 C14 C13 119.5(3) . . ? C15 C14 H14A 120.3 . . ? C13 C14 H14A 120.3 . . ? C14 C15 C16 119.2(3) . . ? C14 C15 H15A 120.4 . . ? C16 C15 H15A 120.4 . . ? N11 C16 C15 122.4(3) . . ? N11 C16 H16A 118.8 . . ? C15 C16 H16A 118.8 . . ? N21 C22 N23 112.1(3) . . ? N21 C22 C12 118.5(3) . . ? N23 C22 C12 129.3(3) . . ? N23 C23 C31 114.0(2) . . ? N23 C23 H23A 108.7 . . ? C31 C23 H23A 108.7 . . ? N23 C23 H23B 108.7 . . ? C31 C23 H23B 108.7 . . ? H23A C23 H23B 107.6 . . ? C29 C24 N23 107.0(3) . . ? C29 C24 C25 122.4(3) . . ? N23 C24 C25 130.6(3) . . ? C26 C25 C24 115.5(3) . . ? C26 C25 H25A 122.2 . . ? C24 C25 H25A 122.2 . . ? C25 C26 C27 122.4(3) . . ? C25 C26 H26A 118.8 . . ? C27 C26 H26A 118.8 . . ? C28 C27 C26 121.5(3) . . ? C28 C27 H27A 119.2 . . ? C26 C27 H27A 119.2 . . ? C27 C28 C29 116.5(3) . . ? C27 C28 H28A 121.7 . . ? C29 C28 H28A 121.7 . . ? C24 C29 N21 108.5(3) . . ? C24 C29 C28 121.6(3) . . ? N21 C29 C28 129.9(3) . . ? C32 C31 C36 115.8(3) . . ? C32 C31 C23 121.0(3) . . ? C36 C31 C23 123.2(3) . . ? F32 C32 C31 119.9(3) . . ? F32 C32 C33 117.0(3) . . ? C31 C32 C33 123.0(3) . . ? F33 C33 C34 120.4(3) . . ? F33 C33 C32 120.7(3) . . ? C34 C33 C32 118.9(4) . . ? F34 C34 C35 120.2(3) . . ? F34 C34 C33 120.0(4) . . ? C35 C34 C33 119.8(3) . . ? F35 C35 C36 120.7(3) . . ? F35 C35 C34 119.8(3) . . ? C36 C35 C34 119.5(3) . . ? F36 C36 C35 117.2(3) . . ? F36 C36 C31 119.8(3) . . ? C35 C36 C31 123.0(3) . . ? O41 C41 Re1 178.8(3) . . ? O51 C51 Re1 178.9(3) . . ? O61 C61 Re1 176.7(3) . . ? 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 C41 Re1 N11 C16 86.3(2) . . . . ? C61 Re1 N11 C16 -2.1(2) . . . . ? N21 Re1 N11 C16 -178.9(2) . . . . ? Cl1 Re1 N11 C16 -95.7(2) . . . . ? C41 Re1 N11 C12 -92.8(2) . . . . ? C61 Re1 N11 C12 178.7(2) . . . . ? N21 Re1 N11 C12 1.89(19) . . . . ? Cl1 Re1 N11 C12 85.2(2) . . . . ? C41 Re1 N21 C22 89.1(2) . . . . ? C61 Re1 N21 C22 -18.6(7) . . . . ? C51 Re1 N21 C22 -179.7(2) . . . . ? N11 Re1 N21 C22 -1.30(19) . . . . ? Cl1 Re1 N21 C22 -88.34(19) . . . . ? C41 Re1 N21 C29 -96.2(3) . . . . ? C61 Re1 N21 C29 156.1(5) . . . . ? C51 Re1 N21 C29 -4.9(3) . . . . ? N11 Re1 N21 C29 173.4(3) . . . . ? Cl1 Re1 N21 C29 86.4(3) . . . . ? C16 N11 C12 C13 -0.2(4) . . . . ? Re1 N11 C12 C13 179.0(2) . . . . ? C16 N11 C12 C22 178.7(2) . . . . ? Re1 N11 C12 C22 -2.1(3) . . . . ? N11 C12 C13 C14 0.0(4) . . . . ? C22 C12 C13 C14 -178.8(3) . . . . ? C12 C13 C14 C15 0.3(5) . . . . ? C13 C14 C15 C16 -0.3(5) . . . . ? C12 N11 C16 C15 0.3(4) . . . . ? Re1 N11 C16 C15 -178.9(2) . . . . ? C14 C15 C16 N11 0.0(5) . . . . ? C29 N21 C22 N23 1.3(3) . . . . ? Re1 N21 C22 N23 177.49(17) . . . . ? C29 N21 C22 C12 -175.5(2) . . . . ? Re1 N21 C22 C12 0.7(3) . . . . ? C24 N23 C22 N21 -0.7(3) . . . . ? C23 N23 C22 N21 178.1(3) . . . . ? C24 N23 C22 C12 175.7(3) . . . . ? C23 N23 C22 C12 -5.5(5) . . . . ? N11 C12 C22 N21 1.0(4) . . . . ? C13 C12 C22 N21 179.8(3) . . . . ? N11 C12 C22 N23 -175.3(3) . . . . ? C13 C12 C22 N23 3.6(5) . . . . ? C22 N23 C23 C31 -72.9(4) . . . . ? C24 N23 C23 C31 105.8(3) . . . . ? C22 N23 C24 C29 -0.2(3) . . . . ? C23 N23 C24 C29 -179.1(2) . . . . ? C22 N23 C24 C25 -178.5(3) . . . . ? C23 N23 C24 C25 2.5(4) . . . . ? C29 C24 C25 C26 -1.3(4) . . . . ? N23 C24 C25 C26 176.9(3) . . . . ? C24 C25 C26 C27 0.4(4) . . . . ? C25 C26 C27 C28 0.1(5) . . . . ? C26 C27 C28 C29 0.3(4) . . . . ? N23 C24 C29 N21 0.9(3) . . . . ? C25 C24 C29 N21 179.5(2) . . . . ? N23 C24 C29 C28 -176.8(2) . . . . ? C25 C24 C29 C28 1.8(4) . . . . ? C22 N21 C29 C24 -1.4(3) . . . . ? Re1 N21 C29 C24 -176.49(19) . . . . ? C22 N21 C29 C28 176.1(3) . . . . ? Re1 N21 C29 C28 1.0(5) . . . . ? C27 C28 C29 C24 -1.2(4) . . . . ? C27 C28 C29 N21 -178.4(3) . . . . ? N23 C23 C31 C32 136.2(3) . . . . ? N23 C23 C31 C36 -45.0(4) . . . . ? C36 C31 C32 F32 -179.2(3) . . . . ? C23 C31 C32 F32 -0.3(5) . . . . ? C36 C31 C32 C33 2.6(5) . . . . ? C23 C31 C32 C33 -178.6(3) . . . . ? F32 C32 C33 F33 -1.5(5) . . . . ? C31 C32 C33 F33 176.8(3) . . . . ? F32 C32 C33 C34 -179.3(3) . . . . ? C31 C32 C33 C34 -1.0(6) . . . . ? F33 C33 C34 F34 -0.3(6) . . . . ? C32 C33 C34 F34 177.5(3) . . . . ? F33 C33 C34 C35 -178.7(4) . . . . ? C32 C33 C34 C35 -0.9(6) . . . . ? F34 C34 C35 F35 1.9(6) . . . . ? C33 C34 C35 F35 -179.7(3) . . . . ? F34 C34 C35 C36 -177.4(3) . . . . ? C33 C34 C35 C36 1.1(6) . . . . ? F35 C35 C36 F36 1.4(5) . . . . ? C34 C35 C36 F36 -179.4(3) . . . . ? F35 C35 C36 C31 -178.5(3) . . . . ? C34 C35 C36 C31 0.7(6) . . . . ? C32 C31 C36 F36 177.6(3) . . . . ? C23 C31 C36 F36 -1.1(5) . . . . ? C32 C31 C36 C35 -2.4(5) . . . . ? C23 C31 C36 C35 178.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.725 _refine_diff_density_min -0.640 _refine_diff_density_rms 0.099 #=END data_test_2 _database_code_depnum_ccdc_archive 'CCDC 245716' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H23 N5 Pt' _chemical_formula_sum 'C33 H23 N5 Pt' _chemical_formula_weight 684.65 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.2261(14) _cell_length_b 12.0913(19) _cell_length_c 22.271(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.635(12) _cell_angle_gamma 90.00 _cell_volume 3245.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 198 _cell_measurement_theta_min 0.796 _cell_measurement_theta_max 1 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.401 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 4.349 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.11 _exptl_absorpt_correction_T_max 0.18 _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 'CCD area detector' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean 8.2 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 20823 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_av_sigmaI/netI 0.0418 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7426 _reflns_number_gt 6063 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1998)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1998)' _computing_data_reduction 'Bruker SHELXTL (Bruker, 1998)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 1998)' _computing_structure_refinement 'Bruker SHELXTL (Bruker, 1998)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1998)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1998)' _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^)+(0.0351P)^2^+1.6351P] 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 7426 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0390 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0744 _refine_ls_wR_factor_gt 0.0717 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.006 _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 Pt1 Pt 1.031027(11) 1.081708(12) -0.096968(6) 0.01970(5) Uani 1 1 d . . . N11 N 1.1300(2) 1.1503(3) -0.02138(14) 0.0213(6) Uani 1 1 d . . . N21 N 1.0981(3) 0.9432(2) -0.05078(14) 0.0212(7) Uani 1 1 d . . . N23 N 1.1987(2) 0.8676(3) 0.03197(13) 0.0215(6) Uani 1 1 d . . . N44 N 0.6767(3) 0.9198(3) -0.23525(18) 0.0411(9) Uani 1 1 d . . . N54 N 0.7698(3) 1.4275(3) -0.14939(15) 0.0314(8) Uani 1 1 d . . . C12 C 1.1417(3) 1.2602(3) -0.01045(17) 0.0277(8) Uani 1 1 d . . . H12A H 1.1060 1.3108 -0.0401 0.033 Uiso 1 1 calc R . . C13 C 1.2039(4) 1.3013(4) 0.0426(2) 0.0341(10) Uani 1 1 d . . . H13A H 1.2117 1.3788 0.0488 0.041 Uiso 1 1 calc R . . C14 C 1.2546(3) 1.2286(3) 0.08627(18) 0.0315(9) Uani 1 1 d . . . H14A H 1.2971 1.2554 0.1230 0.038 Uiso 1 1 calc R . . C15 C 1.2428(3) 1.1165(3) 0.07593(18) 0.0250(8) Uani 1 1 d . . . H15A H 1.2767 1.0654 0.1057 0.030 Uiso 1 1 calc R . . C16 C 1.1816(3) 1.0788(3) 0.02204(17) 0.0215(7) Uani 1 1 d . . . C22 C 1.1620(3) 0.9628(3) 0.00266(15) 0.0175(7) Uani 1 1 d . . . C23 C 1.2749(3) 0.8521(3) 0.09021(16) 0.0230(8) Uani 1 1 d . . . H23A H 1.2719 0.7739 0.1030 0.028 Uiso 1 1 calc R . . H23B H 1.2496 0.8986 0.1218 0.028 Uiso 1 1 calc R . . C24 C 1.1527(3) 0.7808(3) -0.00587(17) 0.0249(8) Uani 1 1 d . . . C25 C 1.1613(4) 0.6669(3) 0.00245(19) 0.0316(9) Uani 1 1 d . . . H25A H 1.2029 0.6344 0.0379 0.038 Uiso 1 1 calc R . . C26 C 1.1044(4) 0.6044(4) -0.0449(2) 0.0405(11) Uani 1 1 d . . . H26A H 1.1060 0.5262 -0.0413 0.049 Uiso 1 1 calc R . . C27 C 1.0451(4) 0.6514(4) -0.09741(19) 0.0371(10) Uani 1 1 d . . . H27A H 1.0101 0.6040 -0.1289 0.045 Uiso 1 1 calc R . . C28 C 1.0354(3) 0.7630(4) -0.10544(18) 0.0306(9) Uani 1 1 d . . . H28A H 0.9933 0.7947 -0.1410 0.037 Uiso 1 1 calc R . . C29 C 1.0918(3) 0.8289(3) -0.05739(17) 0.0234(8) Uani 1 1 d . . . C31 C 1.3941(3) 0.8820(3) 0.08578(17) 0.0235(8) Uani 1 1 d . . . C32 C 1.4581(3) 0.9399(4) 0.13228(19) 0.0323(10) Uani 1 1 d . . . H32A H 1.4268 0.9627 0.1665 0.039 Uiso 1 1 calc R . . C33 C 1.5689(4) 0.9652(4) 0.1295(2) 0.0384(10) Uani 1 1 d . . . H33A H 1.6123 1.0045 0.1620 0.046 Uiso 1 1 calc R . . C34 C 1.6149(4) 0.9338(4) 0.0804(2) 0.0413(11) Uani 1 1 d . . . H34A H 1.6901 0.9512 0.0786 0.050 Uiso 1 1 calc R . . C35 C 1.5511(4) 0.8764(4) 0.0334(2) 0.0391(11) Uani 1 1 d . . . H35A H 1.5829 0.8535 -0.0007 0.047 Uiso 1 1 calc R . . C36 C 1.4409(3) 0.8521(4) 0.03560(19) 0.0319(9) Uani 1 1 d . . . H36A H 1.3973 0.8146 0.0025 0.038 Uiso 1 1 calc R . . C41 C 0.9334(3) 1.0085(3) -0.16316(17) 0.0240(8) Uani 1 1 d . . . C42 C 0.8643(3) 0.9646(4) -0.20168(18) 0.0272(8) Uani 1 1 d . . . C43 C 0.7821(3) 0.9112(3) -0.24515(18) 0.0277(8) Uani 1 1 d . . . C45 C 0.5967(4) 0.8722(4) -0.2767(2) 0.0473(12) Uani 1 1 d . . . H45A H 0.5219 0.8787 -0.2707 0.057 Uiso 1 1 calc R . . C46 C 0.6176(4) 0.8153(4) -0.3267(2) 0.0414(11) Uani 1 1 d . . . H46A H 0.5585 0.7837 -0.3545 0.050 Uiso 1 1 calc R . . C47 C 0.7256(4) 0.8046(4) -0.3361(2) 0.0433(12) Uani 1 1 d . . . H47A H 0.7427 0.7645 -0.3700 0.052 Uiso 1 1 calc R . . C48 C 0.8085(4) 0.8539(4) -0.2947(2) 0.0376(10) Uani 1 1 d . . . H48A H 0.8837 0.8485 -0.3004 0.045 Uiso 1 1 calc R . . C51 C 0.9672(3) 1.2203(3) -0.13233(17) 0.0254(8) Uani 1 1 d . . . C52 C 0.9198(3) 1.3036(3) -0.15157(17) 0.0256(8) Uani 1 1 d . . . C53 C 0.8578(3) 1.3985(3) -0.17542(17) 0.0256(8) Uani 1 1 d . . . C55 C 0.7108(4) 1.5159(4) -0.17240(19) 0.0361(10) Uani 1 1 d . . . H55A H 0.6485 1.5365 -0.1545 0.043 Uiso 1 1 calc R . . C56 C 0.7346(4) 1.5789(4) -0.2204(2) 0.0400(11) Uani 1 1 d . . . H56A H 0.6902 1.6410 -0.2348 0.048 Uiso 1 1 calc R . . C57 C 0.8240(4) 1.5491(4) -0.2464(2) 0.0409(11) Uani 1 1 d . . . H57A H 0.8430 1.5910 -0.2793 0.049 Uiso 1 1 calc R . . C58 C 0.8863(4) 1.4582(4) -0.22492(18) 0.0336(10) Uani 1 1 d . . . H58A H 0.9477 1.4361 -0.2432 0.040 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 Pt1 0.01790(8) 0.02273(8) 0.01849(8) 0.00216(6) 0.00308(5) 0.00136(6) N11 0.0186(15) 0.0225(17) 0.0233(16) 0.0022(13) 0.0047(13) -0.0042(12) N21 0.0227(16) 0.0177(16) 0.0221(16) 0.0038(12) 0.0009(13) 0.0024(12) N23 0.0196(16) 0.0239(17) 0.0218(16) 0.0024(13) 0.0057(13) 0.0025(12) N44 0.029(2) 0.050(2) 0.044(2) -0.0074(19) 0.0047(17) -0.0004(17) N54 0.0330(19) 0.034(2) 0.0277(18) 0.0016(15) 0.0058(15) 0.0031(15) C12 0.030(2) 0.023(2) 0.029(2) 0.0045(17) 0.0005(16) 0.0009(17) C13 0.035(2) 0.024(2) 0.041(2) -0.0034(18) 0.001(2) -0.0049(17) C14 0.026(2) 0.038(3) 0.029(2) -0.0129(18) -0.0026(16) -0.0054(17) C15 0.0213(19) 0.026(2) 0.028(2) 0.0036(16) 0.0041(16) 0.0036(15) C16 0.0154(17) 0.0263(19) 0.0234(18) 0.0057(16) 0.0055(14) 0.0003(14) C22 0.0124(16) 0.0234(18) 0.0176(17) 0.0003(14) 0.0048(13) 0.0023(14) C23 0.0212(19) 0.029(2) 0.0183(18) 0.0052(15) 0.0022(15) 0.0060(15) C24 0.024(2) 0.027(2) 0.0242(19) -0.0017(15) 0.0064(16) 0.0013(15) C25 0.035(2) 0.027(2) 0.032(2) 0.0046(18) 0.0044(18) 0.0025(18) C26 0.053(3) 0.021(2) 0.046(3) -0.0019(19) 0.006(2) 0.0014(19) C27 0.043(3) 0.028(2) 0.037(2) -0.0043(19) -0.002(2) 0.0008(18) C28 0.033(2) 0.027(2) 0.031(2) -0.0027(17) 0.0015(17) 0.0024(17) C29 0.025(2) 0.021(2) 0.0256(19) 0.0002(15) 0.0068(16) 0.0017(15) C31 0.0212(19) 0.027(2) 0.0235(19) 0.0102(16) 0.0064(15) 0.0078(15) C32 0.027(2) 0.043(3) 0.028(2) 0.0038(18) 0.0049(17) 0.0056(18) C33 0.030(2) 0.043(3) 0.040(3) 0.007(2) -0.0019(19) -0.002(2) C34 0.026(2) 0.045(3) 0.054(3) 0.019(2) 0.012(2) 0.0056(19) C35 0.037(3) 0.044(3) 0.042(3) 0.003(2) 0.023(2) 0.005(2) C36 0.032(2) 0.036(2) 0.029(2) 0.0000(18) 0.0097(18) 0.0037(18) C41 0.0236(19) 0.027(2) 0.0228(19) 0.0028(16) 0.0091(16) 0.0041(15) C42 0.024(2) 0.033(2) 0.026(2) 0.0005(17) 0.0048(16) 0.0028(17) C43 0.030(2) 0.028(2) 0.0248(19) 0.0010(17) 0.0019(16) 0.0014(17) C45 0.029(2) 0.052(3) 0.059(3) 0.002(3) 0.002(2) -0.006(2) C46 0.038(3) 0.039(3) 0.040(3) 0.001(2) -0.012(2) -0.008(2) C47 0.054(3) 0.045(3) 0.030(2) -0.010(2) 0.003(2) -0.017(2) C48 0.032(2) 0.047(3) 0.034(2) -0.007(2) 0.0060(19) -0.005(2) C51 0.026(2) 0.029(2) 0.0215(18) 0.0046(16) 0.0050(16) -0.0019(16) C52 0.026(2) 0.030(2) 0.0210(19) 0.0056(16) 0.0055(16) -0.0011(16) C53 0.027(2) 0.024(2) 0.0235(19) 0.0033(15) 0.0002(16) -0.0011(15) C55 0.040(3) 0.035(3) 0.034(2) 0.0002(19) 0.009(2) 0.0092(19) C56 0.051(3) 0.036(3) 0.030(2) 0.0056(19) -0.002(2) 0.011(2) C57 0.054(3) 0.040(3) 0.029(2) 0.015(2) 0.008(2) 0.004(2) C58 0.035(2) 0.039(2) 0.027(2) 0.0092(18) 0.0051(18) 0.0034(19) _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 Pt1 C41 1.947(4) . ? Pt1 C51 1.958(4) . ? Pt1 N21 2.062(3) . ? Pt1 N11 2.075(3) . ? N11 C12 1.354(5) . ? N11 C16 1.369(5) . ? N21 C22 1.331(4) . ? N21 C29 1.391(5) . ? N23 C22 1.362(5) . ? N23 C24 1.403(5) . ? N23 C23 1.477(4) . ? N44 C43 1.347(5) . ? N44 C45 1.355(6) . ? N54 C55 1.343(5) . ? N54 C53 1.351(5) . ? C12 C13 1.385(5) . ? C12 H12A 0.9500 . ? C13 C14 1.379(6) . ? C13 H13A 0.9500 . ? C14 C15 1.378(5) . ? C14 H14A 0.9500 . ? C15 C16 1.381(5) . ? C15 H15A 0.9500 . ? C16 C22 1.475(5) . ? C23 C31 1.521(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C29 1.387(5) . ? C24 C25 1.392(6) . ? C25 C26 1.385(6) . ? C25 H25A 0.9500 . ? C26 C27 1.391(6) . ? C26 H26A 0.9500 . ? C27 C28 1.364(6) . ? C27 H27A 0.9500 . ? C28 C29 1.417(5) . ? C28 H28A 0.9500 . ? C31 C32 1.380(6) . ? C31 C36 1.386(5) . ? C32 C33 1.400(6) . ? C32 H32A 0.9500 . ? C33 C34 1.364(6) . ? C33 H33A 0.9500 . ? C34 C35 1.384(7) . ? C34 H34A 0.9500 . ? C35 C36 1.387(6) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C41 C42 1.220(5) . ? C42 C43 1.428(6) . ? C43 C48 1.387(6) . ? C45 C46 1.368(7) . ? C45 H45A 0.9500 . ? C46 C47 1.377(7) . ? C46 H46A 0.9500 . ? C47 C48 1.386(6) . ? C47 H47A 0.9500 . ? C48 H48A 0.9500 . ? C51 C52 1.205(5) . ? C52 C53 1.427(5) . ? C53 C58 1.410(5) . ? C55 C56 1.383(6) . ? C55 H55A 0.9500 . ? C56 C57 1.369(7) . ? C56 H56A 0.9500 . ? C57 C58 1.377(6) . ? C57 H57A 0.9500 . ? C58 H58A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C41 Pt1 C51 86.08(16) . . ? C41 Pt1 N21 98.68(14) . . ? C51 Pt1 N21 173.91(14) . . ? C41 Pt1 N11 175.08(13) . . ? C51 Pt1 N11 97.10(14) . . ? N21 Pt1 N11 77.91(12) . . ? C12 N11 C16 118.1(3) . . ? C12 N11 Pt1 124.6(3) . . ? C16 N11 Pt1 117.2(2) . . ? C22 N21 C29 106.6(3) . . ? C22 N21 Pt1 115.2(2) . . ? C29 N21 Pt1 138.1(3) . . ? C22 N23 C24 106.1(3) . . ? C22 N23 C23 129.6(3) . . ? C24 N23 C23 124.2(3) . . ? C43 N44 C45 117.2(4) . . ? C55 N54 C53 117.3(4) . . ? N11 C12 C13 122.1(4) . . ? N11 C12 H12A 119.0 . . ? C13 C12 H12A 119.0 . . ? C14 C13 C12 119.4(4) . . ? C14 C13 H13A 120.3 . . ? C12 C13 H13A 120.3 . . ? C15 C14 C13 119.1(4) . . ? C15 C14 H14A 120.4 . . ? C13 C14 H14A 120.4 . . ? C14 C15 C16 119.7(4) . . ? C14 C15 H15A 120.1 . . ? C16 C15 H15A 120.1 . . ? N11 C16 C15 121.6(3) . . ? N11 C16 C22 111.1(3) . . ? C15 C16 C22 127.3(3) . . ? N21 C22 N23 112.0(3) . . ? N21 C22 C16 118.2(3) . . ? N23 C22 C16 129.7(3) . . ? N23 C23 C31 112.5(3) . . ? N23 C23 H23A 109.1 . . ? C31 C23 H23A 109.1 . . ? N23 C23 H23B 109.1 . . ? C31 C23 H23B 109.1 . . ? H23A C23 H23B 107.8 . . ? C29 C24 C25 122.9(4) . . ? C29 C24 N23 106.8(3) . . ? C25 C24 N23 130.3(4) . . ? C26 C25 C24 114.9(4) . . ? C26 C25 H25A 122.5 . . ? C24 C25 H25A 122.5 . . ? C25 C26 C27 122.8(4) . . ? C25 C26 H26A 118.6 . . ? C27 C26 H26A 118.6 . . ? C28 C27 C26 122.4(4) . . ? C28 C27 H27A 118.8 . . ? C26 C27 H27A 118.8 . . ? C27 C28 C29 115.8(4) . . ? C27 C28 H28A 122.1 . . ? C29 C28 H28A 122.1 . . ? C24 C29 N21 108.4(3) . . ? C24 C29 C28 121.1(4) . . ? N21 C29 C28 130.5(3) . . ? C32 C31 C36 118.6(4) . . ? C32 C31 C23 120.1(3) . . ? C36 C31 C23 121.3(4) . . ? C31 C32 C33 120.6(4) . . ? C31 C32 H32A 119.7 . . ? C33 C32 H32A 119.7 . . ? C34 C33 C32 120.5(4) . . ? C34 C33 H33A 119.8 . . ? C32 C33 H33A 119.8 . . ? C33 C34 C35 119.3(4) . . ? C33 C34 H34A 120.3 . . ? C35 C34 H34A 120.3 . . ? C34 C35 C36 120.5(4) . . ? C34 C35 H35A 119.7 . . ? C36 C35 H35A 119.7 . . ? C31 C36 C35 120.5(4) . . ? C31 C36 H36A 119.8 . . ? C35 C36 H36A 119.8 . . ? C42 C41 Pt1 174.0(3) . . ? C41 C42 C43 178.1(4) . . ? N44 C43 C48 121.7(4) . . ? N44 C43 C42 116.0(4) . . ? C48 C43 C42 122.3(4) . . ? N44 C45 C46 123.8(5) . . ? N44 C45 H45A 118.1 . . ? C46 C45 H45A 118.1 . . ? C45 C46 C47 119.0(4) . . ? C45 C46 H46A 120.5 . . ? C47 C46 H46A 120.5 . . ? C46 C47 C48 118.1(4) . . ? C46 C47 H47A 120.9 . . ? C48 C47 H47A 120.9 . . ? C47 C48 C43 120.1(4) . . ? C47 C48 H48A 119.9 . . ? C43 C48 H48A 119.9 . . ? C52 C51 Pt1 174.1(3) . . ? C51 C52 C53 176.6(4) . . ? N54 C53 C58 121.4(4) . . ? N54 C53 C52 117.4(3) . . ? C58 C53 C52 121.2(4) . . ? N54 C55 C56 124.4(4) . . ? N54 C55 H55A 117.8 . . ? C56 C55 H55A 117.8 . . ? C57 C56 C55 117.9(4) . . ? C57 C56 H56A 121.0 . . ? C55 C56 H56A 121.0 . . ? C56 C57 C58 119.9(4) . . ? C56 C57 H57A 120.1 . . ? C58 C57 H57A 120.1 . . ? C57 C58 C53 119.1(4) . . ? C57 C58 H58A 120.5 . . ? C53 C58 H58A 120.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C51 Pt1 N11 C12 -4.1(3) . . . . ? N21 Pt1 N11 C12 179.5(3) . . . . ? C51 Pt1 N11 C16 171.8(3) . . . . ? N21 Pt1 N11 C16 -4.6(2) . . . . ? C41 Pt1 N21 C22 -172.8(3) . . . . ? N11 Pt1 N21 C22 3.6(2) . . . . ? C41 Pt1 N21 C29 2.5(4) . . . . ? N11 Pt1 N21 C29 178.9(4) . . . . ? C16 N11 C12 C13 0.3(6) . . . . ? Pt1 N11 C12 C13 176.2(3) . . . . ? N11 C12 C13 C14 -1.0(6) . . . . ? C12 C13 C14 C15 0.5(6) . . . . ? C13 C14 C15 C16 0.6(6) . . . . ? C12 N11 C16 C15 0.8(5) . . . . ? Pt1 N11 C16 C15 -175.4(3) . . . . ? C12 N11 C16 C22 -179.2(3) . . . . ? Pt1 N11 C16 C22 4.7(4) . . . . ? C14 C15 C16 N11 -1.3(6) . . . . ? C14 C15 C16 C22 178.7(4) . . . . ? C29 N21 C22 N23 0.1(4) . . . . ? Pt1 N21 C22 N23 176.8(2) . . . . ? C29 N21 C22 C16 -179.0(3) . . . . ? Pt1 N21 C22 C16 -2.3(4) . . . . ? C24 N23 C22 N21 -0.9(4) . . . . ? C23 N23 C22 N21 176.7(3) . . . . ? C24 N23 C22 C16 178.1(3) . . . . ? C23 N23 C22 C16 -4.3(6) . . . . ? N11 C16 C22 N21 -1.5(4) . . . . ? C15 C16 C22 N21 178.5(3) . . . . ? N11 C16 C22 N23 179.5(3) . . . . ? C15 C16 C22 N23 -0.5(6) . . . . ? C22 N23 C23 C31 -70.8(5) . . . . ? C24 N23 C23 C31 106.4(4) . . . . ? C22 N23 C24 C29 1.3(4) . . . . ? C23 N23 C24 C29 -176.5(3) . . . . ? C22 N23 C24 C25 -178.5(4) . . . . ? C23 N23 C24 C25 3.7(6) . . . . ? C29 C24 C25 C26 0.2(6) . . . . ? N23 C24 C25 C26 -180.0(4) . . . . ? C24 C25 C26 C27 1.3(7) . . . . ? C25 C26 C27 C28 -2.3(8) . . . . ? C26 C27 C28 C29 1.5(7) . . . . ? C25 C24 C29 N21 178.6(4) . . . . ? N23 C24 C29 N21 -1.3(4) . . . . ? C25 C24 C29 C28 -0.9(6) . . . . ? N23 C24 C29 C28 179.2(3) . . . . ? C22 N21 C29 C24 0.7(4) . . . . ? Pt1 N21 C29 C24 -174.8(3) . . . . ? C22 N21 C29 C28 -179.8(4) . . . . ? Pt1 N21 C29 C28 4.6(7) . . . . ? C27 C28 C29 C24 0.1(6) . . . . ? C27 C28 C29 N21 -179.3(4) . . . . ? N23 C23 C31 C32 138.4(4) . . . . ? N23 C23 C31 C36 -41.7(5) . . . . ? C36 C31 C32 C33 -1.7(6) . . . . ? C23 C31 C32 C33 178.2(4) . . . . ? C31 C32 C33 C34 0.6(7) . . . . ? C32 C33 C34 C35 -0.1(7) . . . . ? C33 C34 C35 C36 0.8(7) . . . . ? C32 C31 C36 C35 2.3(6) . . . . ? C23 C31 C36 C35 -177.6(4) . . . . ? C34 C35 C36 C31 -1.9(7) . . . . ? C45 N44 C43 C48 -1.5(7) . . . . ? C45 N44 C43 C42 178.4(4) . . . . ? C43 N44 C45 C46 1.1(7) . . . . ? N44 C45 C46 C47 0.2(8) . . . . ? C45 C46 C47 C48 -1.1(7) . . . . ? C46 C47 C48 C43 0.7(7) . . . . ? N44 C43 C48 C47 0.7(7) . . . . ? C42 C43 C48 C47 -179.2(4) . . . . ? C55 N54 C53 C58 -0.3(6) . . . . ? C55 N54 C53 C52 -179.2(4) . . . . ? C53 N54 C55 C56 -0.4(7) . . . . ? N54 C55 C56 C57 0.3(7) . . . . ? C55 C56 C57 C58 0.5(7) . . . . ? C56 C57 C58 C53 -1.1(7) . . . . ? N54 C53 C58 C57 1.0(6) . . . . ? C52 C53 C58 C57 179.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 3.996 _refine_diff_density_min -0.668 _refine_diff_density_rms 0.122 #=END data_test _database_code_depnum_ccdc_archive 'CCDC 245717' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H19 Cl N3 O3 Re, C4 H8 O' _chemical_formula_sum 'C36 H27 Cl N3 O4 Re' _chemical_formula_weight 787.26 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.055(2) _cell_length_b 12.376(3) _cell_length_c 13.047(2) _cell_angle_alpha 108.288(14) _cell_angle_beta 100.199(15) _cell_angle_gamma 99.195(13) _cell_volume 1770.0(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 118 _cell_measurement_theta_min 0.588 _cell_measurement_theta_max 0.7 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.477 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 3.548 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.48 _exptl_absorpt_correction_T_max 0.70 _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 'CCD area detector' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean 8.2 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 18904 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_sigmaI/netI 0.0525 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 27.52 _reflns_number_total 8044 _reflns_number_gt 6832 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1998)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1998)' _computing_data_reduction 'Bruker SHELXTL (Bruker, 1998)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 1998)' _computing_structure_refinement 'Bruker SHELXTL (Bruker, 1998)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1998)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1998)' _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^)+(0.0324P)^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 8044 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0375 _refine_ls_R_factor_gt 0.0284 _refine_ls_wR_factor_ref 0.0668 _refine_ls_wR_factor_gt 0.0647 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.976 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.419019(11) 0.222275(12) 0.686018(12) 0.02419(5) Uani 1 1 d . . . Cl1 Cl 0.60695(7) 0.26683(8) 0.63688(8) 0.03033(19) Uani 1 1 d . . . O31 O 0.1849(2) 0.1686(3) 0.7417(3) 0.0523(8) Uani 1 1 d . . . O41 O 0.4682(3) 0.0051(3) 0.7347(3) 0.0607(9) Uani 1 1 d . . . O51 O 0.5144(3) 0.3597(3) 0.9363(2) 0.0517(8) Uani 1 1 d . . . N11 N 0.3498(2) 0.1405(2) 0.5047(3) 0.0266(6) Uani 1 1 d . . . N21 N 0.3836(2) 0.3616(2) 0.6274(2) 0.0221(6) Uani 1 1 d . . . N23 N 0.3489(2) 0.4307(2) 0.4892(2) 0.0229(6) Uani 1 1 d . . . C12 C 0.3209(3) 0.2099(3) 0.4459(3) 0.0255(7) Uani 1 1 d . . . C13 C 0.2685(3) 0.1643(3) 0.3337(3) 0.0319(8) Uani 1 1 d . . . H13A H 0.2475 0.2142 0.2949 0.038 Uiso 1 1 calc R . . C14 C 0.2470(3) 0.0442(3) 0.2779(3) 0.0390(9) Uani 1 1 d . . . H14A H 0.2099 0.0110 0.2009 0.047 Uiso 1 1 calc R . . C15 C 0.2798(3) -0.0256(3) 0.3353(3) 0.0394(9) Uani 1 1 d . . . H15A H 0.2680 -0.1074 0.2981 0.047 Uiso 1 1 calc R . . C16 C 0.3302(3) 0.0244(3) 0.4478(3) 0.0336(8) Uani 1 1 d . . . H16A H 0.3520 -0.0248 0.4871 0.040 Uiso 1 1 calc R . . C22 C 0.3500(3) 0.3337(3) 0.5178(3) 0.0221(7) Uani 1 1 d . . . C23 C 0.3241(3) 0.4393(3) 0.3774(3) 0.0238(7) Uani 1 1 d . . . H23A H 0.3537 0.3791 0.3266 0.029 Uiso 1 1 calc R . . H23B H 0.3660 0.5169 0.3817 0.029 Uiso 1 1 calc R . . C24 C 0.3834(3) 0.5272(3) 0.5887(3) 0.0215(7) Uani 1 1 d . . . C25 C 0.3993(3) 0.6470(3) 0.6082(3) 0.0267(7) Uani 1 1 d . . . H25A H 0.3837 0.6767 0.5496 0.032 Uiso 1 1 calc R . . C26 C 0.4392(3) 0.7195(3) 0.7184(3) 0.0310(8) Uani 1 1 d . . . H26A H 0.4518 0.8017 0.7361 0.037 Uiso 1 1 calc R . . C27 C 0.4617(3) 0.6753(3) 0.8054(3) 0.0281(8) Uani 1 1 d . . . H27A H 0.4890 0.7285 0.8799 0.034 Uiso 1 1 calc R . . C28 C 0.4448(3) 0.5563(3) 0.7851(3) 0.0242(7) Uani 1 1 d . . . H28A H 0.4593 0.5267 0.8438 0.029 Uiso 1 1 calc R . . C29 C 0.4056(3) 0.4821(3) 0.6741(3) 0.0204(7) Uani 1 1 d . . . C31 C 0.2712(3) 0.1889(3) 0.7181(3) 0.0354(9) Uani 1 1 d . . . C41 C 0.4506(3) 0.0861(4) 0.7161(4) 0.0391(10) Uani 1 1 d . . . C51 C 0.4803(3) 0.3089(3) 0.8421(3) 0.0335(8) Uani 1 1 d . . . C61 C 0.1956(3) 0.4232(3) 0.3292(3) 0.0238(7) Uani 1 1 d . . . C62 C 0.1562(3) 0.4027(3) 0.2147(3) 0.0250(7) Uani 1 1 d . . . C63 C 0.0352(3) 0.3883(3) 0.1697(3) 0.0272(8) Uani 1 1 d . . . C63' C 0.2307(3) 0.3952(3) 0.1397(3) 0.0327(8) Uani 1 1 d . . . H63A H 0.3113 0.4042 0.1675 0.039 Uiso 1 1 calc R . . C64 C -0.0413(3) 0.3992(3) 0.2416(3) 0.0337(9) Uani 1 1 d . . . C64' C 0.1895(3) 0.3756(4) 0.0304(3) 0.0413(10) Uani 1 1 d . . . H64A H 0.2422 0.3723 -0.0161 0.050 Uiso 1 1 calc R . . C65 C 0.0013(3) 0.4189(4) 0.3535(3) 0.0354(9) Uani 1 1 d . . . H65A H -0.0503 0.4247 0.4013 0.042 Uiso 1 1 calc R . . C66 C 0.1174(3) 0.4301(3) 0.3963(3) 0.0297(8) Uani 1 1 d . . . H66A H 0.1445 0.4427 0.4731 0.036 Uiso 1 1 calc R . . C71 C 0.0694(3) 0.3598(4) -0.0172(3) 0.0358(9) Uani 1 1 d . . . C72 C -0.0080(3) 0.3675(3) 0.0551(3) 0.0328(8) Uani 1 1 d . . . C73' C -0.2032(3) 0.3659(4) 0.0862(4) 0.0480(11) Uani 1 1 d . . . H73A H -0.2836 0.3571 0.0576 0.058 Uiso 1 1 calc R . . C73 C -0.1273(3) 0.3553(4) 0.0110(3) 0.0384(9) Uani 1 1 d . . . C74 C -0.1679(3) 0.3347(4) -0.1015(4) 0.0423(10) Uani 1 1 d . . . H74A H -0.2481 0.3254 -0.1313 0.051 Uiso 1 1 calc R . . C74' C -0.1635(3) 0.3878(4) 0.1948(4) 0.0459(11) Uani 1 1 d . . . H74B H -0.2155 0.3961 0.2421 0.055 Uiso 1 1 calc R . . C75 C -0.0925(4) 0.3276(4) -0.1704(3) 0.0436(10) Uani 1 1 d . . . H75A H -0.1214 0.3142 -0.2470 0.052 Uiso 1 1 calc R . . C76 C 0.0252(3) 0.3397(4) -0.1292(3) 0.0432(10) Uani 1 1 d . . . H76A H 0.0757 0.3343 -0.1779 0.052 Uiso 1 1 calc R . . O101 O 0.0627(4) 0.1944(5) 0.4837(4) 0.0995(15) Uani 1 1 d . . . C102 C -0.0168(5) 0.1212(6) 0.3790(7) 0.113(3) Uani 1 1 d . . . H10A H -0.0106 0.0389 0.3616 0.136 Uiso 1 1 calc R . . H10B H 0.0013 0.1472 0.3182 0.136 Uiso 1 1 calc R . . C103 C -0.1363(5) 0.1316(7) 0.3903(7) 0.134(4) Uani 1 1 d . . . H10C H -0.1749 0.1581 0.3322 0.160 Uiso 1 1 calc R . . H10D H -0.1836 0.0552 0.3830 0.160 Uiso 1 1 calc R . . C104 C -0.1227(5) 0.2166(7) 0.4998(6) 0.096(2) Uani 1 1 d . . . H10E H -0.1762 0.1863 0.5391 0.115 Uiso 1 1 calc R . . H10F H -0.1401 0.2902 0.4937 0.115 Uiso 1 1 calc R . . C105 C -0.0026(6) 0.2377(7) 0.5605(6) 0.103(2) Uani 1 1 d . . . H10G H 0.0292 0.3225 0.6009 0.124 Uiso 1 1 calc R . . H10H H 0.0013 0.1976 0.6154 0.124 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 Re1 0.02596(8) 0.02602(8) 0.02509(8) 0.01347(6) 0.00590(6) 0.00958(5) Cl1 0.0265(4) 0.0359(5) 0.0344(5) 0.0195(4) 0.0062(4) 0.0101(4) O31 0.0415(17) 0.059(2) 0.070(2) 0.0292(18) 0.0291(16) 0.0186(15) O41 0.068(2) 0.0503(19) 0.094(3) 0.053(2) 0.030(2) 0.0317(16) O51 0.0616(19) 0.065(2) 0.0256(17) 0.0131(15) -0.0005(15) 0.0252(16) N11 0.0228(14) 0.0256(15) 0.0320(18) 0.0112(13) 0.0059(13) 0.0056(12) N21 0.0207(13) 0.0230(14) 0.0225(16) 0.0084(12) 0.0017(12) 0.0078(11) N23 0.0192(13) 0.0271(15) 0.0222(15) 0.0101(12) 0.0021(12) 0.0057(11) C12 0.0227(16) 0.0268(18) 0.0261(19) 0.0083(15) 0.0059(15) 0.0055(14) C13 0.0315(19) 0.034(2) 0.027(2) 0.0103(17) 0.0025(16) 0.0064(16) C14 0.043(2) 0.034(2) 0.030(2) 0.0010(18) 0.0024(18) 0.0075(17) C15 0.049(2) 0.0244(19) 0.034(2) -0.0024(17) 0.0076(19) 0.0079(17) C16 0.0324(19) 0.0255(18) 0.042(2) 0.0109(17) 0.0071(17) 0.0081(15) C22 0.0184(15) 0.0258(17) 0.0219(18) 0.0101(14) 0.0009(13) 0.0054(13) C23 0.0211(16) 0.0325(19) 0.0210(18) 0.0134(15) 0.0042(14) 0.0082(14) C24 0.0143(14) 0.0275(17) 0.0230(18) 0.0096(14) 0.0028(13) 0.0062(13) C25 0.0236(16) 0.0268(18) 0.035(2) 0.0163(16) 0.0075(15) 0.0089(14) C26 0.0319(19) 0.0235(18) 0.036(2) 0.0071(16) 0.0081(17) 0.0078(15) C27 0.0219(16) 0.0278(18) 0.029(2) 0.0049(16) 0.0030(15) 0.0060(14) C28 0.0189(15) 0.0315(18) 0.0232(19) 0.0104(15) 0.0039(14) 0.0084(13) C29 0.0153(14) 0.0237(16) 0.0235(18) 0.0088(14) 0.0040(13) 0.0076(12) C31 0.042(2) 0.034(2) 0.037(2) 0.0176(18) 0.0136(19) 0.0131(17) C41 0.039(2) 0.042(2) 0.052(3) 0.027(2) 0.022(2) 0.0183(18) C51 0.037(2) 0.040(2) 0.032(2) 0.0209(19) 0.0074(18) 0.0186(17) C61 0.0190(16) 0.0290(18) 0.0244(19) 0.0102(15) 0.0029(14) 0.0090(13) C62 0.0203(16) 0.0297(18) 0.0256(19) 0.0101(15) 0.0030(14) 0.0094(14) C63 0.0199(16) 0.035(2) 0.0242(19) 0.0078(16) 0.0023(14) 0.0086(14) C63' 0.0213(17) 0.051(2) 0.028(2) 0.0142(18) 0.0042(15) 0.0154(16) C64 0.0200(17) 0.050(2) 0.031(2) 0.0131(19) 0.0061(16) 0.0118(16) C64' 0.031(2) 0.071(3) 0.025(2) 0.015(2) 0.0099(17) 0.020(2) C65 0.0245(18) 0.055(2) 0.026(2) 0.0125(19) 0.0072(16) 0.0118(17) C66 0.0230(17) 0.045(2) 0.0234(19) 0.0129(17) 0.0055(15) 0.0126(15) C71 0.0318(19) 0.050(2) 0.024(2) 0.0102(18) 0.0036(16) 0.0159(18) C72 0.0249(18) 0.042(2) 0.026(2) 0.0068(17) -0.0002(16) 0.0098(16) C73' 0.0197(18) 0.077(3) 0.042(3) 0.015(2) 0.0026(18) 0.0145(19) C73 0.0288(19) 0.048(2) 0.028(2) 0.0043(18) -0.0031(17) 0.0099(17) C74 0.027(2) 0.053(3) 0.036(2) 0.009(2) -0.0072(18) 0.0089(18) C74' 0.0229(19) 0.077(3) 0.038(3) 0.018(2) 0.0065(18) 0.015(2) C75 0.045(2) 0.054(3) 0.026(2) 0.008(2) -0.0026(19) 0.018(2) C76 0.042(2) 0.058(3) 0.025(2) 0.007(2) 0.0030(18) 0.020(2) O101 0.067(3) 0.158(5) 0.084(3) 0.042(3) 0.033(2) 0.039(3) C102 0.075(4) 0.084(5) 0.135(7) -0.026(5) 0.042(5) -0.001(4) C103 0.058(4) 0.112(6) 0.153(8) -0.045(5) 0.023(4) -0.004(4) C104 0.066(4) 0.132(6) 0.098(6) 0.041(5) 0.035(4) 0.022(4) C105 0.094(5) 0.156(7) 0.077(5) 0.043(5) 0.031(4) 0.061(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C31 1.913(4) . ? Re1 C51 1.920(4) . ? Re1 C41 1.925(4) . ? Re1 N21 2.166(3) . ? Re1 N11 2.201(3) . ? Re1 Cl1 2.4868(9) . ? O31 C31 1.148(4) . ? O41 C41 1.146(4) . ? O51 C51 1.153(5) . ? N11 C16 1.353(4) . ? N11 C12 1.364(4) . ? N21 C22 1.329(4) . ? N21 C29 1.382(4) . ? N23 C22 1.365(4) . ? N23 C24 1.400(4) . ? N23 C23 1.478(4) . ? C12 C13 1.379(5) . ? C12 C22 1.470(5) . ? C13 C14 1.392(5) . ? C13 H13A 0.9500 . ? C14 C15 1.368(5) . ? C14 H14A 0.9500 . ? C15 C16 1.379(5) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C23 C61 1.521(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.399(4) . ? C24 C29 1.399(4) . ? C25 C26 1.382(5) . ? C25 H25A 0.9500 . ? C26 C27 1.410(5) . ? C26 H26A 0.9500 . ? C27 C28 1.386(5) . ? C27 H27A 0.9500 . ? C28 C29 1.396(5) . ? C28 H28A 0.9500 . ? C61 C66 1.390(4) . ? C61 C62 1.412(5) . ? C62 C63 1.433(4) . ? C62 C63' 1.433(5) . ? C63 C72 1.419(5) . ? C63 C64 1.419(5) . ? C63' C64' 1.354(5) . ? C63' H63A 0.9500 . ? C64 C65 1.388(5) . ? C64 C74' 1.456(5) . ? C64' C71 1.426(5) . ? C64' H64A 0.9500 . ? C65 C66 1.380(5) . ? C65 H65A 0.9500 . ? C66 H66A 0.9500 . ? C71 C76 1.392(5) . ? C71 C72 1.432(5) . ? C72 C73 1.417(5) . ? C73' C74' 1.338(6) . ? C73' C73 1.446(5) . ? C73' H73A 0.9500 . ? C73 C74 1.390(6) . ? C74 C75 1.381(6) . ? C74 H74A 0.9500 . ? C74' H74B 0.9500 . ? C75 C76 1.391(5) . ? C75 H75A 0.9500 . ? C76 H76A 0.9500 . ? O101 C105 1.409(7) . ? O101 C102 1.445(8) . ? C102 C103 1.495(8) . ? C102 H10A 0.9900 . ? C102 H10B 0.9900 . ? C103 C104 1.447(9) . ? C103 H10C 0.9900 . ? C103 H10D 0.9900 . ? C104 C105 1.461(8) . ? C104 H10E 0.9900 . ? C104 H10F 0.9900 . ? C105 H10G 0.9900 . ? C105 H10H 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C31 Re1 C51 87.52(16) . . ? C31 Re1 C41 88.52(15) . . ? C51 Re1 C41 87.48(17) . . ? C31 Re1 N21 94.77(13) . . ? C51 Re1 N21 100.32(13) . . ? C41 Re1 N21 171.64(14) . . ? C31 Re1 N11 93.93(14) . . ? C51 Re1 N11 174.06(12) . . ? C41 Re1 N11 98.31(15) . . ? N21 Re1 N11 73.82(10) . . ? C31 Re1 Cl1 177.53(12) . . ? C51 Re1 Cl1 94.37(11) . . ? C41 Re1 Cl1 93.15(11) . . ? N21 Re1 Cl1 83.33(7) . . ? N11 Re1 Cl1 84.03(7) . . ? C16 N11 C12 117.6(3) . . ? C16 N11 Re1 124.0(2) . . ? C12 N11 Re1 118.4(2) . . ? C22 N21 C29 107.0(3) . . ? C22 N21 Re1 116.6(2) . . ? C29 N21 Re1 135.3(2) . . ? C22 N23 C24 106.6(3) . . ? C22 N23 C23 129.1(3) . . ? C24 N23 C23 124.1(3) . . ? N11 C12 C13 121.9(3) . . ? N11 C12 C22 111.5(3) . . ? C13 C12 C22 126.6(3) . . ? C12 C13 C14 119.2(3) . . ? C12 C13 H13A 120.4 . . ? C14 C13 H13A 120.4 . . ? C15 C14 C13 119.3(4) . . ? C15 C14 H14A 120.4 . . ? C13 C14 H14A 120.4 . . ? C14 C15 C16 119.1(4) . . ? C14 C15 H15A 120.4 . . ? C16 C15 H15A 120.4 . . ? N11 C16 C15 122.8(3) . . ? N11 C16 H16A 118.6 . . ? C15 C16 H16A 118.6 . . ? N21 C22 N23 111.6(3) . . ? N21 C22 C12 119.0(3) . . ? N23 C22 C12 129.4(3) . . ? N23 C23 C61 112.8(3) . . ? N23 C23 H23A 109.0 . . ? C61 C23 H23A 109.0 . . ? N23 C23 H23B 109.0 . . ? C61 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? C25 C24 C29 122.9(3) . . ? C25 C24 N23 130.9(3) . . ? C29 C24 N23 106.1(3) . . ? C26 C25 C24 115.6(3) . . ? C26 C25 H25A 122.2 . . ? C24 C25 H25A 122.2 . . ? C25 C26 C27 122.2(3) . . ? C25 C26 H26A 118.9 . . ? C27 C26 H26A 118.9 . . ? C28 C27 C26 121.7(3) . . ? C28 C27 H27A 119.1 . . ? C26 C27 H27A 119.1 . . ? C27 C28 C29 116.8(3) . . ? C27 C28 H28A 121.6 . . ? C29 C28 H28A 121.6 . . ? N21 C29 C28 130.5(3) . . ? N21 C29 C24 108.6(3) . . ? C28 C29 C24 120.8(3) . . ? O31 C31 Re1 177.0(4) . . ? O41 C41 Re1 179.1(3) . . ? O51 C51 Re1 178.2(3) . . ? C66 C61 C62 120.0(3) . . ? C66 C61 C23 121.1(3) . . ? C62 C61 C23 119.0(3) . . ? C61 C62 C63 118.8(3) . . ? C61 C62 C63' 123.7(3) . . ? C63 C62 C63' 117.5(3) . . ? C72 C63 C64 119.9(3) . . ? C72 C63 C62 120.6(3) . . ? C64 C63 C62 119.5(3) . . ? C64' C63' C62 121.9(3) . . ? C64' C63' H63A 119.1 . . ? C62 C63' H63A 119.1 . . ? C65 C64 C63 119.6(3) . . ? C65 C64 C74' 121.8(3) . . ? C63 C64 C74' 118.6(3) . . ? C63' C64' C71 122.1(3) . . ? C63' C64' H64A 119.0 . . ? C71 C64' H64A 119.0 . . ? C66 C65 C64 120.9(3) . . ? C66 C65 H65A 119.6 . . ? C64 C65 H65A 119.6 . . ? C65 C66 C61 121.2(3) . . ? C65 C66 H66A 119.4 . . ? C61 C66 H66A 119.4 . . ? C76 C71 C64' 123.0(3) . . ? C76 C71 C72 119.1(3) . . ? C64' C71 C72 117.9(3) . . ? C73 C72 C63 120.6(3) . . ? C73 C72 C71 119.2(3) . . ? C63 C72 C71 120.1(3) . . ? C74' C73' C73 121.9(3) . . ? C74' C73' H73A 119.1 . . ? C73 C73' H73A 119.1 . . ? C74 C73 C72 119.8(4) . . ? C74 C73 C73' 122.1(3) . . ? C72 C73 C73' 118.2(4) . . ? C75 C74 C73 120.5(4) . . ? C75 C74 H74A 119.8 . . ? C73 C74 H74A 119.8 . . ? C73' C74' C64 120.8(4) . . ? C73' C74' H74B 119.6 . . ? C64 C74' H74B 119.6 . . ? C74 C75 C76 121.0(4) . . ? C74 C75 H75A 119.5 . . ? C76 C75 H75A 119.5 . . ? C75 C76 C71 120.5(4) . . ? C75 C76 H76A 119.8 . . ? C71 C76 H76A 119.8 . . ? C105 O101 C102 108.2(5) . . ? O101 C102 C103 107.5(5) . . ? O101 C102 H10A 110.2 . . ? C103 C102 H10A 110.2 . . ? O101 C102 H10B 110.2 . . ? C103 C102 H10B 110.2 . . ? H10A C102 H10B 108.5 . . ? C104 C103 C102 106.2(6) . . ? C104 C103 H10C 110.5 . . ? C102 C103 H10C 110.5 . . ? C104 C103 H10D 110.5 . . ? C102 C103 H10D 110.5 . . ? H10C C103 H10D 108.7 . . ? C103 C104 C105 107.2(6) . . ? C103 C104 H10E 110.3 . . ? C105 C104 H10E 110.3 . . ? C103 C104 H10F 110.3 . . ? C105 C104 H10F 110.3 . . ? H10E C104 H10F 108.5 . . ? O101 C105 C104 108.7(6) . . ? O101 C105 H10G 110.0 . . ? C104 C105 H10G 110.0 . . ? O101 C105 H10H 110.0 . . ? C104 C105 H10H 110.0 . . ? H10G C105 H10H 108.3 . . ? 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 C31 Re1 N11 C16 -83.1(3) . . . . ? C41 Re1 N11 C16 5.9(3) . . . . ? N21 Re1 N11 C16 -177.0(3) . . . . ? Cl1 Re1 N11 C16 98.3(3) . . . . ? C31 Re1 N11 C12 94.4(2) . . . . ? C41 Re1 N11 C12 -176.5(2) . . . . ? N21 Re1 N11 C12 0.6(2) . . . . ? Cl1 Re1 N11 C12 -84.2(2) . . . . ? C31 Re1 N21 C22 -98.3(2) . . . . ? C51 Re1 N21 C22 173.4(2) . . . . ? N11 Re1 N21 C22 -5.6(2) . . . . ? Cl1 Re1 N21 C22 80.1(2) . . . . ? C31 Re1 N21 C29 95.6(3) . . . . ? C51 Re1 N21 C29 7.2(3) . . . . ? N11 Re1 N21 C29 -171.7(3) . . . . ? Cl1 Re1 N21 C29 -86.0(3) . . . . ? C16 N11 C12 C13 2.9(5) . . . . ? Re1 N11 C12 C13 -174.8(2) . . . . ? C16 N11 C12 C22 -178.4(3) . . . . ? Re1 N11 C12 C22 3.9(3) . . . . ? N11 C12 C13 C14 -1.5(5) . . . . ? C22 C12 C13 C14 -180.0(3) . . . . ? C12 C13 C14 C15 -1.0(5) . . . . ? C13 C14 C15 C16 2.0(6) . . . . ? C12 N11 C16 C15 -1.9(5) . . . . ? Re1 N11 C16 C15 175.7(3) . . . . ? C14 C15 C16 N11 -0.6(6) . . . . ? C29 N21 C22 N23 0.1(3) . . . . ? Re1 N21 C22 N23 -169.76(19) . . . . ? C29 N21 C22 C12 179.8(3) . . . . ? Re1 N21 C22 C12 9.9(4) . . . . ? C24 N23 C22 N21 -0.6(3) . . . . ? C23 N23 C22 N21 175.9(3) . . . . ? C24 N23 C22 C12 179.8(3) . . . . ? C23 N23 C22 C12 -3.7(5) . . . . ? N11 C12 C22 N21 -9.0(4) . . . . ? C13 C12 C22 N21 169.5(3) . . . . ? N11 C12 C22 N23 170.6(3) . . . . ? C13 C12 C22 N23 -10.9(5) . . . . ? C22 N23 C23 C61 86.7(4) . . . . ? C24 N23 C23 C61 -97.4(3) . . . . ? C22 N23 C24 C25 178.7(3) . . . . ? C23 N23 C24 C25 2.0(5) . . . . ? C22 N23 C24 C29 0.8(3) . . . . ? C23 N23 C24 C29 -175.9(3) . . . . ? C29 C24 C25 C26 0.2(5) . . . . ? N23 C24 C25 C26 -177.4(3) . . . . ? C24 C25 C26 C27 -0.3(5) . . . . ? C25 C26 C27 C28 -0.1(5) . . . . ? C26 C27 C28 C29 0.6(5) . . . . ? C22 N21 C29 C28 -178.8(3) . . . . ? Re1 N21 C29 C28 -11.7(5) . . . . ? C22 N21 C29 C24 0.4(3) . . . . ? Re1 N21 C29 C24 167.5(2) . . . . ? C27 C28 C29 N21 178.3(3) . . . . ? C27 C28 C29 C24 -0.8(4) . . . . ? C25 C24 C29 N21 -178.9(3) . . . . ? N23 C24 C29 N21 -0.7(3) . . . . ? C25 C24 C29 C28 0.4(5) . . . . ? N23 C24 C29 C28 178.5(3) . . . . ? N23 C23 C61 C66 15.2(5) . . . . ? N23 C23 C61 C62 -165.8(3) . . . . ? C66 C61 C62 C63 -0.5(5) . . . . ? C23 C61 C62 C63 -179.6(3) . . . . ? C66 C61 C62 C63' 179.5(3) . . . . ? C23 C61 C62 C63' 0.4(5) . . . . ? C61 C62 C63 C72 -180.0(3) . . . . ? C63' C62 C63 C72 0.0(5) . . . . ? C61 C62 C63 C64 2.3(5) . . . . ? C63' C62 C63 C64 -177.7(3) . . . . ? C61 C62 C63' C64' -179.9(4) . . . . ? C63 C62 C63' C64' 0.2(6) . . . . ? C72 C63 C64 C65 179.6(4) . . . . ? C62 C63 C64 C65 -2.7(6) . . . . ? C72 C63 C64 C74' 0.5(6) . . . . ? C62 C63 C64 C74' 178.1(4) . . . . ? C62 C63' C64' C71 -0.8(7) . . . . ? C63 C64 C65 C66 1.2(6) . . . . ? C74' C64 C65 C66 -179.6(4) . . . . ? C64 C65 C66 C61 0.6(6) . . . . ? C62 C61 C66 C65 -0.9(5) . . . . ? C23 C61 C66 C65 178.1(3) . . . . ? C63' C64' C71 C76 179.9(4) . . . . ? C63' C64' C71 C72 1.3(6) . . . . ? C64 C63 C72 C73 -1.2(6) . . . . ? C62 C63 C72 C73 -178.9(4) . . . . ? C64 C63 C72 C71 178.2(4) . . . . ? C62 C63 C72 C71 0.5(6) . . . . ? C76 C71 C72 C73 -0.4(6) . . . . ? C64' C71 C72 C73 178.3(4) . . . . ? C76 C71 C72 C63 -179.8(4) . . . . ? C64' C71 C72 C63 -1.1(6) . . . . ? C63 C72 C73 C74 -179.8(4) . . . . ? C71 C72 C73 C74 0.7(6) . . . . ? C63 C72 C73 C73' 0.7(6) . . . . ? C71 C72 C73 C73' -178.7(4) . . . . ? C74' C73' C73 C74 -178.8(5) . . . . ? C74' C73' C73 C72 0.7(7) . . . . ? C72 C73 C74 C75 -0.9(6) . . . . ? C73' C73 C74 C75 178.6(4) . . . . ? C73 C73' C74' C64 -1.5(7) . . . . ? C65 C64 C74' C73' -178.3(4) . . . . ? C63 C64 C74' C73' 0.9(7) . . . . ? C73 C74 C75 C76 0.6(7) . . . . ? C74 C75 C76 C71 -0.2(7) . . . . ? C64' C71 C76 C75 -178.5(4) . . . . ? C72 C71 C76 C75 0.1(6) . . . . ? C105 O101 C102 C103 6.3(9) . . . . ? O101 C102 C103 C104 3.4(10) . . . . ? C102 C103 C104 C105 -11.5(10) . . . . ? C102 O101 C105 C104 -13.7(9) . . . . ? C103 C104 C105 O101 15.8(9) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.724 _refine_diff_density_min -0.683 _refine_diff_density_rms 0.114 #=END data_steaks _database_code_depnum_ccdc_archive 'CCDC 245718' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H23 N3 Pt' _chemical_formula_sum 'C30 H23 N3 Pt' _chemical_formula_weight 620.60 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.435(4) _cell_length_b 7.5867(13) _cell_length_c 23.436(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.215(14) _cell_angle_gamma 90.00 _cell_volume 2305.0(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 71 _cell_measurement_theta_min 0.527 _cell_measurement_theta_max 0.74 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.788 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 6.112 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.09 _exptl_absorpt_correction_T_max 0.16 _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 'CCD area detector' _diffrn_measurement_method '\w rotatio with narrow frames' _diffrn_detector_area_resol_mean 8.2 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 11834 _diffrn_reflns_av_R_equivalents 0.0422 _diffrn_reflns_av_sigmaI/netI 0.0583 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5140 _reflns_number_gt 4018 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1998)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1998)' _computing_data_reduction 'Bruker SHELXTL (Bruker, 1998)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 1998)' _computing_structure_refinement 'Bruker SHELXTL (Bruker, 1998)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1998)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1998)' _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^)+(0.0260P)^2^+3.9862P] 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 5140 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.0763 _refine_ls_wR_factor_gt 0.0696 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _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 Pt1 Pt 0.441983(15) 0.19114(3) 0.509234(8) 0.01940(7) Uani 1 1 d . . . N11 N 0.4853(3) 0.2369(6) 0.43164(18) 0.0220(10) Uani 1 1 d . . . N21 N 0.5842(3) 0.3114(6) 0.54019(17) 0.0200(9) Uani 1 1 d . . . N23 N 0.7173(3) 0.4537(6) 0.52168(18) 0.0216(10) Uani 1 1 d . . . C1 C 0.7903(4) 0.5299(8) 0.4918(2) 0.0275(13) Uani 1 1 d . . . H1A H 0.8295 0.6257 0.5165 0.033 Uiso 1 1 calc R . . H1B H 0.7517 0.5817 0.4537 0.033 Uiso 1 1 calc R . . C2 C 0.8650(4) 0.3927(9) 0.4807(3) 0.0340(15) Uani 1 1 d . . . H2A H 0.9133 0.4483 0.4613 0.051 Uiso 1 1 calc R . . H2B H 0.8266 0.2997 0.4552 0.051 Uiso 1 1 calc R . . H2C H 0.9035 0.3414 0.5184 0.051 Uiso 1 1 calc R . . C12 C 0.5770(4) 0.3204(8) 0.4369(2) 0.0227(11) Uani 1 1 d . . . C13 C 0.6113(4) 0.3569(8) 0.3874(2) 0.0264(13) Uani 1 1 d . . . H13A H 0.6751 0.4165 0.3918 0.032 Uiso 1 1 calc R . . C14 C 0.5545(4) 0.3083(8) 0.3317(2) 0.0286(12) Uani 1 1 d . . . H14A H 0.5784 0.3322 0.2978 0.034 Uiso 1 1 calc R . . C15 C 0.4604(5) 0.2224(8) 0.3268(2) 0.0281(13) Uani 1 1 d . . . H15A H 0.4184 0.1881 0.2892 0.034 Uiso 1 1 calc R . . C16 C 0.4295(4) 0.1882(8) 0.3776(2) 0.0256(12) Uani 1 1 d . . . H16A H 0.3662 0.1278 0.3740 0.031 Uiso 1 1 calc R . . C22 C 0.6289(4) 0.3641(7) 0.4982(2) 0.0210(11) Uani 1 1 d . . . C24 C 0.7290(4) 0.4629(7) 0.5826(2) 0.0205(11) Uani 1 1 d . . . C25 C 0.8039(4) 0.5439(8) 0.6273(2) 0.0279(13) Uani 1 1 d . . . H25A H 0.8590 0.6094 0.6193 0.033 Uiso 1 1 calc R . . C26 C 0.7935(4) 0.5235(9) 0.6843(2) 0.0310(14) Uani 1 1 d . . . H26A H 0.8427 0.5768 0.7163 0.037 Uiso 1 1 calc R . . C27 C 0.7125(4) 0.4264(9) 0.6957(2) 0.0314(14) Uani 1 1 d . . . H27A H 0.7088 0.4146 0.7355 0.038 Uiso 1 1 calc R . . C28 C 0.6373(4) 0.3467(8) 0.6511(2) 0.0278(13) Uani 1 1 d . . . H28A H 0.5828 0.2799 0.6592 0.033 Uiso 1 1 calc R . . C29 C 0.6463(4) 0.3704(7) 0.5936(2) 0.0240(12) Uani 1 1 d . . . C31 C 0.4085(4) 0.1662(7) 0.5846(2) 0.0224(12) Uani 1 1 d . . . C32 C 0.3903(4) 0.1561(7) 0.6322(2) 0.0252(12) Uani 1 1 d . . . C33 C 0.3796(4) 0.1429(7) 0.6921(2) 0.0229(12) Uani 1 1 d . . . C34 C 0.3105(4) 0.0280(8) 0.7073(2) 0.0256(12) Uani 1 1 d . . . H34A H 0.2693 -0.0467 0.6779 0.031 Uiso 1 1 calc R . . C35 C 0.3002(4) 0.0199(9) 0.7649(2) 0.0305(14) Uani 1 1 d . . . H35A H 0.2514 -0.0580 0.7743 0.037 Uiso 1 1 calc R . . C36 C 0.3614(5) 0.1259(9) 0.8084(2) 0.0332(14) Uani 1 1 d . . . H36A H 0.3549 0.1202 0.8477 0.040 Uiso 1 1 calc R . . C37 C 0.4317(4) 0.2397(9) 0.7946(2) 0.0313(14) Uani 1 1 d . . . H37A H 0.4742 0.3109 0.8246 0.038 Uiso 1 1 calc R . . C38 C 0.4409(4) 0.2508(8) 0.7372(2) 0.0264(12) Uani 1 1 d . . . H38A H 0.4886 0.3313 0.7281 0.032 Uiso 1 1 calc R . . C41 C 0.3069(4) 0.0934(7) 0.4706(2) 0.0216(11) Uani 1 1 d . . . C42 C 0.2221(4) 0.0417(7) 0.4443(2) 0.0223(11) Uani 1 1 d . . . C43 C 0.1210(4) -0.0233(7) 0.4147(2) 0.0226(12) Uani 1 1 d . . . C44 C 0.0363(4) 0.0196(8) 0.4352(2) 0.0255(12) Uani 1 1 d . . . H44A H 0.0440 0.1016 0.4667 0.031 Uiso 1 1 calc R . . C45 C -0.0600(4) -0.0557(9) 0.4105(2) 0.0296(13) Uani 1 1 d . . . H45A H -0.1171 -0.0261 0.4255 0.035 Uiso 1 1 calc R . . C46 C -0.0723(4) -0.1724(8) 0.3645(3) 0.0326(14) Uani 1 1 d . . . H46A H -0.1372 -0.2271 0.3484 0.039 Uiso 1 1 calc R . . C47 C 0.0104(4) -0.2106(8) 0.3414(2) 0.0302(13) Uani 1 1 d . . . H47A H 0.0013 -0.2889 0.3088 0.036 Uiso 1 1 calc R . . C48 C 0.1064(4) -0.1352(8) 0.3656(2) 0.0274(13) Uani 1 1 d . . . H48A H 0.1621 -0.1595 0.3489 0.033 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 Pt1 0.01769(10) 0.01874(11) 0.02105(10) 0.00026(10) 0.00381(7) 0.00223(10) N11 0.021(2) 0.020(3) 0.023(2) 0.0001(18) 0.0018(18) 0.002(2) N21 0.017(2) 0.021(2) 0.0210(19) -0.0040(19) 0.0033(16) -0.002(2) N23 0.020(2) 0.018(3) 0.025(2) 0.0003(19) 0.0028(17) 0.003(2) C1 0.023(3) 0.029(4) 0.030(3) 0.001(2) 0.007(2) -0.002(3) C2 0.025(3) 0.043(4) 0.036(3) 0.003(3) 0.012(3) 0.008(3) C12 0.019(2) 0.024(3) 0.024(2) 0.002(2) 0.004(2) 0.005(3) C13 0.021(3) 0.032(4) 0.027(3) 0.001(2) 0.007(2) 0.002(2) C14 0.037(3) 0.028(3) 0.024(2) 0.002(3) 0.012(2) 0.007(3) C15 0.036(3) 0.027(4) 0.020(2) -0.002(2) 0.005(2) 0.008(3) C16 0.024(3) 0.026(3) 0.023(2) -0.004(2) 0.000(2) 0.001(3) C22 0.021(3) 0.017(3) 0.024(3) 0.001(2) 0.005(2) 0.004(2) C24 0.022(3) 0.017(3) 0.022(2) 0.003(2) 0.006(2) 0.004(2) C25 0.021(3) 0.026(3) 0.032(3) 0.000(2) 0.001(2) 0.000(3) C26 0.024(3) 0.034(4) 0.029(3) -0.007(3) -0.003(2) 0.000(3) C27 0.027(3) 0.040(4) 0.024(3) -0.004(3) 0.002(2) 0.008(3) C28 0.025(3) 0.034(4) 0.026(3) 0.001(2) 0.010(2) 0.004(3) C29 0.025(3) 0.020(3) 0.025(3) -0.001(2) 0.002(2) 0.005(2) C31 0.016(2) 0.021(3) 0.028(3) 0.002(2) 0.002(2) -0.003(2) C32 0.023(3) 0.024(3) 0.028(3) 0.002(2) 0.005(2) 0.003(2) C33 0.022(3) 0.023(3) 0.025(3) 0.000(2) 0.008(2) 0.009(2) C34 0.019(3) 0.027(3) 0.029(3) 0.001(2) 0.003(2) 0.002(2) C35 0.024(3) 0.034(4) 0.035(3) 0.010(3) 0.010(2) 0.004(3) C36 0.036(3) 0.038(4) 0.027(3) 0.005(3) 0.010(3) 0.013(3) C37 0.029(3) 0.033(4) 0.027(3) -0.004(2) -0.002(2) 0.004(3) C38 0.022(3) 0.026(3) 0.030(3) -0.001(2) 0.006(2) 0.002(2) C41 0.025(3) 0.018(3) 0.023(2) 0.000(2) 0.008(2) 0.004(2) C42 0.028(3) 0.018(3) 0.022(2) 0.003(2) 0.007(2) 0.002(2) C43 0.026(3) 0.020(3) 0.021(2) 0.004(2) 0.003(2) 0.000(2) C44 0.026(3) 0.027(3) 0.023(3) 0.002(2) 0.007(2) 0.002(3) C45 0.024(3) 0.030(4) 0.033(3) 0.004(3) 0.005(2) 0.003(3) C46 0.022(3) 0.028(4) 0.040(3) 0.003(3) -0.005(2) -0.002(3) C47 0.032(3) 0.027(3) 0.026(3) -0.006(2) -0.003(2) 0.005(3) C48 0.024(3) 0.027(3) 0.029(3) 0.000(2) 0.004(2) 0.008(3) _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 Pt1 C31 1.942(5) . ? Pt1 C41 1.950(5) . ? Pt1 N21 2.070(4) . ? Pt1 N11 2.079(4) . ? N11 C16 1.344(6) . ? N11 C12 1.362(7) . ? N21 C22 1.341(6) . ? N21 C29 1.383(6) . ? N23 C22 1.355(7) . ? N23 C24 1.396(6) . ? N23 C1 1.465(6) . ? C1 C2 1.515(8) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C12 C13 1.385(7) . ? C12 C22 1.460(7) . ? C13 C14 1.378(7) . ? C13 H13A 0.9500 . ? C14 C15 1.400(8) . ? C14 H14A 0.9500 . ? C15 C16 1.384(7) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C24 C25 1.391(7) . ? C24 C29 1.394(7) . ? C25 C26 1.387(7) . ? C25 H25A 0.9500 . ? C26 C27 1.397(8) . ? C26 H26A 0.9500 . ? C27 C28 1.388(8) . ? C27 H27A 0.9500 . ? C28 C29 1.397(7) . ? C28 H28A 0.9500 . ? C31 C32 1.207(7) . ? C32 C33 1.450(7) . ? C33 C34 1.387(7) . ? C33 C38 1.418(8) . ? C34 C35 1.393(7) . ? C34 H34A 0.9500 . ? C35 C36 1.386(9) . ? C35 H35A 0.9500 . ? C36 C37 1.380(9) . ? C36 H36A 0.9500 . ? C37 C38 1.383(8) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? C41 C42 1.210(7) . ? C42 C43 1.440(7) . ? C43 C44 1.386(7) . ? C43 C48 1.401(7) . ? C44 C45 1.394(8) . ? C44 H44A 0.9500 . ? C45 C46 1.372(8) . ? C45 H45A 0.9500 . ? C46 C47 1.388(8) . ? C46 H46A 0.9500 . ? C47 C48 1.388(8) . ? C47 H47A 0.9500 . ? C48 H48A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C31 Pt1 C41 88.6(2) . . ? C31 Pt1 N21 97.88(18) . . ? C41 Pt1 N21 172.69(18) . . ? C31 Pt1 N11 175.0(2) . . ? C41 Pt1 N11 95.61(19) . . ? N21 Pt1 N11 77.77(16) . . ? C16 N11 C12 118.7(4) . . ? C16 N11 Pt1 124.3(4) . . ? C12 N11 Pt1 116.9(3) . . ? C22 N21 C29 106.7(4) . . ? C22 N21 Pt1 115.1(3) . . ? C29 N21 Pt1 137.9(3) . . ? C22 N23 C24 107.0(4) . . ? C22 N23 C1 129.0(4) . . ? C24 N23 C1 124.0(4) . . ? N23 C1 C2 111.6(5) . . ? N23 C1 H1A 109.3 . . ? C2 C1 H1A 109.3 . . ? N23 C1 H1B 109.3 . . ? C2 C1 H1B 109.3 . . ? H1A C1 H1B 108.0 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N11 C12 C13 120.6(5) . . ? N11 C12 C22 112.4(4) . . ? C13 C12 C22 127.0(5) . . ? C14 C13 C12 121.1(5) . . ? C14 C13 H13A 119.5 . . ? C12 C13 H13A 119.5 . . ? C13 C14 C15 117.8(5) . . ? C13 C14 H14A 121.1 . . ? C15 C14 H14A 121.1 . . ? C16 C15 C14 119.0(5) . . ? C16 C15 H15A 120.5 . . ? C14 C15 H15A 120.5 . . ? N11 C16 C15 122.7(5) . . ? N11 C16 H16A 118.7 . . ? C15 C16 H16A 118.7 . . ? N21 C22 N23 111.4(4) . . ? N21 C22 C12 117.7(5) . . ? N23 C22 C12 130.9(5) . . ? C25 C24 C29 122.5(5) . . ? C25 C24 N23 131.1(5) . . ? C29 C24 N23 106.4(4) . . ? C26 C25 C24 116.1(5) . . ? C26 C25 H25A 121.9 . . ? C24 C25 H25A 121.9 . . ? C25 C26 C27 121.6(5) . . ? C25 C26 H26A 119.2 . . ? C27 C26 H26A 119.2 . . ? C28 C27 C26 122.4(5) . . ? C28 C27 H27A 118.8 . . ? C26 C27 H27A 118.8 . . ? C27 C28 C29 116.1(5) . . ? C27 C28 H28A 121.9 . . ? C29 C28 H28A 121.9 . . ? N21 C29 C24 108.5(4) . . ? N21 C29 C28 130.3(5) . . ? C24 C29 C28 121.2(5) . . ? C32 C31 Pt1 177.4(5) . . ? C31 C32 C33 174.2(6) . . ? C34 C33 C38 117.8(5) . . ? C34 C33 C32 122.4(5) . . ? C38 C33 C32 119.7(5) . . ? C33 C34 C35 121.4(5) . . ? C33 C34 H34A 119.3 . . ? C35 C34 H34A 119.3 . . ? C36 C35 C34 119.7(6) . . ? C36 C35 H35A 120.1 . . ? C34 C35 H35A 120.1 . . ? C37 C36 C35 120.1(5) . . ? C37 C36 H36A 120.0 . . ? C35 C36 H36A 120.0 . . ? C36 C37 C38 120.5(6) . . ? C36 C37 H37A 119.8 . . ? C38 C37 H37A 119.8 . . ? C37 C38 C33 120.5(6) . . ? C37 C38 H38A 119.7 . . ? C33 C38 H38A 119.7 . . ? C42 C41 Pt1 176.0(5) . . ? C41 C42 C43 178.1(6) . . ? C44 C43 C48 118.5(5) . . ? C44 C43 C42 120.5(5) . . ? C48 C43 C42 121.0(5) . . ? C43 C44 C45 121.1(5) . . ? C43 C44 H44A 119.5 . . ? C45 C44 H44A 119.5 . . ? C46 C45 C44 119.9(5) . . ? C46 C45 H45A 120.1 . . ? C44 C45 H45A 120.1 . . ? C45 C46 C47 119.8(5) . . ? C45 C46 H46A 120.1 . . ? C47 C46 H46A 120.1 . . ? C48 C47 C46 120.5(5) . . ? C48 C47 H47A 119.7 . . ? C46 C47 H47A 119.7 . . ? C47 C48 C43 120.0(5) . . ? C47 C48 H48A 120.0 . . ? C43 C48 H48A 120.0 . . ? 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 C41 Pt1 N11 C16 -5.2(5) . . . . ? N21 Pt1 N11 C16 177.9(5) . . . . ? C41 Pt1 N11 C12 175.5(4) . . . . ? N21 Pt1 N11 C12 -1.4(4) . . . . ? C31 Pt1 N21 C22 -174.5(4) . . . . ? N11 Pt1 N21 C22 3.1(4) . . . . ? C31 Pt1 N21 C29 -2.0(6) . . . . ? N11 Pt1 N21 C29 175.5(6) . . . . ? C22 N23 C1 C2 -82.3(7) . . . . ? C24 N23 C1 C2 97.7(6) . . . . ? C16 N11 C12 C13 1.0(8) . . . . ? Pt1 N11 C12 C13 -179.6(4) . . . . ? C16 N11 C12 C22 -179.7(5) . . . . ? Pt1 N11 C12 C22 -0.3(6) . . . . ? N11 C12 C13 C14 -0.8(9) . . . . ? C22 C12 C13 C14 -179.9(6) . . . . ? C12 C13 C14 C15 0.7(9) . . . . ? C13 C14 C15 C16 -0.9(8) . . . . ? C12 N11 C16 C15 -1.3(8) . . . . ? Pt1 N11 C16 C15 179.4(4) . . . . ? C14 C15 C16 N11 1.2(9) . . . . ? C29 N21 C22 N23 0.4(6) . . . . ? Pt1 N21 C22 N23 175.1(3) . . . . ? C29 N21 C22 C12 -179.0(5) . . . . ? Pt1 N21 C22 C12 -4.3(6) . . . . ? C24 N23 C22 N21 -1.5(6) . . . . ? C1 N23 C22 N21 178.5(5) . . . . ? C24 N23 C22 C12 177.8(6) . . . . ? C1 N23 C22 C12 -2.2(9) . . . . ? N11 C12 C22 N21 3.1(7) . . . . ? C13 C12 C22 N21 -177.7(6) . . . . ? N11 C12 C22 N23 -176.2(5) . . . . ? C13 C12 C22 N23 3.0(10) . . . . ? C22 N23 C24 C25 -177.8(6) . . . . ? C1 N23 C24 C25 2.2(9) . . . . ? C22 N23 C24 C29 2.0(6) . . . . ? C1 N23 C24 C29 -178.0(5) . . . . ? C29 C24 C25 C26 1.8(8) . . . . ? N23 C24 C25 C26 -178.5(6) . . . . ? C24 C25 C26 C27 0.2(9) . . . . ? C25 C26 C27 C28 -0.8(10) . . . . ? C26 C27 C28 C29 -0.7(9) . . . . ? C22 N21 C29 C24 0.9(6) . . . . ? Pt1 N21 C29 C24 -171.9(4) . . . . ? C22 N21 C29 C28 -177.6(6) . . . . ? Pt1 N21 C29 C28 9.5(10) . . . . ? C25 C24 C29 N21 178.0(5) . . . . ? N23 C24 C29 N21 -1.8(6) . . . . ? C25 C24 C29 C28 -3.3(8) . . . . ? N23 C24 C29 C28 176.9(5) . . . . ? C27 C28 C29 N21 -179.0(6) . . . . ? C27 C28 C29 C24 2.6(8) . . . . ? C38 C33 C34 C35 0.9(8) . . . . ? C32 C33 C34 C35 -178.8(5) . . . . ? C33 C34 C35 C36 -1.3(9) . . . . ? C34 C35 C36 C37 0.4(9) . . . . ? C35 C36 C37 C38 0.8(9) . . . . ? C36 C37 C38 C33 -1.2(9) . . . . ? C34 C33 C38 C37 0.4(8) . . . . ? C32 C33 C38 C37 -179.9(5) . . . . ? C48 C43 C44 C45 4.3(8) . . . . ? C42 C43 C44 C45 -173.8(5) . . . . ? C43 C44 C45 C46 -0.9(9) . . . . ? C44 C45 C46 C47 -2.2(9) . . . . ? C45 C46 C47 C48 1.8(9) . . . . ? C46 C47 C48 C43 1.7(9) . . . . ? C44 C43 C48 C47 -4.7(8) . . . . ? C42 C43 C48 C47 173.4(5) . . . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 3.016 _refine_diff_density_min -1.478 _refine_diff_density_rms 0.159 #=END data_stones _database_code_depnum_ccdc_archive 'CCDC 245719' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H15 Cl N3 O3 Re, C H2 Cl2' _chemical_formula_sum 'C23 H17 Cl3 N3 O3 Re' _chemical_formula_weight 675.95 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c a 2 1' _symmetry_space_group_name_Hall 'P 2c -2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 8.908(3) _cell_length_b 12.523(4) _cell_length_c 20.764(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2316.3(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 56 _cell_measurement_theta_min 0.26 _cell_measurement_theta_max 0.43 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.938 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 5.624 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.11 _exptl_absorpt_correction_T_max 0.43 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 '\w rotation with narrow frames' _diffrn_detector_area_resol_mean 8.5 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 15304 _diffrn_reflns_av_R_equivalents 0.0558 _diffrn_reflns_av_sigmaI/netI 0.0768 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5208 _reflns_number_gt 4615 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1998)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1998)' _computing_data_reduction 'Bruker SHELXTL (Bruker, 1998)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 1998)' _computing_structure_refinement 'Bruker SHELXTL (Bruker, 1998)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1998)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1998)' _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^)+(0.0158P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.017(9) _refine_ls_number_reflns 5208 _refine_ls_number_parameters 283 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0474 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.0876 _refine_ls_wR_factor_gt 0.0846 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.46561(2) 0.181324(17) 0.432170(15) 0.01086(8) Uani 1 1 d . . . Cl1 Cl 0.2967(2) 0.18812(14) 0.52695(9) 0.0152(3) Uani 1 1 d . . . O41 O 0.2043(6) 0.2164(5) 0.3387(2) 0.0201(11) Uani 1 1 d . . . O51 O 0.4302(7) -0.0609(4) 0.4095(3) 0.0268(14) Uani 1 1 d . . . O61 O 0.6751(7) 0.1819(5) 0.3167(3) 0.0251(13) Uani 1 1 d . . . N11 N 0.6427(8) 0.1728(5) 0.5071(3) 0.0127(15) Uani 1 1 d . . . N21 N 0.5122(6) 0.3448(5) 0.4584(3) 0.0100(11) Uani 1 1 d . . . N23 N 0.6300(6) 0.4663(4) 0.5181(2) 0.0095(11) Uani 1 1 d . . . C12 C 0.6816(8) 0.2668(6) 0.5369(3) 0.0120(14) Uani 1 1 d . . . C13 C 0.7781(9) 0.2666(6) 0.5879(3) 0.0177(16) Uani 1 1 d . . . H13A H 0.8025 0.3304 0.6083 0.021 Uiso 1 1 calc R . . C14 C 0.8409(8) 0.1702(6) 0.6097(4) 0.0176(16) Uani 1 1 d . . . H14A H 0.9097 0.1692 0.6433 0.021 Uiso 1 1 calc R . . C15 C 0.7972(9) 0.0768(6) 0.5794(3) 0.0200(17) Uani 1 1 d . . . H15A H 0.8344 0.0114 0.5934 0.024 Uiso 1 1 calc R . . C16 C 0.6987(8) 0.0812(6) 0.5288(3) 0.0170(15) Uiso 1 1 d . . . H16A H 0.6701 0.0178 0.5088 0.020 Uiso 1 1 calc R . . C22 C 0.6093(8) 0.3599(6) 0.5063(3) 0.0094(13) Uani 1 1 d . . . C23 C 0.7202(8) 0.5221(6) 0.5667(3) 0.0125(14) Uani 1 1 d . . . H23A H 0.7546 0.5895 0.5490 0.015 Uiso 1 1 calc R . . H23B H 0.8079 0.4794 0.5768 0.015 Uiso 1 1 calc R . . C24 C 0.5401(7) 0.5221(6) 0.4744(3) 0.0113(14) Uani 1 1 d . . . C25 C 0.5186(8) 0.6296(6) 0.4645(4) 0.0154(15) Uani 1 1 d . . . H25A H 0.5660 0.6809 0.4898 0.018 Uiso 1 1 calc R . . C26 C 0.4230(8) 0.6569(6) 0.4153(3) 0.0140(17) Uani 1 1 d . . . H26A H 0.4068 0.7288 0.4066 0.017 Uiso 1 1 calc R . . C27 C 0.3494(8) 0.5809(6) 0.3780(3) 0.0168(15) Uani 1 1 d . . . H27A H 0.2867 0.6035 0.3449 0.020 Uiso 1 1 calc R . . C28 C 0.3667(7) 0.4737(6) 0.3888(3) 0.0130(14) Uani 1 1 d . . . H28A H 0.3154 0.4234 0.3642 0.016 Uiso 1 1 calc R . . C29 C 0.4673(8) 0.4421(6) 0.4393(5) 0.0166(19) Uani 1 1 d . . . C31 C 0.6328(7) 0.5433(6) 0.6281(3) 0.0112(13) Uani 1 1 d . . . C32 C 0.6447(8) 0.6434(6) 0.6561(3) 0.0153(15) Uani 1 1 d . . . H32A H 0.7031 0.6961 0.6369 0.018 Uiso 1 1 calc R . . C33 C 0.5671(10) 0.6649(7) 0.7144(4) 0.0238(18) Uani 1 1 d . . . H33A H 0.5728 0.7324 0.7329 0.029 Uiso 1 1 calc R . . C34 C 0.4855(8) 0.5881(7) 0.7429(3) 0.0217(18) Uani 1 1 d . . . H34A H 0.4376 0.6022 0.7818 0.026 Uiso 1 1 calc R . . C35 C 0.4719(9) 0.4880(8) 0.7149(4) 0.0217(19) Uani 1 1 d . . . H35A H 0.4115 0.4365 0.7341 0.026 Uiso 1 1 calc R . . C36 C 0.5480(8) 0.4645(7) 0.6585(4) 0.0173(17) Uani 1 1 d . . . H36A H 0.5425 0.3962 0.6410 0.021 Uiso 1 1 calc R . . C41 C 0.3046(8) 0.2019(6) 0.3727(3) 0.0116(14) Uiso 1 1 d . . . C51 C 0.4404(7) 0.0308(6) 0.4187(3) 0.0130(17) Uani 1 1 d . . . C61 C 0.6007(9) 0.1820(6) 0.3595(4) 0.0084(18) Uiso 1 1 d . . . Cl11 Cl 0.5482(2) -0.15765(17) 0.18294(11) 0.0264(4) Uani 1 1 d . . . Cl12 Cl 0.3778(2) 0.02583(17) 0.22904(10) 0.0282(4) Uani 1 1 d . . . C100 C 0.4879(9) -0.0852(7) 0.2512(4) 0.0251(18) Uani 1 1 d . . . H10A H 0.4297 -0.1317 0.2790 0.030 Uiso 1 1 calc R . . H10B H 0.5748 -0.0609 0.2752 0.030 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.01242(12) 0.00615(12) 0.01403(12) -0.0025(2) -0.00054(17) -0.00047(9) Cl1 0.0169(9) 0.0099(8) 0.0188(9) 0.0007(7) 0.0010(7) 0.0005(7) O41 0.014(3) 0.022(3) 0.024(3) -0.007(2) -0.004(2) 0.001(2) O51 0.032(3) 0.010(3) 0.038(3) -0.009(2) 0.009(2) -0.007(2) O61 0.024(3) 0.023(3) 0.028(3) 0.000(3) -0.001(3) -0.001(2) N11 0.015(4) 0.017(4) 0.006(3) -0.004(2) -0.001(3) 0.007(3) N21 0.009(3) 0.005(3) 0.016(3) -0.005(2) 0.002(2) 0.001(2) N23 0.013(3) 0.002(3) 0.013(3) -0.001(2) 0.001(2) 0.001(2) C12 0.013(3) 0.004(3) 0.019(3) -0.002(3) -0.001(3) -0.003(3) C13 0.020(4) 0.010(4) 0.022(4) -0.012(3) -0.004(3) 0.002(3) C14 0.015(4) 0.017(4) 0.021(4) 0.003(3) -0.009(3) 0.002(3) C15 0.019(4) 0.011(4) 0.030(4) -0.002(3) 0.000(3) 0.000(3) C22 0.009(3) 0.010(3) 0.009(3) -0.003(3) 0.001(2) -0.003(3) C23 0.010(3) 0.009(3) 0.019(3) -0.003(3) -0.002(3) -0.003(3) C24 0.009(3) 0.012(4) 0.014(3) 0.003(3) 0.004(3) 0.001(3) C25 0.013(4) 0.007(3) 0.026(4) -0.004(3) 0.003(3) -0.001(3) C26 0.014(3) 0.006(3) 0.023(5) 0.006(3) 0.003(3) -0.001(3) C27 0.013(3) 0.017(4) 0.020(4) -0.001(3) -0.004(3) 0.005(3) C28 0.012(3) 0.011(4) 0.016(3) -0.003(3) 0.001(3) 0.004(3) C29 0.020(3) 0.021(4) 0.009(5) 0.004(3) 0.002(3) -0.003(3) C31 0.011(3) 0.010(3) 0.012(3) 0.002(3) -0.001(2) -0.004(3) C32 0.014(4) 0.010(4) 0.022(4) -0.005(3) 0.000(3) 0.000(3) C33 0.024(4) 0.029(5) 0.019(4) -0.007(4) 0.001(3) 0.008(4) C34 0.014(4) 0.038(5) 0.013(3) -0.009(4) 0.001(3) 0.000(3) C35 0.024(4) 0.027(5) 0.014(4) 0.006(4) -0.002(3) -0.002(4) C36 0.017(4) 0.014(4) 0.021(4) 0.010(4) -0.004(3) -0.004(3) C51 0.010(3) 0.016(3) 0.013(5) 0.005(3) 0.000(2) -0.003(2) Cl11 0.0187(10) 0.0226(10) 0.0380(11) -0.0067(9) 0.0016(8) 0.0018(8) Cl12 0.0264(10) 0.0188(10) 0.0393(11) -0.0010(9) 0.0000(8) 0.0066(8) C100 0.021(4) 0.028(5) 0.026(4) 0.007(4) 0.005(3) 0.006(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C41 1.910(7) . ? Re1 C51 1.919(7) . ? Re1 C61 1.930(8) . ? Re1 N21 2.159(6) . ? Re1 N11 2.218(7) . ? Re1 Cl1 2.4786(19) . ? O41 C41 1.153(8) . ? O51 C51 1.168(9) . ? O61 C61 1.107(10) . ? N11 C16 1.330(10) . ? N11 C12 1.374(9) . ? N21 C22 1.331(9) . ? N21 C29 1.342(10) . ? N23 C22 1.368(9) . ? N23 C24 1.397(8) . ? N23 C23 1.466(8) . ? C12 C13 1.364(10) . ? C12 C22 1.475(10) . ? C13 C14 1.405(10) . ? C13 H13A 0.9300 . ? C14 C15 1.384(10) . ? C14 H14A 0.9300 . ? C15 C16 1.371(10) . ? C15 H15A 0.9300 . ? C16 H16A 0.9300 . ? C23 C31 1.518(9) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.376(10) . ? C24 C29 1.398(11) . ? C25 C26 1.373(10) . ? C25 H25A 0.9300 . ? C26 C27 1.392(10) . ? C26 H26A 0.9300 . ? C27 C28 1.368(10) . ? C27 H27A 0.9300 . ? C28 C29 1.436(11) . ? C28 H28A 0.9300 . ? C31 C32 1.387(10) . ? C31 C36 1.394(10) . ? C32 C33 1.419(10) . ? C32 H32A 0.9300 . ? C33 C34 1.342(12) . ? C33 H33A 0.9300 . ? C34 C35 1.388(13) . ? C34 H34A 0.9300 . ? C35 C36 1.384(10) . ? C35 H35A 0.9300 . ? C36 H36A 0.9300 . ? Cl11 C100 1.767(9) . ? Cl12 C100 1.763(9) . ? C100 H10A 0.9700 . ? C100 H10B 0.9700 . ? 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 C41 Re1 C51 87.2(3) . . ? C41 Re1 C61 87.8(3) . . ? C51 Re1 C61 87.9(3) . . ? C41 Re1 N21 100.3(3) . . ? C51 Re1 N21 172.2(2) . . ? C61 Re1 N21 94.2(3) . . ? C41 Re1 N11 173.7(3) . . ? C51 Re1 N11 97.9(2) . . ? C61 Re1 N11 96.0(3) . . ? N21 Re1 N11 74.4(2) . . ? C41 Re1 Cl1 93.0(2) . . ? C51 Re1 Cl1 94.48(19) . . ? C61 Re1 Cl1 177.5(2) . . ? N21 Re1 Cl1 83.31(16) . . ? N11 Re1 Cl1 82.91(18) . . ? C16 N11 C12 119.5(7) . . ? C16 N11 Re1 123.0(5) . . ? C12 N11 Re1 117.0(5) . . ? C22 N21 C29 106.6(6) . . ? C22 N21 Re1 116.6(5) . . ? C29 N21 Re1 136.8(5) . . ? C22 N23 C24 107.1(5) . . ? C22 N23 C23 131.4(6) . . ? C24 N23 C23 121.5(6) . . ? C13 C12 N11 120.4(7) . . ? C13 C12 C22 127.7(7) . . ? N11 C12 C22 111.9(6) . . ? C12 C13 C14 120.2(7) . . ? C12 C13 H13A 119.9 . . ? C14 C13 H13A 119.9 . . ? C15 C14 C13 117.9(7) . . ? C15 C14 H14A 121.1 . . ? C13 C14 H14A 121.1 . . ? C16 C15 C14 119.7(7) . . ? C16 C15 H15A 120.2 . . ? C14 C15 H15A 120.2 . . ? N11 C16 C15 122.3(7) . . ? N11 C16 H16A 118.9 . . ? C15 C16 H16A 118.9 . . ? N21 C22 N23 111.0(6) . . ? N21 C22 C12 119.6(6) . . ? N23 C22 C12 129.4(6) . . ? N23 C23 C31 112.4(5) . . ? N23 C23 H23A 109.1 . . ? C31 C23 H23A 109.1 . . ? N23 C23 H23B 109.1 . . ? C31 C23 H23B 109.1 . . ? H23A C23 H23B 107.9 . . ? C25 C24 N23 131.8(7) . . ? C25 C24 C29 124.0(7) . . ? N23 C24 C29 104.2(6) . . ? C26 C25 C24 116.2(7) . . ? C26 C25 H25A 121.9 . . ? C24 C25 H25A 121.9 . . ? C25 C26 C27 122.4(7) . . ? C25 C26 H26A 118.8 . . ? C27 C26 H26A 118.8 . . ? C28 C27 C26 121.8(7) . . ? C28 C27 H27A 119.1 . . ? C26 C27 H27A 119.1 . . ? C27 C28 C29 117.4(7) . . ? C27 C28 H28A 121.3 . . ? C29 C28 H28A 121.3 . . ? N21 C29 C24 111.0(7) . . ? N21 C29 C28 130.7(8) . . ? C24 C29 C28 118.2(7) . . ? C32 C31 C36 119.5(7) . . ? C32 C31 C23 118.1(6) . . ? C36 C31 C23 122.3(7) . . ? C31 C32 C33 119.4(7) . . ? C31 C32 H32A 120.3 . . ? C33 C32 H32A 120.3 . . ? C34 C33 C32 120.3(8) . . ? C34 C33 H33A 119.9 . . ? C32 C33 H33A 119.9 . . ? C33 C34 C35 120.6(7) . . ? C33 C34 H34A 119.7 . . ? C35 C34 H34A 119.7 . . ? C36 C35 C34 120.3(9) . . ? C36 C35 H35A 119.9 . . ? C34 C35 H35A 119.9 . . ? C35 C36 C31 119.8(9) . . ? C35 C36 H36A 120.1 . . ? C31 C36 H36A 120.1 . . ? O41 C41 Re1 177.3(6) . . ? O51 C51 Re1 177.5(6) . . ? O61 C61 Re1 178.2(7) . . ? Cl12 C100 Cl11 111.4(4) . . ? Cl12 C100 H10A 109.3 . . ? Cl11 C100 H10A 109.3 . . ? Cl12 C100 H10B 109.3 . . ? Cl11 C100 H10B 109.3 . . ? H10A C100 H10B 108.0 . . ? 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 C51 Re1 N11 C16 0.3(6) . . . . ? C61 Re1 N11 C16 -88.4(6) . . . . ? N21 Re1 N11 C16 178.9(6) . . . . ? Cl1 Re1 N11 C16 93.9(6) . . . . ? C51 Re1 N11 C12 -171.9(5) . . . . ? C61 Re1 N11 C12 99.3(6) . . . . ? N21 Re1 N11 C12 6.6(5) . . . . ? Cl1 Re1 N11 C12 -78.4(5) . . . . ? C41 Re1 N21 C22 172.1(5) . . . . ? C61 Re1 N21 C22 -99.4(5) . . . . ? N11 Re1 N21 C22 -4.3(5) . . . . ? Cl1 Re1 N21 C22 80.2(5) . . . . ? C41 Re1 N21 C29 -7.2(8) . . . . ? C61 Re1 N21 C29 81.3(8) . . . . ? N11 Re1 N21 C29 176.4(8) . . . . ? Cl1 Re1 N21 C29 -99.1(8) . . . . ? C16 N11 C12 C13 0.7(11) . . . . ? Re1 N11 C12 C13 173.3(5) . . . . ? C16 N11 C12 C22 179.9(6) . . . . ? Re1 N11 C12 C22 -7.6(8) . . . . ? N11 C12 C13 C14 1.1(11) . . . . ? C22 C12 C13 C14 -177.8(7) . . . . ? C12 C13 C14 C15 -2.4(12) . . . . ? C13 C14 C15 C16 1.8(12) . . . . ? C12 N11 C16 C15 -1.4(11) . . . . ? Re1 N11 C16 C15 -173.4(6) . . . . ? C14 C15 C16 N11 0.1(12) . . . . ? C29 N21 C22 N23 -0.9(8) . . . . ? Re1 N21 C22 N23 179.6(4) . . . . ? C29 N21 C22 C12 -178.8(6) . . . . ? Re1 N21 C22 C12 1.7(8) . . . . ? C24 N23 C22 N21 -0.2(7) . . . . ? C23 N23 C22 N21 177.5(6) . . . . ? C24 N23 C22 C12 177.4(6) . . . . ? C23 N23 C22 C12 -4.9(11) . . . . ? C13 C12 C22 N21 -177.0(7) . . . . ? N11 C12 C22 N21 4.0(9) . . . . ? C13 C12 C22 N23 5.5(12) . . . . ? N11 C12 C22 N23 -173.5(7) . . . . ? C22 N23 C23 C31 -90.0(8) . . . . ? C24 N23 C23 C31 87.5(7) . . . . ? C22 N23 C24 C25 -179.4(7) . . . . ? C23 N23 C24 C25 2.6(11) . . . . ? C22 N23 C24 C29 1.2(7) . . . . ? C23 N23 C24 C29 -176.8(6) . . . . ? N23 C24 C25 C26 178.4(7) . . . . ? C29 C24 C25 C26 -2.4(11) . . . . ? C24 C25 C26 C27 1.1(10) . . . . ? C25 C26 C27 C28 0.8(11) . . . . ? C26 C27 C28 C29 -1.5(11) . . . . ? C22 N21 C29 C24 1.7(9) . . . . ? Re1 N21 C29 C24 -179.0(5) . . . . ? C22 N21 C29 C28 178.3(8) . . . . ? Re1 N21 C29 C28 -2.4(15) . . . . ? C25 C24 C29 N21 178.8(7) . . . . ? N23 C24 C29 N21 -1.8(9) . . . . ? C25 C24 C29 C28 1.7(11) . . . . ? N23 C24 C29 C28 -178.9(7) . . . . ? C27 C28 C29 N21 -176.1(8) . . . . ? C27 C28 C29 C24 0.3(11) . . . . ? N23 C23 C31 C32 -135.5(6) . . . . ? N23 C23 C31 C36 47.7(9) . . . . ? C36 C31 C32 C33 -1.6(11) . . . . ? C23 C31 C32 C33 -178.6(7) . . . . ? C31 C32 C33 C34 1.4(12) . . . . ? C32 C33 C34 C35 -2.0(13) . . . . ? C33 C34 C35 C36 2.9(13) . . . . ? C34 C35 C36 C31 -3.1(12) . . . . ? C32 C31 C36 C35 2.5(11) . . . . ? C23 C31 C36 C35 179.3(7) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 3.529 _refine_diff_density_min -1.852 _refine_diff_density_rms 0.192 #=END data_tapes _database_code_depnum_ccdc_archive 'CCDC 245720' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C47 H35 N7 Ru, C3 H6 O, 2(F6 P)' _chemical_formula_sum 'C50 H41 F12 N7 O P2 Ru' _chemical_formula_weight 1146.91 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' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 22.253(7) _cell_length_b 8.776(3) _cell_length_c 26.835(13) _cell_angle_alpha 90.00 _cell_angle_beta 113.88(2) _cell_angle_gamma 90.00 _cell_volume 4792(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 45 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2320 _exptl_absorpt_coefficient_mu 0.488 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 0.98 _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 'CCD area detector' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean 8.2 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 17884 _diffrn_reflns_av_R_equivalents 0.1463 _diffrn_reflns_av_sigmaI/netI 0.2473 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 25.02 _reflns_number_total 8428 _reflns_number_gt 3115 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1998)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1998)' _computing_data_reduction 'Bruker SHELXTL (Bruker, 1998)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 1998)' _computing_structure_refinement 'Bruker SHELXTL (Bruker, 1998)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1998)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1998)' _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^)+(0.0686P)^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 8428 _refine_ls_number_parameters 660 _refine_ls_number_restraints 84 _refine_ls_R_factor_all 0.2293 _refine_ls_R_factor_gt 0.0721 _refine_ls_wR_factor_ref 0.1930 _refine_ls_wR_factor_gt 0.1393 _refine_ls_goodness_of_fit_ref 0.935 _refine_ls_restrained_S_all 0.971 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.04008(4) 1.04061(9) 0.32318(3) 0.0419(3) Uani 1 1 d . . . N11 N -0.0393(3) 1.1081(8) 0.2528(3) 0.040(2) Uani 1 1 d . . . N21 N 0.0675(3) 0.9713(8) 0.2620(3) 0.0390(18) Uani 1 1 d . . . N23 N 0.0512(4) 0.9750(9) 0.1743(3) 0.050(2) Uani 1 1 d . . . N31 N -0.0133(4) 0.8506(10) 0.3250(4) 0.056(2) Uani 1 1 d . . . N41 N 0.0004(4) 1.1081(11) 0.3768(3) 0.053(2) Uani 1 1 d . . . N51 N 0.0978(4) 1.2275(9) 0.3314(3) 0.044(2) Uani 1 1 d . . . N61 N 0.1226(4) 0.9854(10) 0.3916(3) 0.047(2) Uani 1 1 d . . . C12 C -0.0376(4) 1.0687(11) 0.2042(4) 0.043(3) Uani 1 1 d . . . C13 C -0.0917(5) 1.0897(11) 0.1563(4) 0.054(3) Uani 1 1 d . . . H13A H -0.0906 1.0581 0.1228 0.064 Uiso 1 1 calc R . . C14 C -0.1477(5) 1.1564(12) 0.1565(5) 0.065(3) Uani 1 1 d . . . H14A H -0.1853 1.1707 0.1234 0.078 Uiso 1 1 calc R . . C15 C -0.1479(5) 1.2019(12) 0.2053(5) 0.066(3) Uani 1 1 d . . . H15A H -0.1850 1.2537 0.2061 0.079 Uiso 1 1 calc R . . C16 C -0.0942(5) 1.1721(11) 0.2530(4) 0.051(3) Uani 1 1 d . . . H16A H -0.0960 1.1972 0.2869 0.062 Uiso 1 1 calc R . . C32 C -0.0438(5) 0.8609(14) 0.3599(5) 0.057(3) Uani 1 1 d . . . C22 C 0.0259(4) 1.0027(10) 0.2115(4) 0.041(3) Uani 1 1 d . . . C23 C 0.0179(5) 0.9988(12) 0.1149(3) 0.055(3) Uani 1 1 d . . . H23A H -0.0154 1.0802 0.1076 0.066 Uiso 1 1 calc R . . H23B H -0.0054 0.9041 0.0977 0.066 Uiso 1 1 calc R . . C24 C 0.1128(5) 0.9099(11) 0.2030(4) 0.047(3) Uani 1 1 d . . . C25 C 0.1603(5) 0.8523(12) 0.1871(4) 0.062(3) Uani 1 1 d . . . H25A H 0.1542 0.8549 0.1500 0.075 Uiso 1 1 calc R . . C26 C 0.2169(5) 0.7908(13) 0.2264(5) 0.062(3) Uani 1 1 d . . . H26A H 0.2492 0.7468 0.2161 0.075 Uiso 1 1 calc R . . C27 C 0.2269(5) 0.7933(11) 0.2817(4) 0.055(3) Uani 1 1 d . . . H27A H 0.2661 0.7514 0.3084 0.066 Uiso 1 1 calc R . . C28 C 0.1803(5) 0.8561(11) 0.2980(4) 0.046(3) Uani 1 1 d . . . H28A H 0.1879 0.8615 0.3354 0.055 Uiso 1 1 calc R . . C29 C 0.1230(4) 0.9101(10) 0.2583(4) 0.039(2) Uani 1 1 d . . . C33 C -0.0808(6) 0.7375(17) 0.3648(6) 0.082(4) Uani 1 1 d . . . H33A H -0.1026 0.7446 0.3887 0.098 Uiso 1 1 calc R . . C34 C -0.0860(6) 0.6091(17) 0.3361(6) 0.092(5) Uani 1 1 d . . . H34A H -0.1105 0.5251 0.3402 0.111 Uiso 1 1 calc R . . C35 C -0.0558(6) 0.6003(12) 0.3011(5) 0.074(4) Uani 1 1 d . . . H35A H -0.0595 0.5110 0.2800 0.089 Uiso 1 1 calc R . . C36 C -0.0197(5) 0.7234(14) 0.2968(5) 0.062(3) Uani 1 1 d . . . H36A H 0.0016 0.7166 0.2725 0.075 Uiso 1 1 calc R . . C42 C -0.0361(5) 1.0022(13) 0.3895(4) 0.054(3) Uani 1 1 d . . . C43 C -0.0625(5) 1.0346(17) 0.4264(5) 0.079(4) Uani 1 1 d . . . H43A H -0.0861 0.9581 0.4360 0.095 Uiso 1 1 calc R . . C44 C -0.0550(6) 1.179(2) 0.4500(5) 0.093(5) Uani 1 1 d . . . H44A H -0.0748 1.2041 0.4744 0.112 Uiso 1 1 calc R . . C45 C -0.0185(6) 1.2823(16) 0.4369(5) 0.079(4) Uani 1 1 d . . . H45A H -0.0117 1.3807 0.4530 0.095 Uiso 1 1 calc R . . C46 C 0.0087(5) 1.2470(15) 0.4007(4) 0.066(3) Uani 1 1 d . . . H46A H 0.0340 1.3217 0.3923 0.079 Uiso 1 1 calc R . . C52 C 0.1566(5) 1.2315(13) 0.3760(4) 0.046(3) Uani 1 1 d . . . C53 C 0.1998(5) 1.3496(13) 0.3852(4) 0.058(3) Uani 1 1 d . . . H53A H 0.2399 1.3488 0.4168 0.070 Uiso 1 1 calc R . . C54 C 0.1862(5) 1.4689(14) 0.3495(4) 0.064(3) Uani 1 1 d . . . H54A H 0.2160 1.5518 0.3564 0.076 Uiso 1 1 calc R . . C55 C 0.1281(5) 1.4666(12) 0.3031(4) 0.057(3) Uani 1 1 d . . . H55A H 0.1176 1.5460 0.2769 0.068 Uiso 1 1 calc R . . C56 C 0.0864(5) 1.3474(12) 0.2962(4) 0.050(3) Uani 1 1 d . . . H56A H 0.0464 1.3473 0.2645 0.060 Uiso 1 1 calc R . . C62 C 0.1689(5) 1.0950(12) 0.4114(4) 0.048(3) Uani 1 1 d . . . C63 C 0.2218(5) 1.0804(14) 0.4606(5) 0.066(3) Uani 1 1 d . . . H63A H 0.2530 1.1602 0.4745 0.079 Uiso 1 1 calc R . . C64 C 0.2282(6) 0.9463(18) 0.4892(5) 0.075(4) Uani 1 1 d . . . H64A H 0.2650 0.9324 0.5229 0.090 Uiso 1 1 calc R . . C65 C 0.1826(6) 0.8343(15) 0.4701(5) 0.071(4) Uani 1 1 d . . . H65A H 0.1865 0.7435 0.4904 0.085 Uiso 1 1 calc R . . C66 C 0.1309(5) 0.8547(12) 0.4208(4) 0.056(3) Uani 1 1 d . . . H66A H 0.0998 0.7749 0.4066 0.068 Uiso 1 1 calc R . . C71 C 0.0657(5) 1.0435(15) 0.0883(4) 0.052(3) Uani 1 1 d . . . C72 C 0.0763(5) 0.9432(15) 0.0531(4) 0.057(3) Uani 1 1 d . . . C73 C 0.0470(6) 0.7948(17) 0.0394(5) 0.079(4) Uani 1 1 d . . . H73A H 0.0173 0.7609 0.0544 0.095 Uiso 1 1 calc R . . C74 C 0.0613(7) 0.7039(16) 0.0057(5) 0.088(4) Uani 1 1 d . . . H74A H 0.0420 0.6054 -0.0017 0.106 Uiso 1 1 calc R . . C75 C 0.1036(7) 0.7463(19) -0.0195(5) 0.088(5) Uani 1 1 d . . . H75A H 0.1109 0.6813 -0.0448 0.106 Uiso 1 1 calc R . . C76 C 0.1328(7) 0.881(2) -0.0062(5) 0.092(5) Uani 1 1 d . . . H76A H 0.1649 0.9065 -0.0197 0.110 Uiso 1 1 calc R . . C77 C 0.1193(5) 0.9880(17) 0.0265(4) 0.062(3) Uani 1 1 d . . . C78 C 0.1475(6) 1.131(2) 0.0379(5) 0.087(4) Uani 1 1 d . . . H78A H 0.1760 1.1607 0.0211 0.105 Uiso 1 1 calc R . . C79 C 0.1366(6) 1.2330(17) 0.0719(5) 0.072(4) Uani 1 1 d . . . C80 C 0.1644(6) 1.3822(19) 0.0824(5) 0.089(4) Uani 1 1 d . . . H80A H 0.1925 1.4119 0.0653 0.107 Uiso 1 1 calc R . . C81 C 0.1529(8) 1.4832(17) 0.1154(7) 0.106(5) Uani 1 1 d . . . H81A H 0.1726 1.5814 0.1212 0.127 Uiso 1 1 calc R . . C82 C 0.1109(7) 1.4410(17) 0.1414(6) 0.096(4) Uani 1 1 d . . . H82A H 0.1010 1.5126 0.1636 0.115 Uiso 1 1 calc R . . C83 C 0.0846(6) 1.2961(16) 0.1345(5) 0.082(4) Uani 1 1 d . . . H83A H 0.0589 1.2682 0.1540 0.098 Uiso 1 1 calc R . . C84 C 0.0943(5) 1.1878(15) 0.0996(5) 0.059(3) Uani 1 1 d . . . P1 P -0.06890(17) 0.5887(4) 0.13874(16) 0.0759(11) Uani 1 1 d . . . P2 P 0.16342(18) 1.4146(4) 0.53483(14) 0.0740(10) Uani 1 1 d . . . F11 F -0.0971(5) 0.7402(11) 0.1114(7) 0.253(8) Uani 1 1 d . . . F12 F -0.0972(5) 0.6164(18) 0.1809(4) 0.240(7) Uani 1 1 d . . . F13 F -0.0005(4) 0.6664(11) 0.1759(4) 0.158(3) Uani 1 1 d U . . F14 F -0.0412(4) 0.5695(11) 0.0950(3) 0.148(3) Uani 1 1 d U . . F15 F -0.1349(3) 0.5105(8) 0.1031(3) 0.102(2) Uani 1 1 d U . . F16 F -0.0381(4) 0.4361(10) 0.1650(4) 0.146(3) Uani 1 1 d U . . F21 F 0.2291(4) 1.3867(11) 0.5292(3) 0.142(3) Uani 1 1 d U . . F22 F 0.1886(5) 1.5785(9) 0.5576(3) 0.143(3) Uani 1 1 d U . . F23 F 0.1371(3) 1.2517(8) 0.5127(3) 0.109(2) Uani 1 1 d U . . F24 F 0.1944(3) 1.3549(8) 0.5957(3) 0.100(2) Uani 1 1 d U . . F25 F 0.1320(4) 1.4770(10) 0.4752(3) 0.145(3) Uani 1 1 d U . . F26 F 0.0963(3) 1.4448(9) 0.5395(3) 0.113(2) Uani 1 1 d U . . O102 O -0.1808(5) 1.2491(13) 0.3134(4) 0.133(4) Uani 1 1 d U . . C102 C -0.2319(7) 1.222(2) 0.3183(6) 0.108(6) Uani 1 1 d U . . C101 C -0.2826(7) 1.3368(17) 0.3026(7) 0.137(6) Uani 1 1 d U . . H10A H -0.2974 1.3513 0.3320 0.205 Uiso 1 1 calc R . . H10B H -0.3198 1.3041 0.2695 0.205 Uiso 1 1 calc R . . H10C H -0.2651 1.4330 0.2956 0.205 Uiso 1 1 calc R . . C103 C -0.2410(7) 1.085(2) 0.3434(9) 0.191(10) Uani 1 1 d U . . H10D H -0.2668 1.0123 0.3151 0.287 Uiso 1 1 calc R . . H10E H -0.2644 1.1086 0.3665 0.287 Uiso 1 1 calc R . . H10F H -0.1981 1.0406 0.3656 0.287 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 Ru1 0.0381(4) 0.0480(5) 0.0443(5) 0.0034(5) 0.0214(4) 0.0007(5) N11 0.041(5) 0.038(5) 0.048(5) -0.006(4) 0.024(4) -0.010(4) N21 0.029(4) 0.039(5) 0.050(5) -0.004(4) 0.018(4) -0.005(4) N23 0.037(5) 0.068(6) 0.043(5) 0.000(5) 0.016(4) 0.004(5) N31 0.044(5) 0.061(6) 0.074(7) 0.009(5) 0.037(5) 0.004(5) N41 0.039(5) 0.072(7) 0.050(6) 0.001(5) 0.020(5) 0.008(5) N51 0.054(6) 0.045(5) 0.039(5) 0.004(4) 0.024(5) 0.006(5) N61 0.046(5) 0.058(6) 0.046(5) 0.015(5) 0.027(4) 0.010(5) C12 0.038(6) 0.047(7) 0.046(6) -0.001(6) 0.019(5) -0.003(5) C13 0.036(6) 0.077(8) 0.047(7) 0.009(6) 0.015(5) -0.005(6) C14 0.039(7) 0.071(8) 0.075(9) 0.022(7) 0.014(6) 0.009(6) C15 0.056(8) 0.068(9) 0.079(9) 0.001(8) 0.033(8) 0.008(7) C16 0.037(6) 0.069(8) 0.052(7) 0.004(6) 0.022(6) 0.006(6) C32 0.039(6) 0.072(9) 0.074(8) 0.015(7) 0.036(6) 0.004(6) C22 0.035(5) 0.059(8) 0.033(6) -0.002(5) 0.018(5) -0.008(5) C23 0.055(6) 0.081(9) 0.026(6) 0.008(5) 0.012(5) 0.008(6) C24 0.038(6) 0.066(8) 0.047(7) 0.002(6) 0.026(5) 0.005(5) C25 0.066(8) 0.097(9) 0.030(6) -0.002(6) 0.025(6) 0.010(7) C26 0.041(7) 0.093(9) 0.059(8) -0.003(7) 0.026(6) 0.011(6) C27 0.047(7) 0.057(7) 0.057(8) 0.009(6) 0.017(6) 0.000(6) C28 0.040(6) 0.057(7) 0.048(7) -0.010(6) 0.025(6) -0.006(6) C29 0.037(6) 0.045(7) 0.034(6) 0.002(5) 0.015(5) -0.004(5) C33 0.080(9) 0.084(10) 0.104(11) 0.034(9) 0.062(9) 0.008(9) C34 0.077(10) 0.082(11) 0.141(14) 0.039(10) 0.069(10) -0.002(9) C35 0.083(9) 0.038(7) 0.101(10) 0.007(7) 0.038(8) -0.014(7) C36 0.056(7) 0.064(9) 0.073(9) 0.016(7) 0.032(7) 0.000(7) C42 0.045(6) 0.077(10) 0.053(7) 0.008(6) 0.032(6) 0.011(6) C43 0.067(8) 0.120(12) 0.062(8) 0.030(9) 0.040(7) 0.024(9) C44 0.054(9) 0.177(16) 0.065(9) 0.011(10) 0.041(8) 0.042(10) C45 0.055(8) 0.112(11) 0.073(9) -0.019(8) 0.027(7) 0.029(8) C46 0.057(8) 0.087(10) 0.053(8) 0.007(7) 0.023(6) 0.018(7) C52 0.035(6) 0.058(8) 0.043(7) -0.007(6) 0.014(6) -0.003(6) C53 0.043(7) 0.066(8) 0.061(8) -0.003(7) 0.016(6) -0.003(7) C54 0.065(8) 0.056(8) 0.060(7) -0.009(7) 0.014(6) -0.007(7) C55 0.059(7) 0.044(6) 0.068(7) 0.009(7) 0.026(6) -0.012(7) C56 0.040(6) 0.058(7) 0.045(7) -0.002(6) 0.010(5) -0.005(6) C62 0.040(6) 0.051(8) 0.057(8) -0.010(6) 0.025(6) -0.005(6) C63 0.059(8) 0.076(10) 0.059(8) -0.005(7) 0.021(7) 0.003(7) C64 0.058(8) 0.116(12) 0.049(7) 0.021(9) 0.019(6) 0.022(9) C65 0.064(8) 0.096(10) 0.053(8) 0.031(8) 0.025(7) 0.010(8) C66 0.051(7) 0.065(8) 0.058(8) 0.013(7) 0.028(7) 0.007(6) C71 0.050(6) 0.074(8) 0.038(6) 0.013(7) 0.023(5) 0.008(7) C72 0.058(7) 0.081(9) 0.029(6) 0.007(7) 0.014(5) 0.013(7) C73 0.074(9) 0.113(12) 0.051(8) -0.009(8) 0.026(7) -0.002(9) C74 0.089(10) 0.099(11) 0.063(9) 0.004(9) 0.016(8) 0.022(9) C75 0.086(11) 0.121(13) 0.043(8) -0.033(9) 0.012(8) 0.038(10) C76 0.079(10) 0.155(15) 0.031(8) 0.004(9) 0.012(7) 0.033(11) C77 0.041(7) 0.103(11) 0.040(7) 0.004(7) 0.015(6) 0.012(7) C78 0.061(9) 0.141(15) 0.052(9) 0.014(10) 0.016(7) 0.003(10) C79 0.058(8) 0.089(11) 0.059(9) 0.034(8) 0.011(7) -0.001(8) C80 0.084(10) 0.107(13) 0.077(10) 0.017(9) 0.034(8) -0.030(10) C81 0.125(14) 0.075(12) 0.107(13) 0.015(10) 0.036(11) 0.010(10) C82 0.106(12) 0.071(11) 0.096(11) -0.003(10) 0.024(9) 0.023(10) C83 0.070(9) 0.073(10) 0.097(11) 0.019(9) 0.028(8) 0.022(8) C84 0.056(8) 0.060(9) 0.057(8) 0.016(7) 0.017(6) 0.010(7) P1 0.067(2) 0.076(3) 0.091(3) -0.018(2) 0.038(2) -0.015(2) P2 0.087(3) 0.086(3) 0.062(2) -0.005(2) 0.043(2) -0.016(2) F11 0.158(10) 0.098(8) 0.53(3) 0.030(11) 0.165(14) 0.021(7) F12 0.130(8) 0.47(2) 0.161(9) -0.176(12) 0.099(7) -0.082(10) F13 0.119(6) 0.171(7) 0.190(7) -0.055(6) 0.068(6) -0.055(6) F14 0.146(6) 0.205(7) 0.121(6) -0.007(5) 0.082(5) -0.001(6) F15 0.062(4) 0.121(6) 0.111(5) -0.011(4) 0.023(4) -0.008(4) F16 0.084(5) 0.129(6) 0.186(7) 0.070(6) 0.013(5) -0.017(5) F21 0.094(5) 0.238(8) 0.130(6) -0.042(5) 0.082(5) -0.037(5) F22 0.203(7) 0.108(6) 0.092(5) 0.004(4) 0.033(5) -0.041(5) F23 0.087(5) 0.087(5) 0.152(6) -0.020(4) 0.047(4) 0.000(4) F24 0.071(4) 0.147(6) 0.089(5) 0.028(4) 0.039(4) -0.006(4) F25 0.169(6) 0.174(7) 0.080(5) 0.024(5) 0.039(5) -0.058(6) F26 0.100(5) 0.147(6) 0.100(5) 0.006(5) 0.047(4) 0.047(5) O102 0.099(8) 0.200(11) 0.124(8) 0.028(8) 0.071(7) 0.031(8) C102 0.046(9) 0.167(17) 0.121(13) -0.023(12) 0.044(9) -0.011(11) C101 0.088(11) 0.132(14) 0.190(17) -0.030(13) 0.056(12) 0.013(11) C103 0.069(11) 0.143(17) 0.34(3) 0.074(18) 0.062(14) -0.015(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 N51 2.040(8) . ? Ru1 N41 2.056(8) . ? Ru1 N31 2.059(9) . ? Ru1 N61 2.061(8) . ? Ru1 N21 2.061(7) . ? Ru1 N11 2.082(7) . ? N11 C16 1.349(10) . ? N11 C12 1.365(10) . ? N21 C22 1.324(10) . ? N21 C29 1.387(10) . ? N23 C22 1.353(10) . ? N23 C24 1.393(11) . ? N23 C23 1.475(10) . ? N31 C36 1.323(12) . ? N31 C32 1.366(11) . ? N41 C46 1.356(12) . ? N41 C42 1.366(11) . ? N51 C56 1.367(11) . ? N51 C52 1.370(11) . ? N61 C62 1.351(11) . ? N61 C66 1.360(11) . ? C12 C13 1.372(12) . ? C12 C22 1.466(12) . ? C13 C14 1.377(12) . ? C13 H13A 0.9500 . ? C14 C15 1.371(13) . ? C14 H14A 0.9500 . ? C15 C16 1.378(13) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C32 C33 1.397(14) . ? C32 C42 1.445(14) . ? C23 C71 1.551(12) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.385(12) . ? C24 C29 1.409(11) . ? C25 C26 1.383(12) . ? C25 H25A 0.9500 . ? C26 C27 1.409(13) . ? C26 H26A 0.9500 . ? C27 C28 1.391(12) . ? C27 H27A 0.9500 . ? C28 C29 1.372(12) . ? C28 H28A 0.9500 . ? C33 C34 1.344(15) . ? C33 H33A 0.9500 . ? C34 C35 1.359(15) . ? C34 H34A 0.9500 . ? C35 C36 1.379(13) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C42 C43 1.369(13) . ? C43 C44 1.397(17) . ? C43 H43A 0.9500 . ? C44 C45 1.355(16) . ? C44 H44A 0.9500 . ? C45 C46 1.370(13) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? C52 C53 1.367(13) . ? C52 C62 1.484(13) . ? C53 C54 1.367(13) . ? C53 H53A 0.9500 . ? C54 C55 1.386(13) . ? C54 H54A 0.9500 . ? C55 C56 1.359(12) . ? C55 H55A 0.9500 . ? C56 H56A 0.9500 . ? C62 C63 1.373(13) . ? C63 C64 1.382(14) . ? C63 H63A 0.9500 . ? C64 C65 1.355(15) . ? C64 H64A 0.9500 . ? C65 C66 1.368(13) . ? C65 H65A 0.9500 . ? C66 H66A 0.9500 . ? C71 C72 1.379(13) . ? C71 C84 1.396(14) . ? C72 C73 1.436(15) . ? C72 C77 1.461(14) . ? C73 C74 1.338(15) . ? C73 H73A 0.9500 . ? C74 C75 1.413(17) . ? C74 H74A 0.9500 . ? C75 C76 1.326(16) . ? C75 H75A 0.9500 . ? C76 C77 1.398(16) . ? C76 H76A 0.9500 . ? C77 C78 1.383(16) . ? C78 C79 1.367(16) . ? C78 H78A 0.9500 . ? C79 C80 1.427(16) . ? C79 C84 1.470(15) . ? C80 C81 1.348(16) . ? C80 H80A 0.9500 . ? C81 C82 1.423(18) . ? C81 H81A 0.9500 . ? C82 C83 1.381(16) . ? C82 H82A 0.9500 . ? C83 C84 1.411(15) . ? C83 H83A 0.9500 . ? P1 F12 1.521(9) . ? P1 F11 1.525(11) . ? P1 F14 1.539(8) . ? P1 F16 1.539(8) . ? P1 F15 1.551(7) . ? P1 F13 1.596(8) . ? P2 F21 1.548(7) . ? P2 F25 1.564(8) . ? P2 F23 1.568(7) . ? P2 F26 1.571(7) . ? P2 F22 1.574(8) . ? P2 F24 1.584(7) . ? O102 C102 1.219(14) . ? C102 C103 1.429(19) . ? C102 C101 1.443(18) . ? C101 H10A 0.9800 . ? C101 H10B 0.9800 . ? C101 H10C 0.9800 . ? C103 H10D 0.9800 . ? C103 H10E 0.9800 . ? C103 H10F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N51 Ru1 N41 97.1(3) . . ? N51 Ru1 N31 173.1(3) . . ? N41 Ru1 N31 78.6(4) . . ? N51 Ru1 N61 78.3(3) . . ? N41 Ru1 N61 85.7(3) . . ? N31 Ru1 N61 95.9(3) . . ? N51 Ru1 N21 86.9(3) . . ? N41 Ru1 N21 172.6(3) . . ? N31 Ru1 N21 98.0(3) . . ? N61 Ru1 N21 101.3(3) . . ? N51 Ru1 N11 97.8(3) . . ? N41 Ru1 N11 96.1(3) . . ? N31 Ru1 N11 88.1(3) . . ? N61 Ru1 N11 175.9(3) . . ? N21 Ru1 N11 77.1(3) . . ? C16 N11 C12 119.1(8) . . ? C16 N11 Ru1 123.5(7) . . ? C12 N11 Ru1 117.0(6) . . ? C22 N21 C29 106.3(7) . . ? C22 N21 Ru1 116.4(6) . . ? C29 N21 Ru1 136.9(6) . . ? C22 N23 C24 106.0(7) . . ? C22 N23 C23 126.5(8) . . ? C24 N23 C23 127.4(8) . . ? C36 N31 C32 118.7(9) . . ? C36 N31 Ru1 126.8(7) . . ? C32 N31 Ru1 114.5(8) . . ? C46 N41 C42 118.3(9) . . ? C46 N41 Ru1 125.2(8) . . ? C42 N41 Ru1 116.5(8) . . ? C56 N51 C52 115.3(8) . . ? C56 N51 Ru1 127.7(7) . . ? C52 N51 Ru1 116.9(7) . . ? C62 N61 C66 118.0(9) . . ? C62 N61 Ru1 116.5(7) . . ? C66 N61 Ru1 125.2(7) . . ? N11 C12 C13 120.5(8) . . ? N11 C12 C22 111.7(8) . . ? C13 C12 C22 127.8(9) . . ? C12 C13 C14 120.4(10) . . ? C12 C13 H13A 119.8 . . ? C14 C13 H13A 119.8 . . ? C15 C14 C13 118.7(11) . . ? C15 C14 H14A 120.7 . . ? C13 C14 H14A 120.7 . . ? C14 C15 C16 119.7(10) . . ? C14 C15 H15A 120.1 . . ? C16 C15 H15A 120.1 . . ? N11 C16 C15 121.4(10) . . ? N11 C16 H16A 119.3 . . ? C15 C16 H16A 119.3 . . ? N31 C32 C33 119.2(11) . . ? N31 C32 C42 116.9(10) . . ? C33 C32 C42 123.9(11) . . ? N21 C22 N23 113.1(8) . . ? N21 C22 C12 117.1(8) . . ? N23 C22 C12 129.8(8) . . ? N23 C23 C71 113.2(7) . . ? N23 C23 H23A 108.9 . . ? C71 C23 H23A 108.9 . . ? N23 C23 H23B 108.9 . . ? C71 C23 H23B 108.9 . . ? H23A C23 H23B 107.8 . . ? C25 C24 N23 133.0(9) . . ? C25 C24 C29 120.5(9) . . ? N23 C24 C29 106.5(8) . . ? C26 C25 C24 118.8(9) . . ? C26 C25 H25A 120.6 . . ? C24 C25 H25A 120.6 . . ? C25 C26 C27 120.2(9) . . ? C25 C26 H26A 119.9 . . ? C27 C26 H26A 119.9 . . ? C28 C27 C26 121.1(10) . . ? C28 C27 H27A 119.4 . . ? C26 C27 H27A 119.4 . . ? C29 C28 C27 118.1(9) . . ? C29 C28 H28A 121.0 . . ? C27 C28 H28A 121.0 . . ? C28 C29 N21 130.8(9) . . ? C28 C29 C24 121.3(9) . . ? N21 C29 C24 107.9(8) . . ? C34 C33 C32 120.9(12) . . ? C34 C33 H33A 119.6 . . ? C32 C33 H33A 119.6 . . ? C33 C34 C35 119.5(12) . . ? C33 C34 H34A 120.3 . . ? C35 C34 H34A 120.3 . . ? C34 C35 C36 118.7(12) . . ? C34 C35 H35A 120.6 . . ? C36 C35 H35A 120.6 . . ? N31 C36 C35 123.0(11) . . ? N31 C36 H36A 118.5 . . ? C35 C36 H36A 118.5 . . ? N41 C42 C43 120.8(11) . . ? N41 C42 C32 113.4(9) . . ? C43 C42 C32 125.8(11) . . ? C42 C43 C44 120.6(12) . . ? C42 C43 H43A 119.7 . . ? C44 C43 H43A 119.7 . . ? C45 C44 C43 117.6(12) . . ? C45 C44 H44A 121.2 . . ? C43 C44 H44A 121.2 . . ? C44 C45 C46 121.0(13) . . ? C44 C45 H45A 119.5 . . ? C46 C45 H45A 119.5 . . ? N41 C46 C45 121.7(12) . . ? N41 C46 H46A 119.2 . . ? C45 C46 H46A 119.2 . . ? C53 C52 N51 122.1(10) . . ? C53 C52 C62 124.2(10) . . ? N51 C52 C62 113.7(9) . . ? C54 C53 C52 120.9(10) . . ? C54 C53 H53A 119.6 . . ? C52 C53 H53A 119.6 . . ? C53 C54 C55 118.7(11) . . ? C53 C54 H54A 120.7 . . ? C55 C54 H54A 120.7 . . ? C56 C55 C54 118.0(10) . . ? C56 C55 H55A 121.0 . . ? C54 C55 H55A 121.0 . . ? C55 C56 N51 125.0(9) . . ? C55 C56 H56A 117.5 . . ? N51 C56 H56A 117.5 . . ? N61 C62 C63 122.1(10) . . ? N61 C62 C52 114.1(9) . . ? C63 C62 C52 123.7(10) . . ? C62 C63 C64 118.0(11) . . ? C62 C63 H63A 121.0 . . ? C64 C63 H63A 121.0 . . ? C65 C64 C63 121.0(11) . . ? C65 C64 H64A 119.5 . . ? C63 C64 H64A 119.5 . . ? C64 C65 C66 118.6(11) . . ? C64 C65 H65A 120.7 . . ? C66 C65 H65A 120.7 . . ? N61 C66 C65 122.2(11) . . ? N61 C66 H66A 118.9 . . ? C65 C66 H66A 118.9 . . ? C72 C71 C84 122.6(10) . . ? C72 C71 C23 119.5(11) . . ? C84 C71 C23 117.9(10) . . ? C71 C72 C73 124.7(11) . . ? C71 C72 C77 119.4(12) . . ? C73 C72 C77 116.0(11) . . ? C74 C73 C72 120.5(13) . . ? C74 C73 H73A 119.8 . . ? C72 C73 H73A 119.8 . . ? C73 C74 C75 123.6(14) . . ? C73 C74 H74A 118.2 . . ? C75 C74 H74A 118.2 . . ? C76 C75 C74 117.0(12) . . ? C76 C75 H75A 121.5 . . ? C74 C75 H75A 121.5 . . ? C75 C76 C77 124.3(14) . . ? C75 C76 H76A 117.9 . . ? C77 C76 H76A 117.9 . . ? C78 C77 C76 123.8(13) . . ? C78 C77 C72 117.8(12) . . ? C76 C77 C72 118.4(13) . . ? C79 C78 C77 123.5(13) . . ? C79 C78 H78A 118.2 . . ? C77 C78 H78A 118.2 . . ? C78 C79 C80 123.5(14) . . ? C78 C79 C84 119.1(13) . . ? C80 C79 C84 117.5(13) . . ? C81 C80 C79 123.5(14) . . ? C81 C80 H80A 118.2 . . ? C79 C80 H80A 118.2 . . ? C80 C81 C82 119.1(15) . . ? C80 C81 H81A 120.4 . . ? C82 C81 H81A 120.4 . . ? C83 C82 C81 120.1(14) . . ? C83 C82 H82A 120.0 . . ? C81 C82 H82A 120.0 . . ? C82 C83 C84 122.6(13) . . ? C82 C83 H83A 118.7 . . ? C84 C83 H83A 118.7 . . ? C71 C84 C83 125.2(11) . . ? C71 C84 C79 117.7(12) . . ? C83 C84 C79 117.1(12) . . ? F12 P1 F11 90.2(7) . . ? F12 P1 F14 176.9(8) . . ? F11 P1 F14 86.7(7) . . ? F12 P1 F16 92.3(7) . . ? F11 P1 F16 177.3(6) . . ? F14 P1 F16 90.7(5) . . ? F12 P1 F15 87.4(5) . . ? F11 P1 F15 89.2(6) . . ? F14 P1 F15 93.1(4) . . ? F16 P1 F15 91.8(4) . . ? F12 P1 F13 92.5(5) . . ? F11 P1 F13 91.8(6) . . ? F14 P1 F13 87.0(5) . . ? F16 P1 F13 87.2(5) . . ? F15 P1 F13 179.0(6) . . ? F21 P2 F25 90.2(5) . . ? F21 P2 F23 92.3(4) . . ? F25 P2 F23 89.3(5) . . ? F21 P2 F26 178.8(5) . . ? F25 P2 F26 88.7(5) . . ? F23 P2 F26 87.9(4) . . ? F21 P2 F22 88.9(5) . . ? F25 P2 F22 91.1(4) . . ? F23 P2 F22 178.7(5) . . ? F26 P2 F22 90.9(5) . . ? F21 P2 F24 90.9(4) . . ? F25 P2 F24 178.5(5) . . ? F23 P2 F24 91.6(4) . . ? F26 P2 F24 90.2(4) . . ? F22 P2 F24 88.0(4) . . ? O102 C102 C103 122.0(17) . . ? O102 C102 C101 118.9(18) . . ? C103 C102 C101 118.8(14) . . ? C102 C101 H10A 109.5 . . ? C102 C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? C102 C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? C102 C103 H10D 109.5 . . ? C102 C103 H10E 109.5 . . ? H10D C103 H10E 109.5 . . ? C102 C103 H10F 109.5 . . ? H10D C103 H10F 109.5 . . ? H10E C103 H10F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N51 Ru1 N11 C16 -98.5(7) . . . . ? N41 Ru1 N11 C16 -0.5(8) . . . . ? N31 Ru1 N11 C16 77.7(7) . . . . ? N21 Ru1 N11 C16 176.4(8) . . . . ? N51 Ru1 N11 C12 89.1(6) . . . . ? N41 Ru1 N11 C12 -172.9(6) . . . . ? N31 Ru1 N11 C12 -94.6(7) . . . . ? N21 Ru1 N11 C12 4.0(6) . . . . ? N51 Ru1 N21 C22 -97.4(7) . . . . ? N31 Ru1 N21 C22 87.4(7) . . . . ? N61 Ru1 N21 C22 -174.9(6) . . . . ? N11 Ru1 N21 C22 1.3(6) . . . . ? N51 Ru1 N21 C29 74.5(9) . . . . ? N31 Ru1 N21 C29 -100.6(9) . . . . ? N61 Ru1 N21 C29 -2.9(9) . . . . ? N11 Ru1 N21 C29 173.2(9) . . . . ? N41 Ru1 N31 C36 178.4(9) . . . . ? N61 Ru1 N31 C36 -97.2(9) . . . . ? N21 Ru1 N31 C36 5.1(9) . . . . ? N11 Ru1 N31 C36 81.8(9) . . . . ? N41 Ru1 N31 C32 -2.4(7) . . . . ? N61 Ru1 N31 C32 81.9(7) . . . . ? N21 Ru1 N31 C32 -175.7(7) . . . . ? N11 Ru1 N31 C32 -99.0(7) . . . . ? N51 Ru1 N41 C46 7.5(8) . . . . ? N31 Ru1 N41 C46 -177.9(9) . . . . ? N61 Ru1 N41 C46 85.2(8) . . . . ? N11 Ru1 N41 C46 -91.1(8) . . . . ? N51 Ru1 N41 C42 -171.3(7) . . . . ? N31 Ru1 N41 C42 3.3(7) . . . . ? N61 Ru1 N41 C42 -93.7(7) . . . . ? N11 Ru1 N41 C42 90.1(7) . . . . ? N41 Ru1 N51 C56 -102.9(8) . . . . ? N61 Ru1 N51 C56 173.1(8) . . . . ? N21 Ru1 N51 C56 70.9(8) . . . . ? N11 Ru1 N51 C56 -5.7(8) . . . . ? N41 Ru1 N51 C52 80.6(7) . . . . ? N61 Ru1 N51 C52 -3.5(6) . . . . ? N21 Ru1 N51 C52 -105.7(6) . . . . ? N11 Ru1 N51 C52 177.7(6) . . . . ? N51 Ru1 N61 C62 6.3(6) . . . . ? N41 Ru1 N61 C62 -91.8(7) . . . . ? N31 Ru1 N61 C62 -169.8(6) . . . . ? N21 Ru1 N61 C62 90.7(6) . . . . ? N51 Ru1 N61 C66 179.6(8) . . . . ? N41 Ru1 N61 C66 81.5(8) . . . . ? N31 Ru1 N61 C66 3.5(8) . . . . ? N21 Ru1 N61 C66 -95.9(7) . . . . ? C16 N11 C12 C13 -1.9(13) . . . . ? Ru1 N11 C12 C13 170.8(7) . . . . ? C16 N11 C12 C22 179.3(8) . . . . ? Ru1 N11 C12 C22 -8.0(10) . . . . ? N11 C12 C13 C14 2.6(15) . . . . ? C22 C12 C13 C14 -178.9(9) . . . . ? C12 C13 C14 C15 0.3(16) . . . . ? C13 C14 C15 C16 -3.8(17) . . . . ? C12 N11 C16 C15 -1.6(14) . . . . ? Ru1 N11 C16 C15 -173.9(8) . . . . ? C14 C15 C16 N11 4.5(17) . . . . ? C36 N31 C32 C33 -0.1(15) . . . . ? Ru1 N31 C32 C33 -179.3(8) . . . . ? C36 N31 C32 C42 -179.4(9) . . . . ? Ru1 N31 C32 C42 1.4(11) . . . . ? C29 N21 C22 N23 -3.7(10) . . . . ? Ru1 N21 C22 N23 170.6(6) . . . . ? C29 N21 C22 C12 179.7(7) . . . . ? Ru1 N21 C22 C12 -6.0(10) . . . . ? C24 N23 C22 N21 4.5(11) . . . . ? C23 N23 C22 N21 -179.6(8) . . . . ? C24 N23 C22 C12 -179.4(9) . . . . ? C23 N23 C22 C12 -3.4(16) . . . . ? N11 C12 C22 N21 9.1(12) . . . . ? C13 C12 C22 N21 -169.5(9) . . . . ? N11 C12 C22 N23 -166.9(9) . . . . ? C13 C12 C22 N23 14.5(17) . . . . ? C22 N23 C23 C71 148.1(9) . . . . ? C24 N23 C23 C71 -36.8(14) . . . . ? C22 N23 C24 C25 177.0(11) . . . . ? C23 N23 C24 C25 1.1(18) . . . . ? C22 N23 C24 C29 -3.4(10) . . . . ? C23 N23 C24 C29 -179.2(9) . . . . ? N23 C24 C25 C26 -178.4(10) . . . . ? C29 C24 C25 C26 2.0(15) . . . . ? C24 C25 C26 C27 -2.7(16) . . . . ? C25 C26 C27 C28 0.4(16) . . . . ? C26 C27 C28 C29 2.6(14) . . . . ? C27 C28 C29 N21 176.8(9) . . . . ? C27 C28 C29 C24 -3.4(14) . . . . ? C22 N21 C29 C28 -178.9(10) . . . . ? Ru1 N21 C29 C28 8.6(16) . . . . ? C22 N21 C29 C24 1.3(10) . . . . ? Ru1 N21 C29 C24 -171.2(7) . . . . ? C25 C24 C29 C28 1.2(15) . . . . ? N23 C24 C29 C28 -178.5(8) . . . . ? C25 C24 C29 N21 -179.0(9) . . . . ? N23 C24 C29 N21 1.3(10) . . . . ? N31 C32 C33 C34 0.8(18) . . . . ? C42 C32 C33 C34 -180.0(12) . . . . ? C32 C33 C34 C35 -1(2) . . . . ? C33 C34 C35 C36 1.1(19) . . . . ? C32 N31 C36 C35 -0.1(16) . . . . ? Ru1 N31 C36 C35 179.1(8) . . . . ? C34 C35 C36 N31 -0.4(18) . . . . ? C46 N41 C42 C43 -1.4(14) . . . . ? Ru1 N41 C42 C43 177.5(7) . . . . ? C46 N41 C42 C32 177.6(9) . . . . ? Ru1 N41 C42 C32 -3.5(11) . . . . ? N31 C32 C42 N41 1.4(13) . . . . ? C33 C32 C42 N41 -177.9(10) . . . . ? N31 C32 C42 C43 -179.7(9) . . . . ? C33 C32 C42 C43 1.0(17) . . . . ? N41 C42 C43 C44 2.9(16) . . . . ? C32 C42 C43 C44 -176.0(11) . . . . ? C42 C43 C44 C45 -2.9(18) . . . . ? C43 C44 C45 C46 1.5(18) . . . . ? C42 N41 C46 C45 0.0(15) . . . . ? Ru1 N41 C46 C45 -178.8(7) . . . . ? C44 C45 C46 N41 -0.1(17) . . . . ? C56 N51 C52 C53 1.8(13) . . . . ? Ru1 N51 C52 C53 178.8(7) . . . . ? C56 N51 C52 C62 -176.5(8) . . . . ? Ru1 N51 C52 C62 0.5(10) . . . . ? N51 C52 C53 C54 -0.8(15) . . . . ? C62 C52 C53 C54 177.4(9) . . . . ? C52 C53 C54 C55 -1.2(16) . . . . ? C53 C54 C55 C56 2.0(15) . . . . ? C54 C55 C56 N51 -0.9(15) . . . . ? C52 N51 C56 C55 -1.0(14) . . . . ? Ru1 N51 C56 C55 -177.6(7) . . . . ? C66 N61 C62 C63 -2.7(13) . . . . ? Ru1 N61 C62 C63 171.1(7) . . . . ? C66 N61 C62 C52 178.3(8) . . . . ? Ru1 N61 C62 C52 -7.8(10) . . . . ? C53 C52 C62 N61 -173.5(9) . . . . ? N51 C52 C62 N61 4.8(11) . . . . ? C53 C52 C62 C63 7.6(15) . . . . ? N51 C52 C62 C63 -174.1(9) . . . . ? N61 C62 C63 C64 2.2(15) . . . . ? C52 C62 C63 C64 -178.9(9) . . . . ? C62 C63 C64 C65 -1.8(17) . . . . ? C63 C64 C65 C66 1.9(17) . . . . ? C62 N61 C66 C65 2.8(14) . . . . ? Ru1 N61 C66 C65 -170.4(7) . . . . ? C64 C65 C66 N61 -2.4(16) . . . . ? N23 C23 C71 C72 112.3(10) . . . . ? N23 C23 C71 C84 -70.2(12) . . . . ? C84 C71 C72 C73 -178.8(10) . . . . ? C23 C71 C72 C73 -1.4(15) . . . . ? C84 C71 C72 C77 0.3(15) . . . . ? C23 C71 C72 C77 177.6(8) . . . . ? C71 C72 C73 C74 -178.6(10) . . . . ? C77 C72 C73 C74 2.3(15) . . . . ? C72 C73 C74 C75 -1.7(18) . . . . ? C73 C74 C75 C76 3.6(19) . . . . ? C74 C75 C76 C77 -7(2) . . . . ? C75 C76 C77 C78 -176.5(12) . . . . ? C75 C76 C77 C72 7.5(18) . . . . ? C71 C72 C77 C78 -0.3(14) . . . . ? C73 C72 C77 C78 178.8(10) . . . . ? C71 C72 C77 C76 175.9(10) . . . . ? C73 C72 C77 C76 -4.9(14) . . . . ? C76 C77 C78 C79 -176.9(11) . . . . ? C72 C77 C78 C79 -0.8(17) . . . . ? C77 C78 C79 C80 -178.4(11) . . . . ? C77 C78 C79 C84 2.0(18) . . . . ? C78 C79 C80 C81 179.1(13) . . . . ? C84 C79 C80 C81 -1.3(19) . . . . ? C79 C80 C81 C82 0(2) . . . . ? C80 C81 C82 C83 3(2) . . . . ? C81 C82 C83 C84 -3.8(19) . . . . ? C72 C71 C84 C83 179.0(10) . . . . ? C23 C71 C84 C83 1.6(15) . . . . ? C72 C71 C84 C79 0.9(15) . . . . ? C23 C71 C84 C79 -176.6(8) . . . . ? C82 C83 C84 C71 -175.7(11) . . . . ? C82 C83 C84 C79 2.4(17) . . . . ? C78 C79 C84 C71 -1.9(15) . . . . ? C80 C79 C84 C71 178.4(10) . . . . ? C78 C79 C84 C83 179.8(11) . . . . ? C80 C79 C84 C83 0.1(15) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.638 _refine_diff_density_min -0.603 _refine_diff_density_rms 0.093 #=END