Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Massimiliano Arca' 'Alexander J. Blake' 'Jaume Casabò' 'Francesco Demartin' 'Francesco A. Devillanova' 'Alessandra Garau' 'Francesco Isaia' 'Vito Lippolis' 'Raikko Kivekas' 'Vicent Muns' 'Martin Schröder' 'Gaetano Verani' _publ_contact_author_name 'Prof Vito Lippolis' _publ_contact_author_address ; Prof Vito Lippolis Dipartimento di Chimica Inorganica ed Analitica Universita di Cagliari S.S. 554 bivio Sestu Monserrato-Cagliari I-9042 ITALY ; _publ_contact_author_email 'lippolis@unica.it' data_L0.5(H2O) _database_code_CSD 156508 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H18 N2 O1 S2 0.5(H2 O)' _chemical_formula_sum 'C18 H19 N2 O1.50 S2' _chemical_formula_weight 351.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.501(2) _cell_length_b 13.314(3) _cell_length_c 13.579(5) _cell_angle_alpha 112.66(3) _cell_angle_beta 95.78(4) _cell_angle_gamma 101.85(2) _cell_volume 1680.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 14.5 _cell_measurement_theta_max 16 _exptl_crystal_description 'irregular block' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 740 _exptl_absorpt_coefficient_mu 0.326 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Stoe Stadi-4' _diffrn_measurement_method omega/theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 60 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 5962 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI 0.013 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 25.14 _reflns_number_total 5962 _reflns_number_gt 5287 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe STADI-4 (Stoe, 1997a)' _computing_cell_refinement STADI-4 _computing_data_reduction 'Stoe X-RED (Stoe, 1997b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL version 5.03 (Siemens, 1994)' _computing_publication_material 'SHELXL-97; PLATON (Spek, 2001)' _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^)+(0.0634P)^2^+2.0881P] 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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5962 _refine_ls_number_parameters 456 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0553 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1380 _refine_ls_wR_factor_gt 0.1320 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_restrained_S_all 1.124 _refine_ls_shift/su_max 0.250 _refine_ls_shift/su_mean 0.006 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N -0.4258(2) 0.21869(17) 0.30775(16) 0.0243(4) Uani 1 1 d . . . N2 N -0.30384(19) 0.11133(16) 0.14765(16) 0.0217(4) Uani 1 1 d . . . C13 C -0.2404(2) 0.06297(19) 0.07051(19) 0.0229(5) Uani 1 1 d . . . C12 C -0.2785(2) 0.0451(2) -0.03926(19) 0.0249(5) Uani 1 1 d . . . H12 H -0.2310 0.0092 -0.0924 0.030 Uiso 1 1 calc R . . C11 C -0.3843(2) 0.0800(2) -0.0678(2) 0.0249(5) Uani 1 1 d . . . H11 H -0.4127 0.0664 -0.1415 0.030 Uiso 1 1 calc R . . C8 C -0.4511(2) 0.13621(19) 0.01258(19) 0.0235(5) Uani 1 1 d . . . C9 C -0.5581(2) 0.1809(2) -0.0101(2) 0.0273(5) Uani 1 1 d . . . H9 H -0.5908 0.1681 -0.0830 0.033 Uiso 1 1 calc R . . C10 C -0.6130(3) 0.2410(2) 0.0711(2) 0.0288(5) Uani 1 1 d . . . H10 H -0.6815 0.2724 0.0551 0.035 Uiso 1 1 calc R . . C5 C -0.5692(2) 0.2578(2) 0.1809(2) 0.0254(5) Uani 1 1 d . . . C4 C -0.6202(3) 0.3224(2) 0.2686(2) 0.0309(6) Uani 1 1 d . . . H4 H -0.6865 0.3576 0.2565 0.037 Uiso 1 1 calc R . . C3 C -0.5739(3) 0.3344(2) 0.3717(2) 0.0309(6) Uani 1 1 d . . . H3 H -0.6064 0.3792 0.4317 0.037 Uiso 1 1 calc R . . C2 C -0.4771(3) 0.2792(2) 0.3875(2) 0.0275(5) Uani 1 1 d . . . C6 C -0.4695(2) 0.20926(19) 0.20548(19) 0.0220(5) Uani 1 1 d . . . C7 C -0.4063(2) 0.14940(19) 0.11991(19) 0.0216(5) Uani 1 1 d . . . C1 C -0.4218(3) 0.2921(2) 0.4992(2) 0.0352(6) Uani 1 1 d . . . H1A H -0.3874 0.2265 0.4930 0.042 Uiso 1 1 calc R . . H1B H -0.4937 0.2930 0.5412 0.042 Uiso 1 1 calc R . . S1 S -0.28940(9) 0.42087(7) 0.57142(6) 0.0461(2) Uani 1 1 d . . . C18 C -0.1602(3) 0.3970(3) 0.4939(3) 0.0439(7) Uani 1 1 d . . . H18A H -0.1953 0.3837 0.4182 0.053 Uiso 1 1 calc R . . H18B H -0.0858 0.4665 0.5250 0.053 Uiso 1 1 calc R . . C17 C -0.1072(3) 0.2999(2) 0.4910(2) 0.0333(6) Uani 1 1 d . . . H17A H -0.0997 0.2975 0.5633 0.040 Uiso 1 1 calc R . . H17B H -0.1684 0.2280 0.4369 0.040 Uiso 1 1 calc R . . O1 O 0.0215(2) 0.31377(18) 0.46204(16) 0.0438(5) Uani 1 1 d . . . C16 C 0.0338(3) 0.2273(2) 0.3655(2) 0.0335(6) Uani 1 1 d . . . H16A H -0.0272 0.1548 0.3546 0.040 Uiso 1 1 calc R . . H16B H 0.1256 0.2194 0.3729 0.040 Uiso 1 1 calc R . . C15 C 0.0018(3) 0.2519(2) 0.2664(2) 0.0290(6) Uani 1 1 d . . . H15A H 0.0581 0.3271 0.2797 0.035 Uiso 1 1 calc R . . H15B H -0.0921 0.2539 0.2556 0.035 Uiso 1 1 calc R . . S2 S 0.02956(6) 0.14671(6) 0.14483(5) 0.03006(18) Uani 1 1 d . . . C14 C -0.1205(2) 0.0319(2) 0.1076(2) 0.0270(5) Uani 1 1 d . . . H14A H -0.1106 -0.0367 0.0485 0.032 Uiso 1 1 calc R . . H14B H -0.1330 0.0145 0.1713 0.032 Uiso 1 1 calc R . . N2' N 0.0434(2) 0.42837(18) -0.24510(17) 0.0272(5) Uani 1 1 d . . . N1' N -0.1929(2) 0.27694(18) -0.27411(16) 0.0258(4) Uani 1 1 d . . . C2' C -0.3111(2) 0.2050(2) -0.2914(2) 0.0263(5) Uani 1 1 d . A . C3' C -0.4070(3) 0.2333(2) -0.2285(2) 0.0312(6) Uani 1 1 d . . . H3A H -0.4897 0.1800 -0.2430 0.037 Uiso 1 1 calc R . . C4' C -0.3798(3) 0.3383(2) -0.1463(2) 0.0318(6) Uani 1 1 d . . . H4A H -0.4433 0.3585 -0.1024 0.038 Uiso 1 1 calc R . . C5' C -0.2570(3) 0.4170(2) -0.1264(2) 0.0285(5) Uani 1 1 d . . . C10' C -0.2237(3) 0.5282(2) -0.0418(2) 0.0342(6) Uani 1 1 d . . . H10A H -0.2858 0.5511 0.0027 0.041 Uiso 1 1 calc R . . C9' C -0.1045(3) 0.6016(2) -0.0239(2) 0.0351(6) Uani 1 1 d . . . H9A H -0.0836 0.6751 0.0334 0.042 Uiso 1 1 calc R . . C8' C -0.0100(3) 0.5698(2) -0.0903(2) 0.0305(6) Uani 1 1 d . . . C11' C 0.1169(3) 0.6421(2) -0.0722(2) 0.0354(6) Uani 1 1 d . . . H11A H 0.1429 0.7149 -0.0135 0.043 Uiso 1 1 calc R . . C12' C 0.2016(3) 0.6070(2) -0.1392(2) 0.0359(6) Uani 1 1 d . . . H12A H 0.2881 0.6544 -0.1265 0.043 Uiso 1 1 calc R . . C13' C 0.1610(3) 0.5010(2) -0.2268(2) 0.0304(6) Uani 1 1 d . . . C7' C -0.0399(2) 0.4612(2) -0.1765(2) 0.0254(5) Uani 1 1 d . . . C6' C -0.1672(2) 0.3815(2) -0.19357(19) 0.0244(5) Uani 1 1 d . . . C14' C 0.2483(3) 0.4644(2) -0.3071(2) 0.0341(6) Uani 1 1 d . A . H14C H 0.3045 0.5322 -0.3101 0.041 Uiso 1 1 calc R . . H14D H 0.1915 0.4176 -0.3801 0.041 Uiso 1 1 calc R . . S2' S 0.35560(7) 0.38444(7) -0.27691(7) 0.0430(2) Uani 1 1 d D . . C15' C 0.2446(4) 0.2412(4) -0.3427(3) 0.0435(11) Uani 0.860(8) 1 d PD A 1 H15C H 0.1779 0.2366 -0.4024 0.052 Uiso 0.860(8) 1 calc PR A 1 H15D H 0.2969 0.1872 -0.3752 0.052 Uiso 0.860(8) 1 calc PR A 1 C16' C 0.1739(4) 0.2077(3) -0.2643(3) 0.0443(12) Uani 0.860(8) 1 d PD A 1 H16C H 0.2384 0.2254 -0.1976 0.053 Uiso 0.860(8) 1 calc PR A 1 H16D H 0.1070 0.2506 -0.2431 0.053 Uiso 0.860(8) 1 calc PR A 1 C15" C 0.2559(15) 0.2823(12) -0.2461(13) 0.023(5) Uani 0.140(8) 1 d PD A 2 H15E H 0.3119 0.2596 -0.1996 0.027 Uiso 0.140(8) 1 calc PR A 2 H15F H 0.1905 0.3145 -0.2051 0.027 Uiso 0.140(8) 1 calc PR A 2 C16" C 0.181(3) 0.1762(18) -0.3532(17) 0.053(8) Uani 0.140(8) 1 d PD A 2 H16E H 0.1163 0.1954 -0.3964 0.063 Uiso 0.140(8) 1 calc PR A 2 H16F H 0.2447 0.1467 -0.3983 0.063 Uiso 0.140(8) 1 calc PR A 2 O1' O 0.1096(2) 0.08857(18) -0.3156(2) 0.0511(6) Uani 1 1 d D . . C17' C -0.0296(3) 0.0583(3) -0.3622(3) 0.0464(8) Uani 1 1 d . A . H17C H -0.053(4) -0.024(3) -0.425(3) 0.056 Uiso 1 1 d . . . H17D H -0.052(4) 0.110(3) -0.393(3) 0.056 Uiso 1 1 d . . . C18' C -0.1123(3) 0.0542(2) -0.2786(2) 0.0379(6) Uani 1 1 d . . . H18C H -0.1015 0.1321 -0.2240 0.045 Uiso 1 1 calc R A . H18D H -0.0794 0.0117 -0.2404 0.045 Uiso 1 1 calc R . . S1' S -0.28630(7) -0.01133(6) -0.33768(6) 0.0360(2) Uani 1 1 d . A . C1' C -0.3375(3) 0.0904(2) -0.3821(2) 0.0321(6) Uani 1 1 d . . . H1C H -0.2896 0.0963 -0.4396 0.039 Uiso 1 1 calc R A . H1D H -0.4337 0.0621 -0.4142 0.039 Uiso 1 1 calc R . . O1W O -0.3406(2) 0.01097(19) 0.32575(19) 0.0436(5) Uani 1 1 d D . . H1W1 H -0.342(3) 0.059(3) 0.299(3) 0.065 Uiso 1 1 d D . . H1W2 H -0.264(2) -0.003(3) 0.325(3) 0.065 Uiso 1 1 d 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 N1 0.0260(10) 0.0247(10) 0.0238(10) 0.0087(8) 0.0100(8) 0.0108(8) N2 0.0220(10) 0.0196(10) 0.0215(10) 0.0059(8) 0.0066(8) 0.0057(8) C13 0.0222(11) 0.0186(11) 0.0234(12) 0.0043(9) 0.0072(9) 0.0038(9) C12 0.0284(13) 0.0230(12) 0.0213(12) 0.0059(10) 0.0108(10) 0.0060(10) C11 0.0272(12) 0.0232(12) 0.0225(12) 0.0092(10) 0.0064(10) 0.0027(10) C8 0.0240(12) 0.0196(11) 0.0251(12) 0.0091(10) 0.0048(10) 0.0023(9) C9 0.0288(13) 0.0254(12) 0.0274(13) 0.0123(10) 0.0029(10) 0.0052(10) C10 0.0263(12) 0.0298(13) 0.0328(13) 0.0154(11) 0.0018(10) 0.0103(10) C5 0.0220(12) 0.0201(11) 0.0315(13) 0.0086(10) 0.0060(10) 0.0045(9) C4 0.0251(12) 0.0288(13) 0.0396(15) 0.0111(12) 0.0086(11) 0.0140(10) C3 0.0312(13) 0.0326(14) 0.0316(14) 0.0091(11) 0.0147(11) 0.0182(11) C2 0.0296(13) 0.0290(13) 0.0269(13) 0.0105(11) 0.0133(10) 0.0129(10) C6 0.0216(11) 0.0203(11) 0.0247(12) 0.0089(10) 0.0065(9) 0.0068(9) C7 0.0211(11) 0.0177(11) 0.0241(12) 0.0077(9) 0.0051(9) 0.0029(9) C1 0.0448(16) 0.0433(16) 0.0294(14) 0.0167(12) 0.0212(12) 0.0268(13) S1 0.0585(5) 0.0383(4) 0.0332(4) -0.0002(3) -0.0003(3) 0.0299(4) C18 0.0461(17) 0.0342(15) 0.0483(18) 0.0186(14) 0.0008(14) 0.0052(13) C17 0.0374(15) 0.0314(14) 0.0278(13) 0.0078(11) 0.0130(11) 0.0083(11) O1 0.0395(11) 0.0437(12) 0.0272(10) -0.0027(9) 0.0120(9) -0.0006(9) C16 0.0320(14) 0.0393(15) 0.0262(13) 0.0084(12) 0.0085(11) 0.0121(12) C15 0.0301(13) 0.0260(12) 0.0253(13) 0.0033(10) 0.0076(10) 0.0093(10) S2 0.0254(3) 0.0342(4) 0.0262(3) 0.0056(3) 0.0106(3) 0.0100(3) C14 0.0311(13) 0.0271(13) 0.0227(12) 0.0053(10) 0.0098(10) 0.0158(10) N2' 0.0250(11) 0.0277(11) 0.0298(11) 0.0145(9) 0.0032(9) 0.0052(9) N1' 0.0259(10) 0.0279(11) 0.0231(10) 0.0112(9) 0.0039(8) 0.0056(9) C2' 0.0247(12) 0.0292(13) 0.0264(12) 0.0147(11) 0.0031(10) 0.0049(10) C3' 0.0264(13) 0.0382(15) 0.0348(14) 0.0214(12) 0.0065(11) 0.0080(11) C4' 0.0284(13) 0.0404(15) 0.0358(14) 0.0213(12) 0.0127(11) 0.0144(11) C5' 0.0326(13) 0.0322(13) 0.0281(13) 0.0172(11) 0.0071(11) 0.0145(11) C10' 0.0425(16) 0.0337(14) 0.0324(14) 0.0135(12) 0.0117(12) 0.0210(12) C9' 0.0475(17) 0.0251(13) 0.0309(14) 0.0078(11) 0.0050(12) 0.0148(12) C8' 0.0377(14) 0.0253(13) 0.0290(13) 0.0126(11) 0.0014(11) 0.0096(11) C11' 0.0414(15) 0.0211(12) 0.0376(15) 0.0114(11) -0.0032(12) 0.0023(11) C12' 0.0340(14) 0.0283(14) 0.0428(16) 0.0185(12) -0.0003(12) -0.0001(11) C13' 0.0279(13) 0.0303(13) 0.0376(14) 0.0216(12) 0.0016(11) 0.0046(11) C7' 0.0275(12) 0.0228(12) 0.0264(12) 0.0127(10) 0.0010(10) 0.0052(10) C6' 0.0282(13) 0.0235(12) 0.0238(12) 0.0118(10) 0.0036(10) 0.0088(10) C14' 0.0287(13) 0.0363(15) 0.0399(15) 0.0212(13) 0.0050(11) 0.0042(11) S2' 0.0307(4) 0.0483(5) 0.0597(5) 0.0297(4) 0.0143(3) 0.0139(3) C15' 0.051(2) 0.045(2) 0.042(2) 0.0200(19) 0.0172(18) 0.0183(19) C16' 0.049(2) 0.044(2) 0.050(2) 0.0223(19) 0.0212(18) 0.024(2) C15" 0.014(8) 0.011(9) 0.035(11) 0.006(7) 0.008(7) -0.007(7) C16" 0.063(18) 0.039(16) 0.059(18) 0.015(13) 0.020(13) 0.025(14) O1' 0.0381(12) 0.0370(12) 0.0870(18) 0.0295(12) 0.0197(12) 0.0175(9) C17' 0.0473(18) 0.0467(18) 0.058(2) 0.0279(17) 0.0227(16) 0.0209(15) C18' 0.0419(16) 0.0356(15) 0.0406(16) 0.0165(13) 0.0129(13) 0.0165(13) S1' 0.0428(4) 0.0268(3) 0.0369(4) 0.0112(3) 0.0137(3) 0.0077(3) C1' 0.0330(14) 0.0332(14) 0.0268(13) 0.0118(11) 0.0034(11) 0.0043(11) O1W 0.0418(12) 0.0421(12) 0.0561(13) 0.0300(11) 0.0129(10) 0.0097(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C2 1.318(3) . ? N1 C6 1.367(3) . ? N2 C13 1.324(3) . ? N2 C7 1.359(3) . ? C13 C12 1.416(3) . ? C13 C14 1.502(3) . ? C12 C11 1.366(4) . ? C11 C8 1.409(3) . ? C8 C7 1.417(3) . ? C8 C9 1.434(4) . ? C9 C10 1.351(4) . ? C10 C5 1.431(4) . ? C5 C4 1.404(4) . ? C5 C6 1.413(3) . ? C4 C3 1.371(4) . ? C3 C2 1.415(4) . ? C2 C1 1.499(4) . ? C6 C7 1.444(3) . ? C1 S1 1.813(3) . ? S1 C18 1.804(4) . ? C18 C17 1.499(4) . ? C17 O1 1.441(3) . ? O1 C16 1.412(3) . ? C16 C15 1.526(4) . ? C15 S2 1.804(3) . ? S2 C14 1.825(3) . ? N2' C13' 1.336(3) . ? N2' C7' 1.353(3) . ? N1' C2' 1.338(3) . ? N1' C6' 1.349(3) . ? C2' C3' 1.403(4) . ? C2' C1' 1.494(4) . ? C3' C4' 1.360(4) . ? C4' C5' 1.411(4) . ? C5' C6' 1.404(4) . ? C5' C10' 1.424(4) . ? C10' C9' 1.354(4) . ? C9' C8' 1.427(4) . ? C8' C11' 1.410(4) . ? C8' C7' 1.412(4) . ? C11' C12' 1.358(4) . ? C12' C13' 1.394(4) . ? C13' C14' 1.498(4) . ? C7' C6' 1.459(3) . ? C14' S2' 1.818(3) . ? S2' C15" 1.750(12) . ? S2' C15' 1.833(5) . ? C15' C16' 1.508(6) . ? C16' O1' 1.439(4) . ? C15" C16" 1.57(3) . ? C16" O1' 1.536(18) . ? O1' C17' 1.441(4) . ? C17' C18' 1.508(4) . ? C18' S1' 1.803(3) . ? S1' C1' 1.830(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 N1 C6 117.7(2) . . ? C13 N2 C7 117.8(2) . . ? N2 C13 C12 123.0(2) . . ? N2 C13 C14 115.5(2) . . ? C12 C13 C14 121.5(2) . . ? C11 C12 C13 119.2(2) . . ? C12 C11 C8 119.7(2) . . ? C11 C8 C7 116.9(2) . . ? C11 C8 C9 122.9(2) . . ? C7 C8 C9 120.3(2) . . ? C10 C9 C8 120.6(2) . . ? C9 C10 C5 120.8(2) . . ? C4 C5 C6 116.9(2) . . ? C4 C5 C10 123.0(2) . . ? C6 C5 C10 120.2(2) . . ? C3 C4 C5 119.8(2) . . ? C4 C3 C2 119.2(2) . . ? N1 C2 C3 123.0(2) . . ? N1 C2 C1 116.0(2) . . ? C3 C2 C1 120.9(2) . . ? N1 C6 C5 123.4(2) . . ? N1 C6 C7 117.4(2) . . ? C5 C6 C7 119.2(2) . . ? N2 C7 C8 123.4(2) . . ? N2 C7 C6 117.8(2) . . ? C8 C7 C6 118.8(2) . . ? C2 C1 S1 111.6(2) . . ? C18 S1 C1 103.28(14) . . ? C17 C18 S1 114.9(2) . . ? O1 C17 C18 108.9(2) . . ? C16 O1 C17 116.1(2) . . ? O1 C16 C15 111.7(2) . . ? C16 C15 S2 111.62(18) . . ? C15 S2 C14 101.60(12) . . ? C13 C14 S2 111.01(17) . . ? C13' N2' C7' 117.9(2) . . ? C2' N1' C6' 117.9(2) . . ? N1' C2' C3' 122.8(2) . . ? N1' C2' C1' 116.7(2) . . ? C3' C2' C1' 120.4(2) . . ? C4' C3' C2' 119.0(2) . . ? C3' C4' C5' 119.9(2) . . ? C6' C5' C4' 117.2(2) . . ? C6' C5' C10' 120.6(2) . . ? C4' C5' C10' 122.2(2) . . ? C9' C10' C5' 120.8(3) . . ? C10' C9' C8' 120.7(2) . . ? C11' C8' C7' 117.0(3) . . ? C11' C8' C9' 122.6(3) . . ? C7' C8' C9' 120.3(2) . . ? C12' C11' C8' 119.6(3) . . ? C11' C12' C13' 119.6(3) . . ? N2' C13' C12' 122.8(3) . . ? N2' C13' C14' 116.6(2) . . ? C12' C13' C14' 120.6(2) . . ? N2' C7' C8' 122.8(2) . . ? N2' C7' C6' 118.5(2) . . ? C8' C7' C6' 118.6(2) . . ? N1' C6' C5' 123.1(2) . . ? N1' C6' C7' 118.0(2) . . ? C5' C6' C7' 118.8(2) . . ? C13' C14' S2' 114.66(19) . . ? C15" S2' C14' 106.6(6) . . ? C15" S2' C15' 38.8(5) . . ? C14' S2' C15' 100.73(16) . . ? C16' C15' S2' 112.4(3) . . ? O1' C16' C15' 109.2(3) . . ? C16" C15" S2' 110.4(12) . . ? O1' C16" C15" 105.5(13) . . ? C16' O1' C17' 115.6(2) . . ? C16' O1' C16" 44.6(8) . . ? C17' O1' C16" 107.2(11) . . ? O1' C17' C18' 110.5(3) . . ? C17' C18' S1' 112.8(2) . . ? C18' S1' C1' 103.28(13) . . ? C2' C1' S1' 112.90(18) . . ? 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 C7 N2 C13 C12 -2.9(3) . . . . ? C7 N2 C13 C14 174.8(2) . . . . ? N2 C13 C12 C11 0.8(4) . . . . ? C14 C13 C12 C11 -176.7(2) . . . . ? C13 C12 C11 C8 2.0(4) . . . . ? C12 C11 C8 C7 -2.4(3) . . . . ? C12 C11 C8 C9 176.4(2) . . . . ? C11 C8 C9 C10 -175.4(2) . . . . ? C7 C8 C9 C10 3.4(4) . . . . ? C8 C9 C10 C5 -2.4(4) . . . . ? C9 C10 C5 C4 178.0(2) . . . . ? C9 C10 C5 C6 -1.5(4) . . . . ? C6 C5 C4 C3 -0.8(4) . . . . ? C10 C5 C4 C3 179.7(2) . . . . ? C5 C4 C3 C2 -1.3(4) . . . . ? C6 N1 C2 C3 -0.3(4) . . . . ? C6 N1 C2 C1 -177.2(2) . . . . ? C4 C3 C2 N1 2.0(4) . . . . ? C4 C3 C2 C1 178.7(3) . . . . ? C2 N1 C6 C5 -2.1(4) . . . . ? C2 N1 C6 C7 175.8(2) . . . . ? C4 C5 C6 N1 2.6(4) . . . . ? C10 C5 C6 N1 -177.8(2) . . . . ? C4 C5 C6 C7 -175.3(2) . . . . ? C10 C5 C6 C7 4.3(3) . . . . ? C13 N2 C7 C8 2.4(3) . . . . ? C13 N2 C7 C6 -175.7(2) . . . . ? C11 C8 C7 N2 0.3(3) . . . . ? C9 C8 C7 N2 -178.6(2) . . . . ? C11 C8 C7 C6 178.3(2) . . . . ? C9 C8 C7 C6 -0.6(3) . . . . ? N1 C6 C7 N2 -3.1(3) . . . . ? C5 C6 C7 N2 174.9(2) . . . . ? N1 C6 C7 C8 178.8(2) . . . . ? C5 C6 C7 C8 -3.2(3) . . . . ? N1 C2 C1 S1 94.3(2) . . . . ? C3 C2 C1 S1 -82.6(3) . . . . ? C2 C1 S1 C18 -66.1(2) . . . . ? C1 S1 C18 C17 -62.5(2) . . . . ? S1 C18 C17 O1 -159.86(19) . . . . ? C18 C17 O1 C16 -119.3(3) . . . . ? C17 O1 C16 C15 90.5(3) . . . . ? O1 C16 C15 S2 175.67(18) . . . . ? C16 C15 S2 C14 79.6(2) . . . . ? N2 C13 C14 S2 -91.1(2) . . . . ? C12 C13 C14 S2 86.6(2) . . . . ? C15 S2 C14 C13 68.71(19) . . . . ? C6' N1' C2' C3' -1.2(4) . . . . ? C6' N1' C2' C1' 179.2(2) . . . . ? N1' C2' C3' C4' 0.2(4) . . . . ? C1' C2' C3' C4' 179.8(2) . . . . ? C2' C3' C4' C5' 0.6(4) . . . . ? C3' C4' C5' C6' -0.5(4) . . . . ? C3' C4' C5' C10' 179.7(2) . . . . ? C6' C5' C10' C9' -0.4(4) . . . . ? C4' C5' C10' C9' 179.4(3) . . . . ? C5' C10' C9' C8' 0.7(4) . . . . ? C10' C9' C8' C11' -177.7(3) . . . . ? C10' C9' C8' C7' 0.5(4) . . . . ? C7' C8' C11' C12' 2.4(4) . . . . ? C9' C8' C11' C12' -179.3(3) . . . . ? C8' C11' C12' C13' 1.6(4) . . . . ? C7' N2' C13' C12' 1.5(4) . . . . ? C7' N2' C13' C14' -177.3(2) . . . . ? C11' C12' C13' N2' -3.8(4) . . . . ? C11' C12' C13' C14' 174.9(3) . . . . ? C13' N2' C7' C8' 2.9(4) . . . . ? C13' N2' C7' C6' -178.3(2) . . . . ? C11' C8' C7' N2' -4.8(4) . . . . ? C9' C8' C7' N2' 176.8(2) . . . . ? C11' C8' C7' C6' 176.3(2) . . . . ? C9' C8' C7' C6' -2.0(4) . . . . ? C2' N1' C6' C5' 1.4(3) . . . . ? C2' N1' C6' C7' -178.3(2) . . . . ? C4' C5' C6' N1' -0.6(4) . . . . ? C10' C5' C6' N1' 179.3(2) . . . . ? C4' C5' C6' C7' 179.1(2) . . . . ? C10' C5' C6' C7' -1.1(4) . . . . ? N2' C7' C6' N1' 3.0(3) . . . . ? C8' C7' C6' N1' -178.0(2) . . . . ? N2' C7' C6' C5' -176.6(2) . . . . ? C8' C7' C6' C5' 2.3(3) . . . . ? N2' C13' C14' S2' -87.8(3) . . . . ? C12' C13' C14' S2' 93.4(3) . . . . ? C13' C14' S2' C15" 46.9(6) . . . . ? C13' C14' S2' C15' 86.5(2) . . . . ? C15" S2' C15' C16' 7.6(9) . . . . ? C14' S2' C15' C16' -95.5(3) . . . . ? S2' C15' C16' O1' -168.8(2) . . . . ? C14' S2' C15" C16" 83.7(14) . . . . ? C15' S2' C15" C16" -2.9(11) . . . . ? S2' C15" C16" O1' 174.1(11) . . . . ? C15' C16' O1' C17' -97.8(3) . . . . ? C15' C16' O1' C16" -8.9(15) . . . . ? C15" C16" O1' C16' 13.9(8) . . . . ? C15" C16" O1' C17' 123.1(14) . . . . ? C16' O1' C17' C18' -88.7(3) . . . . ? C16" O1' C17' C18' -136.0(8) . . . . ? O1' C17' C18' S1' -167.8(2) . . . . ? C17' C18' S1' C1' -68.8(2) . . . . ? N1' C2' C1' S1' 90.2(2) . . . . ? C3' C2' C1' S1' -89.4(3) . . . . ? C18' S1' C1' C2' -57.2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.14 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.47 _refine_diff_density_min -0.60 _refine_diff_density_rms 0.07 #===END data_Ni(L)Cl(BF4) _database_code_CSD 156509 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H18 N2 Ni O S2 2+, Cl -, (B F4-)' _chemical_formula_sum 'C18 H18 B Cl F4 N2 Ni O S2' _chemical_formula_weight 523.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.730(2) _cell_length_b 13.853(3) _cell_length_c 10.593(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.97(2) _cell_angle_gamma 90.00 _cell_volume 1971.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 31 _cell_measurement_theta_min 12.5 _cell_measurement_theta_max 16.5 _exptl_crystal_description column _exptl_crystal_colour blue _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.764 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 1.383 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.797 _exptl_absorpt_correction_T_max 0.922 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Stoe Stadi-4' _diffrn_measurement_method omega/theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 60 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 3492 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI 0.044 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 25.04 _reflns_number_total 3492 _reflns_number_gt 2774 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe STADI-4 (Stoe, 1997a)' _computing_cell_refinement STADI-4 _computing_data_reduction 'Stoe X-RED (Stoe, 1997b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL version 5.03 (Siemens, 1994)' _computing_publication_material 'SHELXL-97; PLATON (Spek, 2001)' _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^)+(0.0376P)^2^+7.5239P] 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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3492 _refine_ls_number_parameters 271 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0678 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1180 _refine_ls_wR_factor_gt 0.1042 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.83018(4) 0.56432(4) 0.09865(5) 0.01727(17) Uani 1 1 d . . . Cl1 Cl 0.89286(9) 0.72143(9) 0.11049(12) 0.0284(3) Uani 1 1 d . . . S2 S 0.94296(8) 0.52810(9) 0.30613(11) 0.0217(3) Uani 1 1 d . . . S1 S 0.88921(8) 0.52284(9) -0.09615(11) 0.0245(3) Uani 1 1 d . . . O1 O 0.8075(2) 0.4102(2) 0.1024(3) 0.0231(7) Uani 1 1 d . . . N2 N 0.7361(3) 0.5921(3) 0.2175(3) 0.0182(8) Uani 1 1 d . . . N1 N 0.7021(3) 0.5865(3) -0.0347(4) 0.0197(8) Uani 1 1 d . . . C13 C 0.7608(3) 0.6021(3) 0.3444(4) 0.0201(10) Uani 1 1 d . . . C12 C 0.6891(3) 0.6284(4) 0.4156(5) 0.0261(11) Uani 1 1 d . . . H12 H 0.7084 0.6380 0.5061 0.031 Uiso 1 1 calc R . . C11 C 0.5915(4) 0.6404(4) 0.3551(5) 0.0249(11) Uani 1 1 d . . . H11 H 0.5425 0.6548 0.4038 0.030 Uiso 1 1 calc R . . C8 C 0.5643(3) 0.6310(3) 0.2186(4) 0.0213(10) Uani 1 1 d . . . C9 C 0.4663(3) 0.6457(3) 0.1426(5) 0.0252(11) Uani 1 1 d . . . H9 H 0.4132 0.6603 0.1844 0.030 Uiso 1 1 calc R . . C10 C 0.4479(3) 0.6392(4) 0.0114(5) 0.0264(11) Uani 1 1 d . . . H10 H 0.3821 0.6485 -0.0367 0.032 Uiso 1 1 calc R . . C5 C 0.5265(3) 0.6186(3) -0.0553(5) 0.0216(10) Uani 1 1 d . . . C4 C 0.5158(4) 0.6129(4) -0.1910(5) 0.0289(11) Uani 1 1 d . . . H4 H 0.4521 0.6208 -0.2456 0.035 Uiso 1 1 calc R . . C3 C 0.5966(4) 0.5960(4) -0.2431(5) 0.0254(11) Uani 1 1 d . . . H3 H 0.5892 0.5917 -0.3341 0.031 Uiso 1 1 calc R . . C2 C 0.6922(3) 0.5850(4) -0.1618(4) 0.0237(10) Uani 1 1 d . . . C6 C 0.6218(3) 0.6034(3) 0.0187(4) 0.0197(10) Uani 1 1 d . . . C7 C 0.6404(3) 0.6084(3) 0.1556(4) 0.0193(10) Uani 1 1 d . . . C1 C 0.7863(4) 0.5743(4) -0.2122(5) 0.0276(11) Uani 1 1 d . . . H1B H 0.8064 0.6386 -0.2387 0.033 Uiso 1 1 calc R . . H1A H 0.7725 0.5328 -0.2899 0.033 Uiso 1 1 calc R . . C17 C 0.8526(4) 0.3959(4) -0.1016(5) 0.0340(12) Uani 1 1 d . . . H17B H 0.7822 0.3899 -0.1470 0.041 Uiso 1 1 calc R . . H17A H 0.8938 0.3590 -0.1511 0.041 Uiso 1 1 calc R . . C18 C 0.8649(4) 0.3528(4) 0.0333(5) 0.0341(13) Uani 1 1 d . . . H18B H 0.8411 0.2851 0.0280 0.041 Uiso 1 1 calc R . . H18A H 0.9359 0.3535 0.0775 0.041 Uiso 1 1 calc R . . C16 C 0.8139(4) 0.3748(4) 0.2348(5) 0.0338(12) Uani 1 1 d . . . H16B H 0.8072 0.3036 0.2334 0.041 Uiso 1 1 calc R . . H16A H 0.7583 0.4021 0.2697 0.041 Uiso 1 1 calc R . . C15 C 0.9103(4) 0.4022(4) 0.3205(5) 0.0317(12) Uani 1 1 d . . . H15B H 0.9639 0.3612 0.2995 0.038 Uiso 1 1 calc R . . H15A H 0.9064 0.3889 0.4112 0.038 Uiso 1 1 calc R . . C14 C 0.8690(3) 0.5874(4) 0.4070(4) 0.0247(11) Uani 1 1 d . . . H14B H 0.8726 0.5485 0.4863 0.030 Uiso 1 1 calc R . . H14A H 0.8990 0.6511 0.4333 0.030 Uiso 1 1 calc R . . B B 0.3116(3) 0.8700(3) -0.0349(4) 0.0279(13) Uani 1 1 d D . . F1 F 0.3175(2) 0.8137(2) -0.1403(3) 0.0429(8) Uani 1 1 d D . . F2 F 0.2233(3) 0.9219(3) -0.0605(4) 0.0595(11) Uani 1 1 d D . . F3 F 0.3114(3) 0.8123(3) 0.0708(3) 0.0489(9) Uani 1 1 d D . . F4 F 0.3922(3) 0.9309(3) -0.0091(5) 0.0839(15) Uani 1 1 d 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 Ni1 0.0144(3) 0.0212(3) 0.0150(3) 0.0001(2) 0.0002(2) 0.0000(2) Cl1 0.0315(6) 0.0224(6) 0.0301(6) 0.0030(5) 0.0032(5) -0.0038(5) S2 0.0164(5) 0.0278(6) 0.0188(6) 0.0015(5) -0.0009(4) 0.0021(5) S1 0.0192(6) 0.0340(7) 0.0200(6) -0.0045(5) 0.0036(5) -0.0021(5) O1 0.0182(16) 0.0271(18) 0.0236(17) -0.0009(14) 0.0035(13) -0.0024(13) N2 0.0149(18) 0.020(2) 0.0181(19) 0.0004(16) 0.0009(15) 0.0022(15) N1 0.0190(19) 0.021(2) 0.018(2) 0.0005(16) 0.0024(15) -0.0005(16) C13 0.020(2) 0.022(2) 0.018(2) 0.0007(19) 0.0036(18) 0.0012(19) C12 0.026(3) 0.035(3) 0.019(2) 0.001(2) 0.007(2) 0.001(2) C11 0.025(2) 0.026(3) 0.027(3) 0.001(2) 0.014(2) 0.000(2) C8 0.022(2) 0.020(2) 0.022(2) 0.004(2) 0.0060(19) 0.0028(19) C9 0.016(2) 0.022(3) 0.038(3) 0.000(2) 0.006(2) 0.0034(19) C10 0.016(2) 0.027(3) 0.030(3) 0.001(2) -0.009(2) 0.003(2) C5 0.017(2) 0.019(2) 0.025(3) 0.002(2) -0.0026(19) 0.0011(19) C4 0.023(2) 0.029(3) 0.028(3) 0.004(2) -0.010(2) 0.000(2) C3 0.029(3) 0.027(3) 0.016(2) 0.005(2) -0.003(2) 0.001(2) C2 0.026(2) 0.026(3) 0.015(2) -0.002(2) -0.0030(19) -0.001(2) C6 0.019(2) 0.018(2) 0.021(2) 0.0019(19) 0.0015(18) 0.0010(18) C7 0.018(2) 0.018(2) 0.021(2) 0.0021(19) 0.0023(18) -0.0032(18) C1 0.027(3) 0.035(3) 0.020(2) -0.001(2) 0.002(2) 0.000(2) C17 0.038(3) 0.033(3) 0.026(3) -0.008(2) -0.004(2) 0.007(2) C18 0.032(3) 0.031(3) 0.041(3) -0.013(2) 0.010(2) -0.004(2) C16 0.039(3) 0.031(3) 0.032(3) 0.004(2) 0.007(2) 0.001(2) C15 0.041(3) 0.026(3) 0.029(3) 0.003(2) 0.008(2) 0.006(2) C14 0.026(2) 0.032(3) 0.016(2) -0.003(2) 0.0023(19) 0.003(2) B 0.025(3) 0.027(3) 0.032(3) -0.003(3) 0.007(2) 0.001(2) F1 0.053(2) 0.049(2) 0.0263(16) -0.0076(15) 0.0071(14) 0.0055(16) F2 0.057(2) 0.070(3) 0.057(2) 0.030(2) 0.0243(18) 0.039(2) F3 0.055(2) 0.064(2) 0.0289(18) 0.0151(16) 0.0116(15) 0.0249(18) F4 0.067(3) 0.072(3) 0.122(4) -0.043(3) 0.040(3) -0.041(2) _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 Ni1 N2 2.019(4) . ? Ni1 N1 2.038(4) . ? Ni1 O1 2.159(3) . ? Ni1 Cl1 2.3342(14) . ? Ni1 S1 2.4371(13) . ? Ni1 S2 2.4633(13) . ? S2 C15 1.815(5) . ? S2 C14 1.816(5) . ? S1 C1 1.815(5) . ? S1 C17 1.827(6) . ? O1 C18 1.424(6) . ? O1 C16 1.471(6) . ? N2 C13 1.324(6) . ? N2 C7 1.360(6) . ? N1 C2 1.325(6) . ? N1 C6 1.360(6) . ? C13 C12 1.406(6) . ? C13 C14 1.510(6) . ? C12 C11 1.370(7) . ? C11 C8 1.422(7) . ? C8 C7 1.387(6) . ? C8 C9 1.431(6) . ? C9 C10 1.364(7) . ? C10 C5 1.435(7) . ? C5 C6 1.395(6) . ? C5 C4 1.417(7) . ? C4 C3 1.357(7) . ? C3 C2 1.421(6) . ? C2 C1 1.504(7) . ? C6 C7 1.421(6) . ? C17 C18 1.526(8) . ? C16 C15 1.490(7) . ? B F4 1.373(5) . ? B F1 1.377(5) . ? B F3 1.377(5) . ? B F2 1.388(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 N2 Ni1 N1 80.33(15) . . ? N2 Ni1 O1 93.64(13) . . ? N1 Ni1 O1 93.13(13) . . ? N2 Ni1 Cl1 93.76(11) . . ? N1 Ni1 Cl1 98.77(11) . . ? O1 Ni1 Cl1 166.90(9) . . ? N2 Ni1 S1 160.23(11) . . ? N1 Ni1 S1 80.74(11) . . ? O1 Ni1 S1 81.77(9) . . ? Cl1 Ni1 S1 94.69(5) . . ? N2 Ni1 S2 81.23(11) . . ? N1 Ni1 S2 160.33(11) . . ? O1 Ni1 S2 81.29(9) . . ? Cl1 Ni1 S2 89.17(5) . . ? S1 Ni1 S2 116.72(5) . . ? C15 S2 C14 102.0(2) . . ? C15 S2 Ni1 98.64(17) . . ? C14 S2 Ni1 96.20(15) . . ? C1 S1 C17 100.7(2) . . ? C1 S1 Ni1 97.58(16) . . ? C17 S1 Ni1 96.67(18) . . ? C18 O1 C16 111.9(4) . . ? C18 O1 Ni1 116.5(3) . . ? C16 O1 Ni1 111.5(3) . . ? C13 N2 C7 119.4(4) . . ? C13 N2 Ni1 126.2(3) . . ? C7 N2 Ni1 114.2(3) . . ? C2 N1 C6 120.3(4) . . ? C2 N1 Ni1 126.4(3) . . ? C6 N1 Ni1 113.2(3) . . ? N2 C13 C12 120.7(4) . . ? N2 C13 C14 116.9(4) . . ? C12 C13 C14 122.3(4) . . ? C11 C12 C13 120.4(4) . . ? C12 C11 C8 119.3(4) . . ? C7 C8 C11 116.4(4) . . ? C7 C8 C9 118.4(4) . . ? C11 C8 C9 125.2(4) . . ? C10 C9 C8 121.2(4) . . ? C9 C10 C5 121.0(4) . . ? C6 C5 C4 116.7(4) . . ? C6 C5 C10 117.8(4) . . ? C4 C5 C10 125.5(4) . . ? C3 C4 C5 120.1(4) . . ? C4 C3 C2 120.1(4) . . ? N1 C2 C3 120.1(4) . . ? N1 C2 C1 116.6(4) . . ? C3 C2 C1 123.3(4) . . ? N1 C6 C5 122.6(4) . . ? N1 C6 C7 116.4(4) . . ? C5 C6 C7 121.0(4) . . ? N2 C7 C8 123.7(4) . . ? N2 C7 C6 115.8(4) . . ? C8 C7 C6 120.5(4) . . ? C2 C1 S1 113.8(3) . . ? C18 C17 S1 111.8(4) . . ? O1 C18 C17 107.3(4) . . ? O1 C16 C15 111.5(4) . . ? C16 C15 S2 113.4(4) . . ? C13 C14 S2 115.0(3) . . ? F4 B F1 109.2(4) . . ? F4 B F3 109.5(4) . . ? F1 B F3 110.0(4) . . ? F4 B F2 110.8(4) . . ? F1 B F2 109.3(4) . . ? F3 B F2 108.1(4) . . ? 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 C7 N2 C13 C12 0.7(7) . . . . ? C7 N2 C13 C14 -177.4(4) . . . . ? N2 C13 C12 C11 2.5(7) . . . . ? C14 C13 C12 C11 -179.5(5) . . . . ? C13 C12 C11 C8 -3.4(7) . . . . ? C12 C11 C8 C7 1.0(7) . . . . ? C12 C11 C8 C9 -177.1(5) . . . . ? C7 C8 C9 C10 -1.0(7) . . . . ? C11 C8 C9 C10 177.1(5) . . . . ? C8 C9 C10 C5 -0.8(8) . . . . ? C9 C10 C5 C6 1.3(7) . . . . ? C9 C10 C5 C4 -178.2(5) . . . . ? C6 C5 C4 C3 -1.8(7) . . . . ? C10 C5 C4 C3 177.7(5) . . . . ? C5 C4 C3 C2 -0.6(8) . . . . ? C6 N1 C2 C3 -3.3(7) . . . . ? C6 N1 C2 C1 174.9(4) . . . . ? C4 C3 C2 N1 3.2(7) . . . . ? C4 C3 C2 C1 -174.8(5) . . . . ? C2 N1 C6 C5 0.8(7) . . . . ? C2 N1 C6 C7 -177.0(4) . . . . ? C4 C5 C6 N1 1.8(7) . . . . ? C10 C5 C6 N1 -177.8(4) . . . . ? C4 C5 C6 C7 179.5(4) . . . . ? C10 C5 C6 C7 -0.1(7) . . . . ? C13 N2 C7 C8 -3.2(7) . . . . ? C13 N2 C7 C6 175.3(4) . . . . ? C11 C8 C7 N2 2.3(7) . . . . ? C9 C8 C7 N2 -179.4(4) . . . . ? C11 C8 C7 C6 -176.1(4) . . . . ? C9 C8 C7 C6 2.2(7) . . . . ? N1 C6 C7 N2 -2.3(6) . . . . ? C5 C6 C7 N2 179.8(4) . . . . ? N1 C6 C7 C8 176.1(4) . . . . ? C5 C6 C7 C8 -1.7(7) . . . . ? N1 C2 C1 S1 21.0(6) . . . . ? C3 C2 C1 S1 -160.9(4) . . . . ? C17 S1 C1 C2 75.8(4) . . . . ? C1 S1 C17 C18 -134.4(4) . . . . ? C16 O1 C18 C17 179.9(4) . . . . ? S1 C17 C18 O1 56.7(5) . . . . ? C18 O1 C16 C15 76.8(5) . . . . ? O1 C16 C15 S2 47.3(5) . . . . ? C14 S2 C15 C16 80.8(4) . . . . ? N2 C13 C14 S2 -15.2(6) . . . . ? C12 C13 C14 S2 166.8(4) . . . . ? C15 S2 C14 C13 -79.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.93 _refine_diff_density_min -0.55 _refine_diff_density_rms 0.10 #===END data_Pd(L)(BF4)2.0.5CH3CN _database_code_CSD 156510 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Pd C18 H18 N2 S2 O 2+, 2(B F4 -), 0.5(C2 H3 N)' _chemical_formula_sum 'C19 H19.50 B2 F8 N2.50 O Pd S2' _chemical_formula_weight 643.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 13.177(4) _cell_length_b 11.520(4) _cell_length_c 15.006(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.85(3) _cell_angle_gamma 90.00 _cell_volume 2266.0(11) _cell_formula_units_Z 4 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used 43 _cell_measurement_theta_min 12.5 _cell_measurement_theta_max 18 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.885 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1276 _exptl_absorpt_coefficient_mu 1.088 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.754 _exptl_absorpt_correction_T_max 0.930 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 1997b)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 210(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 'Stoe Stadi-4' _diffrn_measurement_method omega/theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% none _diffrn_reflns_number 2128 _diffrn_reflns_av_R_equivalents 0.1281 _diffrn_reflns_av_sigmaI/netI 0.0234 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 24.98 _reflns_number_total 2093 _reflns_number_gt 1818 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe STADI-4 (Stoe, 1997a)' _computing_cell_refinement STADI-4 _computing_data_reduction 'Stoe X-RED (Stoe, 1997b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL version 5.03 (Siemens, 1994)' _computing_publication_material 'SHELXTL-97; PLATON (Spek, 2001)' _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^)+(0.0862P)^2^+57.5390P] 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 2093 _refine_ls_number_parameters 177 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0821 _refine_ls_R_factor_gt 0.0710 _refine_ls_wR_factor_ref 0.1893 _refine_ls_wR_factor_gt 0.1754 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.45895(6) 0.5000 0.26267(5) 0.0271(3) Uani 1 2 d S . . N1 N 0.4333(4) 0.6139(5) 0.1646(4) 0.0276(13) Uani 1 1 d . . . C2 C 0.4384(5) 0.7268(7) 0.1722(5) 0.0324(16) Uani 1 1 d . . . C3 C 0.4077(6) 0.7962(7) 0.0959(6) 0.0400(19) Uani 1 1 d . . . H3 H 0.4101 0.8775 0.1012 0.048 Uiso 1 1 calc R . . C4 C 0.3751(5) 0.7482(8) 0.0160(6) 0.040(2) Uani 1 1 d . . . H4 H 0.3555 0.7955 -0.0338 0.048 Uiso 1 1 calc R . . C5 C 0.3706(5) 0.6240(7) 0.0081(5) 0.0321(17) Uani 1 1 d . . . C6 C 0.4008(5) 0.5625(7) 0.0849(5) 0.0286(15) Uani 1 1 d . . . C10 C 0.3391(6) 0.5595(9) -0.0719(5) 0.041(2) Uani 1 1 d . . . H10 H 0.3181 0.5996 -0.1252 0.050 Uiso 1 1 calc R . . C1 C 0.4801(7) 0.7727(7) 0.2620(5) 0.0341(17) Uani 1 1 d . . . H1B H 0.4408 0.8412 0.2764 0.041 Uiso 1 1 calc R . . H1A H 0.5510 0.7971 0.2593 0.041 Uiso 1 1 calc R . . S1 S 0.47543(15) 0.66437(18) 0.35139(13) 0.0352(5) Uani 1 1 d . . . C18 C 0.3464(7) 0.6902(8) 0.3792(7) 0.048(2) Uani 1 1 d . . . H18B H 0.3431 0.7667 0.4074 0.058 Uiso 1 1 calc R . . H18A H 0.2996 0.6907 0.3241 0.058 Uiso 1 1 calc R . . C17 C 0.3144(10) 0.6034(13) 0.4387(9) 0.100(5) Uani 1 1 d D . . H17B H 0.3645 0.5976 0.4915 0.120 Uiso 1 1 calc R A 1 H17A H 0.2488 0.6259 0.4590 0.120 Uiso 1 1 calc R A 1 O1 O 0.3049(13) 0.5000 0.3977(10) 0.054(6) Uiso 0.59(3) 2 d SPD . 1 O1' O 0.3565(13) 0.5000 0.4565(12) 0.030(6) Uiso 0.41(3) 2 d SPD . 2 B1 B 0.6505(10) 1.0000 0.1595(10) 0.035(3) Uani 1 2 d S . 2 F1 F 0.6339(10) 1.0000 0.0647(6) 0.087(3) Uani 1 2 d S . 2 F2 F 0.7041(4) 0.9001(5) 0.1835(4) 0.0587(15) Uani 1 1 d . . 2 F3 F 0.5592(7) 1.0000 0.1920(8) 0.080(3) Uani 1 2 d S . 2 B2 B 0.7528(10) 0.5000 0.3111(9) 0.036(3) Uani 1 2 d S . 2 F5 F 0.8026(6) 0.5000 0.3959(5) 0.060(2) Uani 1 2 d S . 2 F6 F 0.8237(6) 0.5000 0.2499(5) 0.060(2) Uani 1 2 d S . 2 F7 F 0.6920(4) 0.5978(5) 0.2998(4) 0.0602(15) Uani 1 1 d . . 2 C1S C 0.5000 1.0000 0.5000 0.045(4) Uiso 1 4 d S . 2 N1S N 0.5281(18) 1.091(2) 0.4613(15) 0.022(5) Uiso 0.13 1 d P . 2 C2S C 0.5281(18) 1.091(2) 0.4613(15) 0.022(5) Uiso 0.13 1 d P . 2 N2S N 0.542(3) 1.0000 0.435(2) 0.073(8) Uiso 0.25 2 d SP . 2 C3S C 0.542(3) 1.0000 0.435(2) 0.073(8) Uiso 0.25 2 d SP . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0260(5) 0.0225(5) 0.0318(5) 0.000 -0.0017(3) 0.000 N1 0.017(3) 0.034(4) 0.031(3) 0.010(3) 0.001(2) 0.004(2) C2 0.023(4) 0.032(4) 0.043(4) 0.000(3) 0.006(3) -0.002(3) C3 0.031(4) 0.029(4) 0.060(5) 0.011(4) 0.006(4) 0.001(3) C4 0.021(4) 0.049(5) 0.051(5) 0.021(4) 0.008(3) 0.005(3) C5 0.023(3) 0.050(5) 0.023(3) 0.011(3) 0.005(3) 0.004(3) C6 0.021(3) 0.034(4) 0.031(4) -0.001(3) 0.004(3) -0.003(3) C10 0.027(4) 0.071(6) 0.027(4) 0.004(4) 0.003(3) 0.004(4) C1 0.053(5) 0.020(4) 0.030(4) 0.000(3) 0.009(3) -0.004(3) S1 0.0396(11) 0.0309(10) 0.0338(10) -0.0050(8) -0.0030(8) -0.0028(8) C18 0.053(5) 0.037(5) 0.057(5) -0.009(4) 0.015(4) 0.003(4) C17 0.090(10) 0.081(10) 0.141(13) 0.035(10) 0.071(10) 0.022(8) B1 0.037(7) 0.015(5) 0.055(8) 0.000 0.008(6) 0.000 F1 0.158(10) 0.047(5) 0.048(5) 0.000 -0.025(6) 0.000 F2 0.050(3) 0.058(3) 0.068(4) 0.013(3) 0.003(3) 0.023(3) F3 0.061(5) 0.040(5) 0.147(9) 0.000 0.051(6) 0.000 B2 0.028(6) 0.044(8) 0.034(6) 0.000 -0.003(5) 0.000 F5 0.064(5) 0.077(6) 0.036(4) 0.000 -0.012(4) 0.000 F6 0.045(4) 0.084(6) 0.051(4) 0.000 0.012(4) 0.000 F7 0.053(3) 0.044(3) 0.080(4) -0.004(3) -0.006(3) 0.012(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 Pd1 N1 1.975(6) 6_565 ? Pd1 N1 1.975(6) . ? Pd1 S1 2.312(2) . ? Pd1 S1 2.312(2) 6_565 ? Pd1 O1 3.011(16) . ? N1 C2 1.308(10) . ? N1 C6 1.363(9) . ? C2 C3 1.421(11) . ? C2 C1 1.498(11) . ? C3 C4 1.350(13) . ? C4 C5 1.436(13) . ? C5 C6 1.377(10) . ? C5 C10 1.437(11) . ? C6 C6 1.441(15) 6_565 ? C10 C10 1.37(2) 6_565 ? C1 S1 1.838(7) . ? S1 C18 1.816(9) . ? C18 C17 1.433(15) . ? C17 O1' 1.330(15) . ? C17 O1 1.341(15) . ? O1 C17 1.341(15) 6_565 ? O1' C17 1.330(15) 6_565 ? B1 F3 1.344(15) . ? B1 F2 1.378(9) 6_575 ? B1 F2 1.378(9) . ? B1 F1 1.417(17) . ? B2 F5 1.371(14) . ? B2 F7 1.382(9) 6_565 ? B2 F7 1.382(9) . ? B2 F6 1.376(15) . ? C1S N2S 1.17(3) . ? C1S N1S 1.27(2) . ? N1S N2S 1.14(3) . ? N1S C2S 1.44(5) 2_656 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 N1 83.2(4) 6_565 . ? N1 Pd1 S1 166.4(2) 6_565 . ? N1 Pd1 S1 83.3(2) . . ? S1 Pd1 S1 109.96(11) . 6_565 ? N1 Pd1 O1 115.2(3) 6_565 . ? N1 Pd1 O1 115.2(3) . . ? S1 Pd1 O1 69.07(16) . . ? S1 Pd1 O1 69.07(16) 6_565 . ? C2 N1 C6 121.2(6) . . ? C2 N1 Pd1 126.3(6) . . ? C6 N1 Pd1 112.3(5) . . ? N1 C2 C3 118.8(7) . . ? N1 C2 C1 116.2(7) . . ? C3 C2 C1 125.0(7) . . ? C4 C3 C2 121.6(8) . . ? C3 C4 C5 119.2(7) . . ? C6 C5 C10 117.9(8) . . ? C6 C5 C4 115.9(7) . . ? C10 C5 C4 126.2(7) . . ? N1 C6 C5 123.3(7) . . ? N1 C6 C6 115.7(4) . 6_565 ? C5 C6 C6 121.0(5) . 6_565 ? C10 C10 C5 121.1(5) 6_565 . ? C2 C1 S1 112.3(5) . . ? C18 S1 C1 99.1(4) . . ? C18 S1 Pd1 103.4(3) . . ? C1 S1 Pd1 98.3(2) . . ? C17 C18 S1 111.8(8) . . ? O1' C17 O1 46.7(10) . . ? O1' C17 C18 127.4(12) . . ? O1 C17 C18 110.7(10) . . ? C17 O1 C17 125.3(13) . 6_565 ? C17 O1 Pd1 105.8(9) . . ? C17 O1 Pd1 105.8(9) 6_565 . ? C17 O1' C17 127.3(14) 6_565 . ? F3 B1 F2 111.0(7) . 6_575 ? F3 B1 F2 111.0(7) . . ? F2 B1 F2 113.2(11) 6_575 . ? F3 B1 F1 108.1(12) . . ? F2 B1 F1 106.6(8) 6_575 . ? F2 B1 F1 106.6(8) . . ? F5 B2 F7 109.3(7) . 6_565 ? F5 B2 F7 109.3(7) . . ? F7 B2 F7 109.1(10) 6_565 . ? F5 B2 F6 109.0(10) . . ? F7 B2 F6 110.1(7) 6_565 . ? F7 B2 F6 110.1(7) . . ? C3S C1S N2S 180.000 5_676 . ? 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 C6 N1 C2 C3 1.0(11) . . . . ? C6 N1 C2 C1 -177.1(6) . . . . ? N1 C2 C3 C4 -1.0(12) . . . . ? C1 C2 C3 C4 176.9(7) . . . . ? C2 C3 C4 C5 0.5(12) . . . . ? C3 C4 C5 C6 0.0(11) . . . . ? C3 C4 C5 C10 -179.1(7) . . . . ? C2 N1 C6 C5 -0.6(10) . . . . ? C2 N1 C6 C6 178.7(5) . . . 6_565 ? C10 C5 C6 N1 179.3(6) . . . . ? C4 C5 C6 N1 0.1(10) . . . . ? C10 C5 C6 C6 0.0(8) . . . 6_565 ? C4 C5 C6 C6 -179.2(4) . . . 6_565 ? C6 C5 C10 C10 0.0(8) . . . 6_565 ? C4 C5 C10 C10 179.1(5) . . . 6_565 ? N1 C2 C1 S1 -19.1(9) . . . . ? C3 C2 C1 S1 162.9(6) . . . . ? C2 C1 S1 C18 -86.1(6) . . . . ? C1 S1 C18 C17 170.4(9) . . . . ? S1 C18 C17 O1' -16.6(17) . . . . ? S1 C18 C17 O1 -67.2(12) . . . . ? O1' C17 O1 C17 31.0(17) . . . 6_565 ? C18 C17 O1 C17 153.4(13) . . . 6_565 ? O1 C17 O1' C17 -32.2(18) . . . 6_565 ? C18 C17 O1' C17 -115.9(18) . . . 6_565 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.846 _refine_diff_density_min -1.520 _refine_diff_density_rms 0.188 #===END data_Pd(L)(BF4)2 _database_code_CSD 156511 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H18 N2 O Pd S2 2+, 2(B F4 -)' _chemical_formula_sum 'C18 H18 B2 F8 N2 O Pd S2' _chemical_formula_weight 622.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.220(2) _cell_length_b 11.025(2) _cell_length_c 11.695(2) _cell_angle_alpha 96.68(2) _cell_angle_beta 98.27(2) _cell_angle_gamma 112.04(2) _cell_volume 1071.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.0 _cell_measurement_theta_max 18.5 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.929 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 1.146 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'North, Phillips & Mathews, 1968)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Nonius CAD4 four-circle' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% none _diffrn_reflns_number 3745 _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_sigmaI/netI 0.024 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 24.97 _reflns_number_total 3745 _reflns_number_gt 3305 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe STADI-4 (Stoe, 1997a)' _computing_cell_refinement STADI-4 _computing_data_reduction 'Stoe X-RED (Stoe, 1997b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL version 5.03 (Siemens, 1994)' _computing_publication_material 'SHELXL-97; PLATON (Spek, 2001)' _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^)+(0.0676P)^2^+2.601P] 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 3745 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0530 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1219 _refine_ls_wR_factor_gt 0.1165 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.13385(4) 0.08074(4) 0.27734(3) 0.03871(15) Uani 1 1 d . . . S1 S 0.30505(17) 0.00815(15) 0.38269(14) 0.0560(4) Uani 1 1 d . . . S2 S 0.2426(2) 0.30978(14) 0.29865(13) 0.0550(4) Uani 1 1 d . . . O1 O 0.1665(4) 0.1874(4) 0.5260(3) 0.0518(9) Uani 1 1 d . . . F1A F 0.4421(6) 0.7917(4) 0.1990(4) 0.1079(15) Uani 1.10 1 d P . . F1B F 0.3252(6) 0.6292(4) 0.2966(3) 0.1006(14) Uani 1.10 1 d P . . F1D F 0.2449(6) 0.5994(4) 0.1023(4) 0.1187(18) Uani 1.10 1 d P . . F1C F 0.4783(7) 0.6009(5) 0.1792(6) 0.1281(19) Uani 1.10 1 d P . . F2B F 0.2757(9) 0.6486(7) 0.7481(6) 0.159(3) Uani 1.10 1 d P . . F2A F 0.1513(9) 0.6238(13) 0.5874(9) 0.262(6) Uani 1.10 1 d P . . F2C F 0.3984(7) 0.7165(6) 0.6004(6) 0.151(2) Uani 1.10 1 d P . . F2D F 0.2655(17) 0.8155(8) 0.6825(10) 0.313(8) Uani 1.10 1 d P . . N1 N 0.0064(5) -0.1131(4) 0.2235(4) 0.0428(9) Uani 1 1 d . . . N2 N -0.0332(5) 0.0918(5) 0.1569(4) 0.0482(10) Uani 1 1 d . . . C1 C 0.1664(8) -0.1658(6) 0.3725(6) 0.0595(15) Uani 1 1 d . . . H1A H 0.2246 -0.2229 0.3680 0.071 Uiso 1 1 calc R . . H1B H 0.1218 -0.1742 0.4428 0.071 Uiso 1 1 calc R . . C2 C 0.0348(7) -0.2099(5) 0.2678(5) 0.0499(13) Uani 1 1 d . . . C3 C -0.0625(9) -0.3421(6) 0.2178(7) 0.0671(17) Uani 1 1 d . . . H3 H -0.0430 -0.4103 0.2477 0.080 Uiso 1 1 calc R . . C4 C -0.1866(9) -0.3723(6) 0.1249(7) 0.073(2) Uani 1 1 d . . . H4 H -0.2506 -0.4609 0.0922 0.087 Uiso 1 1 calc R . . C5 C -0.2181(7) -0.2710(7) 0.0785(5) 0.0619(17) Uani 1 1 d . . . C6 C -0.1172(6) -0.1407(6) 0.1315(5) 0.0485(12) Uani 1 1 d . . . C10 C -0.3446(8) -0.2869(9) -0.0171(6) 0.082(2) Uani 1 1 d . . . H7 H -0.4136 -0.3722 -0.0561 0.098 Uiso 1 1 calc R . . C9 C -0.3652(8) -0.1828(10) -0.0509(6) 0.081(2) Uani 1 1 d . . . H8 H -0.4486 -0.1980 -0.1132 0.097 Uiso 1 1 calc R . . C8 C -0.2632(7) -0.0459(8) 0.0049(5) 0.0663(18) Uani 1 1 d . . . C7 C -0.1387(7) -0.0298(6) 0.0965(5) 0.0515(13) Uani 1 1 d . . . C11 C -0.2726(9) 0.0711(10) -0.0228(6) 0.082(2) Uani 1 1 d . . . H11 H -0.3534 0.0657 -0.0833 0.099 Uiso 1 1 calc R . . C12 C -0.1650(10) 0.1936(9) 0.0375(6) 0.076(2) Uani 1 1 d . . . H12 H -0.1725 0.2704 0.0171 0.091 Uiso 1 1 calc R . . C13 C -0.0430(8) 0.2034(7) 0.1302(5) 0.0591(15) Uani 1 1 d . . . C14 C 0.0786(9) 0.3299(7) 0.2035(6) 0.0710(19) Uani 1 1 d . . . H14A H 0.0261 0.3701 0.2524 0.085 Uiso 1 1 calc R . . H14B H 0.1237 0.3907 0.1520 0.085 Uiso 1 1 calc R . . C15 C 0.2155(11) 0.3772(7) 0.4421(6) 0.083(2) Uani 1 1 d . . . H15A H 0.2740 0.4731 0.4594 0.100 Uiso 1 1 calc R . . H15B H 0.1032 0.3583 0.4384 0.100 Uiso 1 1 calc R . . C16 C 0.2714(10) 0.3198(7) 0.5351(6) 0.079(2) Uani 1 1 d . . . H16A H 0.3771 0.3239 0.5299 0.094 Uiso 1 1 calc R . . H16B H 0.2788 0.3705 0.6109 0.094 Uiso 1 1 calc R . . C17 C 0.2348(8) 0.1063(9) 0.5853(5) 0.078(2) Uani 1 1 d . . . H17A H 0.1485 0.0225 0.5865 0.093 Uiso 1 1 calc R . . H17B H 0.2813 0.1512 0.6663 0.093 Uiso 1 1 calc R . . C18 C 0.3582(8) 0.0763(8) 0.5344(6) 0.0687(17) Uani 1 1 d . . . H18A H 0.3854 0.0145 0.5766 0.082 Uiso 1 1 calc R . . H18B H 0.4535 0.1580 0.5479 0.082 Uiso 1 1 calc R . . B1 B 0.3735(8) 0.6573(7) 0.1939(6) 0.0519(15) Uani 1 1 d . . . B2 B 0.2845(9) 0.7105(9) 0.6590(7) 0.0631(18) 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 Pd1 0.0417(2) 0.0381(2) 0.0393(2) 0.00794(15) 0.01122(15) 0.01786(16) S1 0.0457(7) 0.0570(8) 0.0718(10) 0.0109(7) 0.0072(7) 0.0297(7) S2 0.0719(9) 0.0407(7) 0.0512(8) 0.0112(6) 0.0208(7) 0.0173(7) O1 0.044(2) 0.064(2) 0.047(2) 0.0090(18) 0.0107(16) 0.0208(18) F1A 0.145(4) 0.061(2) 0.089(3) 0.014(2) -0.011(3) 0.022(2) F1B 0.157(4) 0.101(3) 0.071(2) 0.031(2) 0.049(3) 0.068(3) F1D 0.137(4) 0.084(3) 0.092(3) 0.023(2) -0.032(3) 0.014(3) F1C 0.130(4) 0.121(4) 0.176(5) 0.048(4) 0.082(4) 0.072(3) F2B 0.197(6) 0.162(6) 0.159(5) 0.099(5) 0.076(5) 0.084(5) F2A 0.112(5) 0.370(15) 0.241(10) -0.056(10) -0.032(6) 0.084(7) F2C 0.122(4) 0.149(5) 0.175(6) 0.022(4) 0.090(4) 0.028(4) F2D 0.62(2) 0.149(6) 0.376(13) 0.164(8) 0.406(16) 0.233(10) N1 0.045(2) 0.042(2) 0.041(2) 0.0050(18) 0.0150(18) 0.0156(19) N2 0.055(3) 0.059(3) 0.043(2) 0.018(2) 0.019(2) 0.030(2) C1 0.071(4) 0.054(3) 0.067(4) 0.019(3) 0.018(3) 0.036(3) C2 0.058(3) 0.041(3) 0.060(3) 0.010(2) 0.026(3) 0.024(2) C3 0.080(5) 0.042(3) 0.084(5) 0.007(3) 0.036(4) 0.024(3) C4 0.073(4) 0.045(3) 0.088(5) -0.006(3) 0.041(4) 0.007(3) C5 0.050(3) 0.069(4) 0.045(3) -0.011(3) 0.017(3) 0.004(3) C6 0.044(3) 0.058(3) 0.041(3) 0.002(2) 0.016(2) 0.017(2) C10 0.057(4) 0.097(6) 0.059(4) -0.013(4) 0.015(3) 0.002(4) C9 0.043(3) 0.132(7) 0.042(3) -0.004(4) 0.003(3) 0.015(4) C8 0.055(4) 0.116(6) 0.038(3) 0.019(3) 0.015(3) 0.043(4) C7 0.046(3) 0.068(4) 0.037(3) 0.007(3) 0.012(2) 0.019(3) C11 0.067(4) 0.154(8) 0.046(4) 0.032(5) 0.016(3) 0.060(5) C12 0.093(5) 0.122(7) 0.060(4) 0.052(4) 0.038(4) 0.076(5) C13 0.077(4) 0.072(4) 0.054(3) 0.031(3) 0.032(3) 0.045(3) C14 0.097(5) 0.059(4) 0.084(5) 0.038(4) 0.039(4) 0.046(4) C15 0.133(7) 0.062(4) 0.061(4) 0.000(3) 0.016(4) 0.051(5) C16 0.087(5) 0.071(4) 0.054(4) -0.006(3) 0.007(3) 0.014(4) C17 0.058(4) 0.150(7) 0.044(3) 0.039(4) 0.016(3) 0.053(4) C18 0.063(4) 0.088(5) 0.061(4) 0.017(3) 0.004(3) 0.038(4) B1 0.061(4) 0.049(4) 0.045(3) 0.005(3) 0.006(3) 0.023(3) B2 0.055(4) 0.077(5) 0.060(4) 0.024(4) 0.012(3) 0.027(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 Pd1 N2 1.982(4) . ? Pd1 N1 1.984(4) . ? Pd1 S1 2.2951(14) . ? Pd1 S2 2.3077(14) . ? Pd1 O1 2.935(4) . ? S1 C18 1.765(7) . ? S1 C1 1.841(6) . ? S2 C14 1.843(7) . ? S2 C15 1.844(7) . ? O1 C16 1.397(8) . ? O1 C17 1.456(8) . ? F1A B1 1.365(8) . ? F1B B1 1.369(7) . ? F1D B1 1.367(8) . ? F1C B1 1.350(8) . ? F2B B2 1.306(9) . ? F2A B2 1.327(11) . ? F2C B2 1.320(9) . ? F2D B2 1.241(10) . ? N1 C2 1.332(7) . ? N1 C6 1.364(7) . ? N2 C13 1.336(7) . ? N2 C7 1.358(7) . ? C1 C2 1.483(9) . ? C2 C3 1.393(8) . ? C3 C4 1.368(10) . ? C4 C5 1.402(10) . ? C5 C6 1.392(8) . ? C5 C10 1.437(10) . ? C6 C7 1.405(8) . ? C10 C9 1.325(12) . ? C9 C8 1.455(11) . ? C8 C7 1.394(8) . ? C8 C11 1.397(11) . ? C11 C12 1.370(11) . ? C12 C13 1.408(9) . ? C13 C14 1.486(10) . ? C15 C16 1.447(10) . ? C17 C18 1.479(9) . ? 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 N2 Pd1 N1 82.16(19) . . ? N2 Pd1 S1 163.19(14) . . ? N1 Pd1 S1 82.53(13) . . ? N2 Pd1 S2 83.80(14) . . ? N1 Pd1 S2 165.65(13) . . ? S1 Pd1 S2 111.01(6) . . ? N2 Pd1 O1 119.84(15) . . ? N1 Pd1 O1 116.63(14) . . ? S1 Pd1 O1 73.63(9) . . ? S2 Pd1 O1 73.27(9) . . ? C18 S1 C1 104.7(3) . . ? C18 S1 Pd1 113.7(2) . . ? C1 S1 Pd1 98.7(2) . . ? C14 S2 C15 98.6(3) . . ? C14 S2 Pd1 98.8(2) . . ? C15 S2 Pd1 107.1(3) . . ? C16 O1 C17 114.8(5) . . ? C16 O1 Pd1 101.4(3) . . ? C17 O1 Pd1 102.1(3) . . ? C2 N1 C6 121.5(5) . . ? C2 N1 Pd1 125.9(4) . . ? C6 N1 Pd1 112.7(4) . . ? C13 N2 C7 121.1(5) . . ? C13 N2 Pd1 126.2(4) . . ? C7 N2 Pd1 112.7(4) . . ? C2 C1 S1 111.4(4) . . ? N1 C2 C3 119.2(6) . . ? N1 C2 C1 115.7(5) . . ? C3 C2 C1 125.0(6) . . ? C4 C3 C2 120.5(6) . . ? C3 C4 C5 120.7(6) . . ? C6 C5 C4 116.6(6) . . ? C6 C5 C10 116.3(7) . . ? C4 C5 C10 127.1(7) . . ? N1 C6 C5 121.6(6) . . ? N1 C6 C7 115.9(5) . . ? C5 C6 C7 122.5(6) . . ? C9 C10 C5 121.5(7) . . ? C10 C9 C8 123.0(6) . . ? C7 C8 C11 116.0(7) . . ? C7 C8 C9 115.7(7) . . ? C11 C8 C9 128.3(7) . . ? N2 C7 C8 122.6(6) . . ? N2 C7 C6 116.4(5) . . ? C8 C7 C6 120.9(6) . . ? C12 C11 C8 121.2(6) . . ? C11 C12 C13 120.1(7) . . ? N2 C13 C12 119.0(7) . . ? N2 C13 C14 115.8(5) . . ? C12 C13 C14 125.2(6) . . ? C13 C14 S2 114.1(4) . . ? C16 C15 S2 111.3(5) . . ? O1 C16 C15 110.2(6) . . ? O1 C17 C18 116.6(5) . . ? C17 C18 S1 115.8(5) . . ? F1C B1 F1A 111.3(6) . . ? F1C B1 F1D 108.4(6) . . ? F1A B1 F1D 110.4(5) . . ? F1C B1 F1B 106.8(5) . . ? F1A B1 F1B 110.6(5) . . ? F1D B1 F1B 109.3(6) . . ? F2D B2 F2B 111.3(8) . . ? F2D B2 F2C 115.9(8) . . ? F2B B2 F2C 117.7(7) . . ? F2D B2 F2A 107.0(11) . . ? F2B B2 F2A 98.0(9) . . ? F2C B2 F2A 104.4(8) . . ? 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 N2 Pd1 S1 C18 -151.6(5) . . . . ? N1 Pd1 S1 C18 -127.1(3) . . . . ? S2 Pd1 S1 C18 57.8(3) . . . . ? O1 Pd1 S1 C18 -6.4(3) . . . . ? N2 Pd1 S1 C1 -41.3(5) . . . . ? N1 Pd1 S1 C1 -16.7(2) . . . . ? S2 Pd1 S1 C1 168.2(2) . . . . ? O1 Pd1 S1 C1 103.9(2) . . . . ? N2 Pd1 S2 C14 7.4(3) . . . . ? N1 Pd1 S2 C14 19.2(5) . . . . ? S1 Pd1 S2 C14 179.2(2) . . . . ? O1 Pd1 S2 C14 -116.3(2) . . . . ? N2 Pd1 S2 C15 109.3(3) . . . . ? N1 Pd1 S2 C15 121.1(6) . . . . ? S1 Pd1 S2 C15 -79.0(3) . . . . ? O1 Pd1 S2 C15 -14.5(3) . . . . ? N2 Pd1 O1 C16 -88.4(4) . . . . ? N1 Pd1 O1 C16 175.2(4) . . . . ? S1 Pd1 O1 C16 102.6(4) . . . . ? S2 Pd1 O1 C16 -16.0(4) . . . . ? N2 Pd1 O1 C17 152.8(4) . . . . ? N1 Pd1 O1 C17 56.4(4) . . . . ? S1 Pd1 O1 C17 -16.2(3) . . . . ? S2 Pd1 O1 C17 -134.8(4) . . . . ? N2 Pd1 N1 C2 -177.1(4) . . . . ? S1 Pd1 N1 C2 9.9(4) . . . . ? S2 Pd1 N1 C2 171.0(4) . . . . ? O1 Pd1 N1 C2 -57.6(4) . . . . ? N2 Pd1 N1 C6 4.1(3) . . . . ? S1 Pd1 N1 C6 -169.0(3) . . . . ? S2 Pd1 N1 C6 -7.8(7) . . . . ? O1 Pd1 N1 C6 123.6(3) . . . . ? N1 Pd1 N2 C13 179.3(5) . . . . ? S1 Pd1 N2 C13 -156.1(4) . . . . ? S2 Pd1 N2 C13 -3.6(4) . . . . ? O1 Pd1 N2 C13 63.1(5) . . . . ? N1 Pd1 N2 C7 -3.6(3) . . . . ? S1 Pd1 N2 C7 20.9(7) . . . . ? S2 Pd1 N2 C7 173.4(4) . . . . ? O1 Pd1 N2 C7 -119.9(3) . . . . ? C18 S1 C1 C2 141.9(4) . . . . ? Pd1 S1 C1 C2 24.5(4) . . . . ? C6 N1 C2 C3 0.9(8) . . . . ? Pd1 N1 C2 C3 -177.8(4) . . . . ? C6 N1 C2 C1 -176.2(5) . . . . ? Pd1 N1 C2 C1 5.1(7) . . . . ? S1 C1 C2 N1 -21.4(6) . . . . ? S1 C1 C2 C3 161.7(5) . . . . ? N1 C2 C3 C4 -0.5(9) . . . . ? C1 C2 C3 C4 176.4(6) . . . . ? C2 C3 C4 C5 -0.1(9) . . . . ? C3 C4 C5 C6 0.2(9) . . . . ? C3 C4 C5 C10 -179.0(6) . . . . ? C2 N1 C6 C5 -0.9(7) . . . . ? Pd1 N1 C6 C5 178.0(4) . . . . ? C2 N1 C6 C7 177.3(5) . . . . ? Pd1 N1 C6 C7 -3.8(6) . . . . ? C4 C5 C6 N1 0.3(8) . . . . ? C10 C5 C6 N1 179.6(5) . . . . ? C4 C5 C6 C7 -177.7(5) . . . . ? C10 C5 C6 C7 1.5(8) . . . . ? C6 C5 C10 C9 -1.3(9) . . . . ? C4 C5 C10 C9 177.9(6) . . . . ? C5 C10 C9 C8 0.0(11) . . . . ? C10 C9 C8 C7 1.0(9) . . . . ? C10 C9 C8 C11 179.8(7) . . . . ? C13 N2 C7 C8 -0.7(8) . . . . ? Pd1 N2 C7 C8 -177.9(4) . . . . ? C13 N2 C7 C6 179.8(5) . . . . ? Pd1 N2 C7 C6 2.6(6) . . . . ? C11 C8 C7 N2 0.8(8) . . . . ? C9 C8 C7 N2 179.8(5) . . . . ? C11 C8 C7 C6 -179.7(5) . . . . ? C9 C8 C7 C6 -0.7(8) . . . . ? N1 C6 C7 N2 0.8(7) . . . . ? C5 C6 C7 N2 179.0(5) . . . . ? N1 C6 C7 C8 -178.7(5) . . . . ? C5 C6 C7 C8 -0.6(8) . . . . ? C7 C8 C11 C12 -0.1(9) . . . . ? C9 C8 C11 C12 -178.9(6) . . . . ? C8 C11 C12 C13 -0.7(10) . . . . ? C7 N2 C13 C12 -0.2(8) . . . . ? Pd1 N2 C13 C12 176.6(4) . . . . ? C7 N2 C13 C14 179.5(5) . . . . ? Pd1 N2 C13 C14 -3.7(7) . . . . ? C11 C12 C13 N2 0.9(9) . . . . ? C11 C12 C13 C14 -178.8(6) . . . . ? N2 C13 C14 S2 11.0(7) . . . . ? C12 C13 C14 S2 -169.3(5) . . . . ? C15 S2 C14 C13 -120.6(5) . . . . ? Pd1 S2 C14 C13 -11.6(5) . . . . ? C14 S2 C15 C16 152.5(6) . . . . ? Pd1 S2 C15 C16 50.4(7) . . . . ? C17 O1 C16 C15 159.2(6) . . . . ? Pd1 O1 C16 C15 50.0(6) . . . . ? S2 C15 C16 O1 -72.2(8) . . . . ? C16 O1 C17 C18 -68.7(8) . . . . ? Pd1 O1 C17 C18 40.1(7) . . . . ? O1 C17 C18 S1 -52.2(9) . . . . ? C1 S1 C18 C17 -74.9(6) . . . . ? Pd1 S1 C18 C17 31.7(7) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.98 _refine_diff_density_min -0.88 _refine_diff_density_rms 0.10 #===END data_Ru(L')Cl(Cl).4H2O _database_code_CSD 156512 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C18 H18 Cl N2 Ru S3, Cl, 4(H2 O)' _chemical_formula_sum 'C18 H26 Cl2 N2 O4 Ru S3' _chemical_formula_weight 602.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7800(10) _cell_length_b 14.6190(10) _cell_length_c 7.6281(8) _cell_angle_alpha 104.260(9) _cell_angle_beta 95.420(10) _cell_angle_gamma 67.081(7) _cell_volume 1172.66(18) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 17.22 _cell_measurement_theta_max 20.08 _exptl_crystal_description needle _exptl_crystal_colour 'pale red' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.706 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 612 _exptl_absorpt_coefficient_mu 1.191 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.780 _exptl_absorpt_correction_T_max 0.911 _exptl_absorpt_process_details 'North, Phillips & Mathews, 1968' _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC5S' _diffrn_measurement_method '\w--2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 4342 _diffrn_reflns_av_R_equivalents 0.013 _diffrn_reflns_av_sigmaI/netI 0.036 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 24.99 _reflns_number_total 4113 _reflns_number_gt 3386 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; MSC/AFC5S Control Program (Molecular Structure Corporation, 1995) ; _computing_cell_refinement ; MSC/AFC5S Control Program (Molecular Structure Corporation, 1995) ; _computing_data_reduction ; TEXSAN (Molecular Structure Corporation, 1989) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP II (Johnson, 1976)' _computing_publication_material 'SHELXL-97; PLATON (Spek, 2001)' _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 w=1/[\s^2^(Fo^2^)+(0.0504P)^2^+3.9289P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4113 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0596 _refine_ls_R_factor_obs 0.0435 _refine_ls_wR_factor_ref 0.1352 _refine_ls_wR_factor_obs 0.1268 _refine_ls_goodness_of_fit_ref 1.156 _refine_ls_restrained_S_all 1.156 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.52695(4) 0.20188(3) 0.13132(6) 0.03445(16) Uani 1 d . . . Cl1 Cl 0.41280(16) 0.23241(13) 0.4054(2) 0.0516(4) Uani 1 d . . . Cl2 Cl 0.0068(3) 0.2306(3) 0.1465(4) 0.1215(11) Uani 1 d . . . S1 S 0.41187(16) 0.11129(12) -0.0426(2) 0.0441(4) Uani 1 d . . . S2 S 0.70493(15) 0.09889(12) 0.2595(2) 0.0479(4) Uani 1 d . . . S3 S 0.64092(15) 0.15970(12) -0.1258(2) 0.0440(4) Uani 1 d . . . O1 O 0.1294(7) 0.3713(7) 0.3570(12) 0.134(3) Uani 1 d . . . O2 O -0.0325(7) 0.4193(8) 0.6472(11) 0.139(3) Uani 1 d . . . O3 O -0.0399(8) 0.2454(8) 0.7560(14) 0.158(4) Uani 1 d . . . O4A O 0.1166(17) 0.1165(15) 0.476(3) 0.179(10) Uani 0.50 d P . . O4B O 0.012(3) 0.0203(14) 0.516(4) 0.107(9) Uani 0.50 d P . . N1 N 0.3896(4) 0.3215(4) 0.0598(6) 0.0374(11) Uani 1 d . . . N2 N 0.5883(4) 0.3132(4) 0.2519(6) 0.0362(11) Uani 1 d . . . C1 C 0.2731(6) 0.2194(5) -0.0788(11) 0.0586(18) Uani 1 d . . . H1A H 0.2486 0.2055 -0.2045 0.070 Uiso 1 calc R . . H1B H 0.2068 0.2249 -0.0054 0.070 Uiso 1 calc R . . C2 C 0.2886(6) 0.3202(5) -0.0339(8) 0.0455(15) Uani 1 d . . . C3 C 0.2014(6) 0.4109(6) -0.0742(10) 0.0573(18) Uani 1 d . . . H3 H 0.1315 0.4094 -0.1406 0.069 Uiso 1 calc R . . C4 C 0.2178(6) 0.5005(6) -0.0176(9) 0.0555(18) Uani 1 d . . . H4 H 0.1601 0.5596 -0.0467 0.067 Uiso 1 calc R . . C5 C 0.3233(6) 0.5038(5) 0.0859(8) 0.0438(14) Uani 1 d . . . C6 C 0.4063(5) 0.4119(4) 0.1203(8) 0.0371(13) Uani 1 d . . . C7 C 0.5145(6) 0.4070(4) 0.2226(7) 0.0371(13) Uani 1 d . . . C8 C 0.5438(6) 0.4936(5) 0.2874(8) 0.0439(15) Uani 1 d . . . C9 C 0.4578(7) 0.5883(5) 0.2488(9) 0.0487(16) Uani 1 d . . . H9 H 0.4746 0.6471 0.2894 0.058 Uiso 1 calc R . . C10 C 0.3536(7) 0.5931(5) 0.1550(9) 0.0526(17) Uani 1 d . . . H10 H 0.2996 0.6556 0.1340 0.063 Uiso 1 calc R . . C11 C 0.6556(7) 0.4795(5) 0.3851(8) 0.0508(17) Uani 1 d . . . H11 H 0.6801 0.5342 0.4293 0.061 Uiso 1 calc R . . C12 C 0.7261(6) 0.3868(5) 0.4138(9) 0.0505(16) Uani 1 d . . . H12 H 0.7993 0.3782 0.4780 0.061 Uiso 1 calc R . . C13 C 0.6913(6) 0.3020(5) 0.3482(8) 0.0431(14) Uani 1 d . . . C14 C 0.7604(6) 0.1985(5) 0.3861(10) 0.0563(18) Uani 1 d . . . H14A H 0.7549 0.2037 0.5145 0.068 Uiso 1 calc R . . H14B H 0.8467 0.1774 0.3571 0.068 Uiso 1 calc R . . C15 C 0.8169(7) 0.0381(6) 0.0768(10) 0.062(2) Uani 1 d . . . H15A H 0.8990 0.0220 0.1279 0.075 Uiso 1 calc R . . H15B H 0.8097 -0.0255 0.0129 0.075 Uiso 1 calc R . . C16 C 0.8012(6) 0.1029(6) -0.0555(10) 0.0603(19) Uani 1 d . . . H16A H 0.8514 0.0615 -0.1615 0.072 Uiso 1 calc R . . H16B H 0.8305 0.1570 -0.0009 0.072 Uiso 1 calc R . . C17 C 0.6173(7) 0.0459(5) -0.2602(9) 0.0515(16) Uani 1 d . . . H17A H 0.6494 0.0292 -0.3815 0.062 Uiso 1 calc R . . H17B H 0.6612 -0.0116 -0.2055 0.062 Uiso 1 calc R . . C18 C 0.4829(7) 0.0658(5) -0.2686(8) 0.0531(17) Uani 1 d . . . H18A H 0.4714 0.0034 -0.3297 0.064 Uiso 1 calc R . . H18B H 0.4416 0.1164 -0.3392 0.064 Uiso 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 Ru 0.0403(3) 0.0303(3) 0.0342(3) 0.00592(18) -0.00261(18) -0.0164(2) Cl1 0.0617(10) 0.0542(9) 0.0424(9) 0.0078(7) 0.0069(7) -0.0260(8) Cl2 0.107(2) 0.146(3) 0.116(2) -0.007(2) 0.0234(18) -0.069(2) S1 0.0558(10) 0.0440(8) 0.0412(8) 0.0080(7) -0.0030(7) -0.0299(8) S2 0.0485(9) 0.0418(8) 0.0519(10) 0.0149(7) -0.0052(7) -0.0141(7) S3 0.0565(10) 0.0384(8) 0.0417(8) 0.0052(6) 0.0047(7) -0.0241(7) O1 0.094(6) 0.160(8) 0.119(6) 0.005(6) 0.011(5) -0.032(5) O2 0.096(6) 0.214(10) 0.105(6) 0.029(6) -0.014(5) -0.064(6) O3 0.113(7) 0.191(10) 0.143(8) 0.027(7) -0.029(6) -0.042(7) O4A 0.138(15) 0.146(15) 0.143(15) 0.059(13) 0.065(12) 0.093(12) O4B 0.117(15) 0.053(15) 0.067(11) -0.004(12) -0.058(8) 0.033(14) N1 0.041(3) 0.036(3) 0.036(3) 0.008(2) -0.002(2) -0.017(2) N2 0.039(3) 0.038(3) 0.031(2) 0.006(2) 0.001(2) -0.016(2) C1 0.050(4) 0.063(5) 0.066(5) 0.013(4) -0.012(3) -0.029(4) C2 0.042(3) 0.055(4) 0.040(3) 0.012(3) -0.002(3) -0.019(3) C3 0.045(4) 0.059(4) 0.063(5) 0.022(4) -0.006(3) -0.013(3) C4 0.045(4) 0.056(4) 0.056(4) 0.025(3) 0.004(3) -0.001(3) C5 0.050(4) 0.040(3) 0.037(3) 0.011(3) 0.012(3) -0.010(3) C6 0.045(3) 0.034(3) 0.035(3) 0.008(2) 0.007(2) -0.016(3) C7 0.048(3) 0.035(3) 0.030(3) 0.003(2) 0.010(3) -0.018(3) C8 0.062(4) 0.042(3) 0.034(3) -0.001(3) 0.017(3) -0.029(3) C9 0.072(5) 0.030(3) 0.047(4) 0.003(3) 0.019(3) -0.022(3) C10 0.075(5) 0.034(3) 0.047(4) 0.007(3) 0.022(4) -0.014(3) C11 0.069(5) 0.055(4) 0.039(3) -0.005(3) 0.008(3) -0.043(4) C12 0.053(4) 0.065(4) 0.041(3) 0.000(3) 0.001(3) -0.037(4) C13 0.041(3) 0.058(4) 0.031(3) 0.004(3) 0.001(3) -0.024(3) C14 0.048(4) 0.062(4) 0.053(4) 0.013(3) -0.016(3) -0.017(3) C15 0.050(4) 0.051(4) 0.067(5) -0.001(4) 0.003(4) -0.006(3) C16 0.048(4) 0.060(4) 0.064(5) -0.002(4) 0.008(3) -0.019(3) C17 0.068(4) 0.045(4) 0.042(4) 0.002(3) 0.004(3) -0.025(3) C18 0.074(5) 0.058(4) 0.036(3) 0.005(3) -0.003(3) -0.038(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 Ru N2 2.017(5) . ? Ru N1 2.018(5) . ? Ru S3 2.2993(16) . ? Ru S2 2.3447(17) . ? Ru S1 2.3547(16) . ? Ru Cl1 2.4458(16) . ? S1 C1 1.834(7) . ? S1 C18 1.841(7) . ? S2 C15 1.815(7) . ? S2 C14 1.847(7) . ? S3 C16 1.830(7) . ? S3 C17 1.834(6) . ? O4B O4B 0.73(5) 2_556 ? N1 C2 1.334(8) . ? N1 C6 1.372(7) . ? N2 C13 1.332(7) . ? N2 C7 1.368(7) . ? C1 C2 1.508(9) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.410(9) . ? C3 C4 1.357(10) . ? C3 H3 0.9300 . ? C4 C5 1.419(10) . ? C4 H4 0.9300 . ? C5 C6 1.390(8) . ? C5 C10 1.448(9) . ? C6 C7 1.417(8) . ? C7 C8 1.402(8) . ? C8 C11 1.419(9) . ? C8 C9 1.442(9) . ? C9 C10 1.347(10) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.345(10) . ? C11 H11 0.9300 . ? C12 C13 1.417(9) . ? C12 H12 0.9300 . ? C13 C14 1.499(9) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.500(10) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.492(10) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 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 N2 Ru N1 80.91(19) . . ? N2 Ru S3 92.69(13) . . ? N1 Ru S3 94.27(14) . . ? N2 Ru S2 83.08(14) . . ? N1 Ru S2 163.95(14) . . ? S3 Ru S2 87.66(6) . . ? N2 Ru S1 163.17(14) . . ? N1 Ru S1 82.36(14) . . ? S3 Ru S1 86.74(6) . . ? S2 Ru S1 113.68(6) . . ? N2 Ru Cl1 90.15(14) . . ? N1 Ru Cl1 89.68(14) . . ? S3 Ru Cl1 175.46(6) . . ? S2 Ru Cl1 89.17(6) . . ? S1 Ru Cl1 91.57(6) . . ? C1 S1 C18 100.6(3) . . ? C1 S1 Ru 99.1(2) . . ? C18 S1 Ru 104.1(2) . . ? C15 S2 C14 99.9(4) . . ? C15 S2 Ru 104.9(3) . . ? C14 S2 Ru 99.1(2) . . ? C16 S3 C17 100.6(3) . . ? C16 S3 Ru 104.7(3) . . ? C17 S3 Ru 103.4(2) . . ? C2 N1 C6 119.5(5) . . ? C2 N1 Ru 127.0(4) . . ? C6 N1 Ru 113.5(4) . . ? C13 N2 C7 120.0(5) . . ? C13 N2 Ru 126.4(4) . . ? C7 N2 Ru 113.6(4) . . ? C2 C1 S1 114.2(5) . . ? C2 C1 H1A 108.7 . . ? S1 C1 H1A 108.7 . . ? C2 C1 H1B 108.7 . . ? S1 C1 H1B 108.7 . . ? H1A C1 H1B 107.6 . . ? N1 C2 C3 119.9(6) . . ? N1 C2 C1 115.4(6) . . ? C3 C2 C1 124.5(6) . . ? C4 C3 C2 121.0(7) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 119.8(6) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C6 C5 C4 116.5(6) . . ? C6 C5 C10 117.3(6) . . ? C4 C5 C10 126.2(6) . . ? N1 C6 C5 123.1(6) . . ? N1 C6 C7 115.9(5) . . ? C5 C6 C7 121.0(5) . . ? N2 C7 C8 122.6(6) . . ? N2 C7 C6 116.1(5) . . ? C8 C7 C6 121.3(6) . . ? C7 C8 C11 116.6(6) . . ? C7 C8 C9 117.2(6) . . ? C11 C8 C9 126.2(6) . . ? C10 C9 C8 121.3(6) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C9 C10 C5 121.9(6) . . ? C9 C10 H10 119.0 . . ? C5 C10 H10 119.0 . . ? C12 C11 C8 119.8(6) . . ? C12 C11 H11 120.1 . . ? C8 C11 H11 120.1 . . ? C11 C12 C13 121.4(6) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? N2 C13 C12 119.6(6) . . ? N2 C13 C14 116.1(5) . . ? C12 C13 C14 124.3(6) . . ? C13 C14 S2 114.6(4) . . ? C13 C14 H14A 108.6 . . ? S2 C14 H14A 108.6 . . ? C13 C14 H14B 108.6 . . ? S2 C14 H14B 108.6 . . ? H14A C14 H14B 107.6 . . ? C16 C15 S2 113.3(5) . . ? C16 C15 H15A 108.9 . . ? S2 C15 H15A 108.9 . . ? C16 C15 H15B 108.9 . . ? S2 C15 H15B 108.9 . . ? H15A C15 H15B 107.7 . . ? C15 C16 S3 112.8(5) . . ? C15 C16 H16A 109.0 . . ? S3 C16 H16A 109.0 . . ? C15 C16 H16B 109.0 . . ? S3 C16 H16B 109.0 . . ? H16A C16 H16B 107.8 . . ? C18 C17 S3 109.4(5) . . ? C18 C17 H17A 109.8 . . ? S3 C17 H17A 109.8 . . ? C18 C17 H17B 109.8 . . ? S3 C17 H17B 109.8 . . ? H17A C17 H17B 108.2 . . ? C17 C18 S1 112.3(5) . . ? C17 C18 H18A 109.1 . . ? S1 C18 H18A 109.1 . . ? C17 C18 H18B 109.1 . . ? S1 C18 H18B 109.1 . . ? H18A C18 H18B 107.9 . . ? 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 C18 S1 C1 C2 -92.1(6) . . . . ? C6 N1 C2 C3 1.7(9) . . . . ? C6 N1 C2 C1 -174.4(5) . . . . ? S1 C1 C2 N1 -13.4(8) . . . . ? S1 C1 C2 C3 170.7(6) . . . . ? N1 C2 C3 C4 -0.7(10) . . . . ? C1 C2 C3 C4 175.1(7) . . . . ? C2 C3 C4 C5 -0.9(11) . . . . ? C3 C4 C5 C6 1.3(9) . . . . ? C3 C4 C5 C10 179.7(6) . . . . ? C2 N1 C6 C5 -1.3(8) . . . . ? C2 N1 C6 C7 178.5(5) . . . . ? C4 C5 C6 N1 -0.2(9) . . . . ? C10 C5 C6 N1 -178.8(5) . . . . ? C4 C5 C6 C7 -180.0(5) . . . . ? C10 C5 C6 C7 1.4(8) . . . . ? C13 N2 C7 C8 1.3(8) . . . . ? C13 N2 C7 C6 -179.4(5) . . . . ? N1 C6 C7 N2 -1.3(7) . . . . ? C5 C6 C7 N2 178.5(5) . . . . ? N1 C6 C7 C8 178.1(5) . . . . ? C5 C6 C7 C8 -2.1(8) . . . . ? N2 C7 C8 C11 0.5(8) . . . . ? C6 C7 C8 C11 -178.8(5) . . . . ? N2 C7 C8 C9 -179.4(5) . . . . ? C6 C7 C8 C9 1.3(8) . . . . ? C7 C8 C9 C10 0.2(9) . . . . ? C11 C8 C9 C10 -179.7(6) . . . . ? C8 C9 C10 C5 -0.9(9) . . . . ? C6 C5 C10 C9 0.1(9) . . . . ? C4 C5 C10 C9 -178.4(6) . . . . ? C7 C8 C11 C12 -1.1(9) . . . . ? C9 C8 C11 C12 178.8(6) . . . . ? C8 C11 C12 C13 0.0(10) . . . . ? C7 N2 C13 C12 -2.4(8) . . . . ? C7 N2 C13 C14 175.1(5) . . . . ? C11 C12 C13 N2 1.8(9) . . . . ? C11 C12 C13 C14 -175.5(6) . . . . ? N2 C13 C14 S2 10.0(8) . . . . ? C12 C13 C14 S2 -172.6(5) . . . . ? C15 S2 C14 C13 98.9(6) . . . . ? C14 S2 C15 C16 -70.8(6) . . . . ? S2 C15 C16 S3 -46.9(7) . . . . ? C17 S3 C16 C15 -69.1(6) . . . . ? C16 S3 C17 C18 157.1(5) . . . . ? S3 C17 C18 S1 -53.3(6) . . . . ? C1 S1 C18 C17 133.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.77 _refine_diff_density_min -0.86 _refine_diff_density_rms 0.12 #===END data_Ru(L)PPh3(PF6)2.0.25CH3CN _database_code_CSD 156513 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H33.75 N O P Ru S 2+, 2(P F6 -), 0.25(C2 H3 N)' _chemical_formula_sum 'C36.50 H33.75 F12 N2.25 O P3 Ru S2' _chemical_formula_weight 1006.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M I2/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 25.13(2) _cell_length_b 12.55(2) _cell_length_c 25.98(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.15(5) _cell_angle_gamma 90.00 _cell_volume 8089(16) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 44 _cell_measurement_theta_min 12 _cell_measurement_theta_max 13 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.652 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4044 _exptl_absorpt_coefficient_mu 0.699 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.498 _exptl_absorpt_correction_T_max 0.790 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 1997b)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Stoe Satdi-4 four-circle' _diffrn_measurement_method omega/theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% none _diffrn_reflns_number 8760 _diffrn_reflns_av_R_equivalents 0.044 _diffrn_reflns_av_sigmaI/netI 0.056 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 26.03 _reflns_number_total 7958 _reflns_number_gt 5843 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STADI4 (Stoe & Cie, 1997a)' _computing_cell_refinement STADI4 _computing_data_reduction 'X-RED (Stoe & Cie, 1997b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1994)' _computing_publication_material 'SHELXL97; PLATON (Spek, 2001)' _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^)+(0.0737P)^2^+51.4746P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7958 _refine_ls_number_parameters 558 _refine_ls_number_restraints 821 _refine_ls_R_factor_all 0.0872 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.1561 _refine_ls_wR_factor_gt 0.1355 _refine_ls_goodness_of_fit_ref 1.03 _refine_ls_restrained_S_all 1.32 _refine_ls_shift/su_max 0.20 _refine_ls_shift/su_mean 0.01 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.57958(2) 0.58942(4) 0.35573(2) 0.02028(16) Uani 1 1 d . . . P2 P 0.61204(7) 0.45928(14) 0.41252(7) 0.0246(4) Uani 1 1 d . . . S2 S 0.57066(8) 0.47197(15) 0.28471(7) 0.0309(4) Uani 1 1 d . . . P1 P 0.37599(8) 0.45122(17) 0.24895(8) 0.0357(5) Uani 1 1 d D . . P3 P 0.61921(8) 0.43805(16) 0.10855(7) 0.0308(4) Uani 1 1 d D . . S1 S 0.49972(7) 0.60833(14) 0.39021(7) 0.0297(4) Uani 1 1 d . . . F1 F 0.43503(18) 0.4272(4) 0.2801(2) 0.0595(15) Uani 1 1 d D . . C25 C 0.5666(3) 0.3492(5) 0.4203(3) 0.0292(15) Uani 1 1 d U . . N2 N 0.6508(2) 0.6227(5) 0.3325(2) 0.0242(12) Uani 1 1 d . . . N1 N 0.6020(2) 0.7161(4) 0.4025(2) 0.0239(12) Uani 1 1 d . . . C6 C 0.6502(3) 0.7586(6) 0.3947(3) 0.0274(14) Uani 1 1 d U . . F2 F 0.39452(18) 0.5687(4) 0.2366(2) 0.0466(12) Uani 1 1 d D . . O1 O 0.5424(2) 0.7036(4) 0.29818(19) 0.0314(11) Uani 1 1 d . . . F4 F 0.3943(2) 0.4106(5) 0.1967(2) 0.0626(15) Uani 1 1 d D . . F6 F 0.31746(18) 0.4753(4) 0.2184(2) 0.0553(14) Uani 1 1 d D . . F5 F 0.3581(2) 0.3327(4) 0.2605(3) 0.0646(16) Uani 1 1 d D . . F3 F 0.3579(2) 0.4917(5) 0.3014(2) 0.0655(16) Uani 1 1 d D . . C31 C 0.6312(3) 0.5114(5) 0.4787(3) 0.0250(14) Uani 1 1 d U . . C19 C 0.6688(3) 0.3873(6) 0.3928(3) 0.0354(17) Uani 1 1 d U . . C1 C 0.5211(3) 0.7106(6) 0.4398(3) 0.0336(16) Uani 1 1 d U . . H1A H 0.4929 0.7663 0.4373 0.040 Uiso 1 1 calc R . . H1B H 0.5238 0.6775 0.4747 0.040 Uiso 1 1 calc R . . C36 C 0.6741(3) 0.5850(6) 0.4894(3) 0.0310(15) Uani 1 1 d U . . H36 H 0.6965 0.5980 0.4639 0.037 Uiso 1 1 calc R . . C9 C 0.7488(3) 0.8368(7) 0.3748(3) 0.0438(19) Uani 1 1 d U . . H9 H 0.7825 0.8635 0.3684 0.053 Uiso 1 1 calc R . . C33 C 0.6103(3) 0.5484(8) 0.5646(3) 0.045(2) Uani 1 1 d U . . H33 H 0.5884 0.5360 0.5906 0.053 Uiso 1 1 calc R . . C5 C 0.6726(3) 0.8493(6) 0.4219(3) 0.0385(17) Uani 1 1 d U . . C7 C 0.6769(3) 0.7078(6) 0.3577(3) 0.0278(14) Uani 1 1 d U . . C13 C 0.6713(3) 0.5752(6) 0.2947(3) 0.0328(16) Uani 1 1 d U . . C30 C 0.5170(3) 0.3392(6) 0.3887(3) 0.0311(16) Uani 1 1 d U . . H30 H 0.5052 0.3933 0.3640 0.037 Uiso 1 1 calc R . . C11 C 0.7484(3) 0.6903(7) 0.3084(3) 0.0412(18) Uani 1 1 d U . . H11 H 0.7826 0.7109 0.3006 0.049 Uiso 1 1 calc R . . C2 C 0.5739(3) 0.7627(6) 0.4352(3) 0.0315(16) Uani 1 1 d U . . C8 C 0.7258(3) 0.7453(6) 0.3466(3) 0.0343(16) Uani 1 1 d U . . C14 C 0.6391(3) 0.4837(7) 0.2681(3) 0.0384(18) Uani 1 1 d U . . H14A H 0.6589 0.4165 0.2777 0.046 Uiso 1 1 calc R . . H14B H 0.6362 0.4927 0.2299 0.046 Uiso 1 1 calc R . . C20 C 0.6594(3) 0.2888(7) 0.3670(3) 0.0403(18) Uani 1 1 d U . . H20 H 0.6247 0.2572 0.3639 0.048 Uiso 1 1 calc R . . C29 C 0.4843(3) 0.2507(6) 0.3927(3) 0.0376(17) Uani 1 1 d U . . H29 H 0.4499 0.2456 0.3715 0.045 Uiso 1 1 calc R . . C34 C 0.6523(3) 0.6196(7) 0.5739(3) 0.043(2) Uani 1 1 d U . . H34 H 0.6595 0.6559 0.6063 0.051 Uiso 1 1 calc R . . C35 C 0.6838(3) 0.6383(7) 0.5364(3) 0.0372(17) Uani 1 1 d U . . H35 H 0.7125 0.6881 0.5428 0.045 Uiso 1 1 calc R . . F9 F 0.6174(2) 0.3231(4) 0.0836(2) 0.0554(14) Uani 1 1 d D A . F12 F 0.6191(2) 0.5531(4) 0.1343(3) 0.0740(18) Uani 1 1 d D A . C12 C 0.7213(3) 0.6074(7) 0.2823(3) 0.0389(18) Uani 1 1 d U . . H12 H 0.7363 0.5713 0.2558 0.047 Uiso 1 1 calc R . . C32 C 0.5996(3) 0.4944(7) 0.5173(3) 0.0348(17) Uani 1 1 d U . . H32 H 0.5704 0.4455 0.5113 0.042 Uiso 1 1 calc R . . C15 C 0.5307(3) 0.5561(6) 0.2359(3) 0.0359(17) Uani 1 1 d U . . H15A H 0.5382 0.5360 0.2009 0.043 Uiso 1 1 calc R . . H15B H 0.4919 0.5429 0.2365 0.043 Uiso 1 1 calc R . . C4 C 0.6422(4) 0.8953(7) 0.4567(3) 0.048(2) Uani 1 1 d U . . H4 H 0.6555 0.9565 0.4762 0.058 Uiso 1 1 calc R . . C17 C 0.4964(3) 0.7591(6) 0.3119(3) 0.0405(19) Uani 1 1 d U . . H17A H 0.4750 0.7898 0.2800 0.049 Uiso 1 1 calc R . . H17B H 0.5089 0.8184 0.3359 0.049 Uiso 1 1 calc R . . C10 C 0.7235(3) 0.8857(7) 0.4104(3) 0.0443(19) Uani 1 1 d U . . H10 H 0.7399 0.9462 0.4283 0.053 Uiso 1 1 calc R . . C18 C 0.4615(3) 0.6852(6) 0.3375(3) 0.0403(19) Uani 1 1 d U . . H18A H 0.4427 0.6357 0.3110 0.048 Uiso 1 1 calc R . . H18B H 0.4338 0.7276 0.3515 0.048 Uiso 1 1 calc R . . C27 C 0.5510(4) 0.1805(6) 0.4590(3) 0.044(2) Uani 1 1 d U . . H27 H 0.5631 0.1253 0.4830 0.053 Uiso 1 1 calc R . . C16 C 0.5421(3) 0.6735(6) 0.2445(3) 0.0369(18) Uani 1 1 d U . . H16A H 0.5776 0.6905 0.2346 0.044 Uiso 1 1 calc R . . H16B H 0.5144 0.7154 0.2219 0.044 Uiso 1 1 calc R . . C24 C 0.7195(4) 0.4321(8) 0.3953(4) 0.055(2) Uani 1 1 d U . . H24 H 0.7271 0.4986 0.4123 0.066 Uiso 1 1 calc R . . C26 C 0.5828(3) 0.2690(6) 0.4563(3) 0.0383(18) Uani 1 1 d U . . H26 H 0.6162 0.2753 0.4792 0.046 Uiso 1 1 calc R . . C3 C 0.5933(4) 0.8528(7) 0.4632(3) 0.046(2) Uani 1 1 d U . . H3 H 0.5727 0.8849 0.4867 0.055 Uiso 1 1 calc R . . C28 C 0.5020(4) 0.1710(7) 0.4273(3) 0.045(2) Uani 1 1 d U . . H28 H 0.4805 0.1094 0.4294 0.054 Uiso 1 1 calc R . . C23 C 0.7594(4) 0.3807(9) 0.3731(5) 0.068(3) Uani 1 1 d U . . H23 H 0.7938 0.4131 0.3747 0.082 Uiso 1 1 calc R . . C21 C 0.6995(4) 0.2376(8) 0.3462(4) 0.057(2) Uani 1 1 d U . . H21 H 0.6926 0.1700 0.3300 0.069 Uiso 1 1 calc R . . C22 C 0.7498(4) 0.2838(8) 0.3488(5) 0.068(3) Uani 1 1 d U . . H22 H 0.7773 0.2489 0.3341 0.081 Uiso 1 1 calc R . . F11 F 0.6814(3) 0.4412(7) 0.1096(7) 0.095(8) Uani 0.65(2) 1 d PD A 1 F10 F 0.6298(5) 0.3721(6) 0.1627(3) 0.061(5) Uani 0.65(2) 1 d PD A 1 F8 F 0.6061(6) 0.4948(7) 0.0554(3) 0.079(6) Uani 0.65(2) 1 d PD A 1 F7 F 0.5567(3) 0.4261(7) 0.1115(6) 0.081(6) Uani 0.65(2) 1 d PD A 1 F11' F 0.6577(8) 0.4751(13) 0.0684(7) 0.068(9) Uani 0.35(2) 1 d PD A 2 F10' F 0.6692(6) 0.4233(15) 0.1511(6) 0.066(9) Uani 0.35(2) 1 d PD A 2 F8' F 0.5688(7) 0.4647(15) 0.0647(8) 0.081(12) Uani 0.35(2) 1 d PD A 2 F7' F 0.5807(9) 0.4124(16) 0.1489(8) 0.089(13) Uani 0.35(2) 1 d PD A 2 C1S C 0.7500 0.062(3) 0.5000 0.070(9) Uiso 0.50 2 d SPDU B 2 C2S C 0.7500 0.177(3) 0.5000 0.14(2) Uiso 0.50 2 d SPDU B 2 N3S N 0.7500 0.268(3) 0.5000 0.167(19) Uiso 0.50 2 d SPD B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0190(3) 0.0212(3) 0.0192(3) -0.0019(2) -0.00166(18) -0.0007(2) P2 0.0226(8) 0.0236(9) 0.0251(9) -0.0005(7) -0.0044(7) 0.0004(7) S2 0.0369(10) 0.0295(9) 0.0243(9) -0.0064(7) -0.0011(7) -0.0011(8) P1 0.0269(10) 0.0364(11) 0.0417(12) -0.0069(9) -0.0014(8) -0.0064(8) P3 0.0310(10) 0.0346(10) 0.0259(9) -0.0010(8) 0.0025(8) -0.0013(8) S1 0.0213(8) 0.0276(9) 0.0406(10) -0.0045(8) 0.0055(7) -0.0006(7) F1 0.031(3) 0.060(3) 0.079(4) 0.027(3) -0.017(2) -0.008(2) C25 0.033(4) 0.023(3) 0.030(4) -0.003(3) 0.000(3) -0.003(3) N2 0.017(3) 0.032(3) 0.024(3) 0.003(2) 0.004(2) 0.000(2) N1 0.027(3) 0.023(3) 0.021(3) 0.002(2) -0.002(2) 0.000(2) C6 0.025(3) 0.030(4) 0.022(3) 0.003(3) -0.009(3) -0.006(3) F2 0.038(3) 0.039(3) 0.057(3) 0.003(2) -0.009(2) -0.007(2) O1 0.033(3) 0.026(3) 0.030(3) 0.005(2) -0.008(2) 0.004(2) F4 0.055(3) 0.069(4) 0.065(4) -0.024(3) 0.016(3) -0.001(3) F6 0.031(3) 0.064(3) 0.066(3) -0.009(3) -0.008(2) -0.003(2) F5 0.044(3) 0.039(3) 0.112(5) 0.001(3) 0.018(3) -0.010(2) F3 0.082(4) 0.072(4) 0.043(3) -0.005(3) 0.012(3) 0.006(3) C31 0.022(3) 0.025(3) 0.026(3) 0.001(3) -0.004(3) 0.000(3) C19 0.033(4) 0.030(4) 0.039(4) 0.003(3) -0.006(3) 0.010(3) C1 0.031(4) 0.039(4) 0.031(4) -0.008(3) 0.007(3) 0.004(3) C36 0.026(3) 0.041(4) 0.022(3) 0.004(3) -0.005(3) -0.009(3) C9 0.029(4) 0.049(5) 0.047(5) 0.025(4) -0.013(3) -0.013(3) C33 0.042(5) 0.061(5) 0.032(4) -0.010(4) 0.010(3) -0.014(4) C5 0.045(4) 0.032(4) 0.033(4) 0.003(3) -0.012(3) -0.008(3) C7 0.026(3) 0.031(4) 0.024(3) 0.008(3) -0.007(3) -0.004(3) C13 0.032(4) 0.042(4) 0.024(3) 0.008(3) 0.004(3) 0.007(3) C30 0.031(4) 0.031(4) 0.030(4) -0.002(3) 0.001(3) -0.005(3) C11 0.024(4) 0.064(5) 0.034(4) 0.026(4) 0.000(3) -0.002(3) C2 0.033(4) 0.030(4) 0.030(4) -0.002(3) 0.001(3) 0.002(3) C8 0.025(3) 0.042(4) 0.033(4) 0.019(3) -0.004(3) -0.001(3) C14 0.036(4) 0.046(5) 0.035(4) -0.006(4) 0.009(3) 0.008(3) C20 0.036(4) 0.037(4) 0.046(5) -0.005(4) 0.003(4) 0.003(3) C29 0.040(4) 0.039(4) 0.034(4) -0.008(3) 0.006(3) -0.017(3) C34 0.036(4) 0.059(5) 0.028(4) -0.010(4) -0.008(3) -0.005(4) C35 0.033(4) 0.043(4) 0.031(4) -0.003(3) -0.009(3) -0.011(3) F9 0.072(4) 0.032(3) 0.061(3) -0.002(2) 0.007(3) 0.005(2) F12 0.075(4) 0.055(3) 0.090(5) -0.041(3) 0.010(3) -0.014(3) C12 0.031(4) 0.058(5) 0.030(4) 0.013(3) 0.013(3) 0.009(3) C32 0.026(4) 0.045(4) 0.032(4) -0.002(3) 0.001(3) -0.007(3) C15 0.034(4) 0.045(4) 0.025(4) 0.001(3) -0.007(3) -0.004(3) C4 0.062(5) 0.038(5) 0.041(5) -0.013(4) -0.004(4) -0.013(4) C17 0.045(5) 0.031(4) 0.038(4) -0.002(3) -0.015(3) 0.013(3) C10 0.039(4) 0.036(4) 0.049(5) 0.008(3) -0.019(3) -0.021(3) C18 0.029(4) 0.035(4) 0.052(5) -0.010(4) -0.008(3) 0.010(3) C27 0.069(6) 0.032(4) 0.031(4) 0.004(3) 0.007(4) -0.005(4) C16 0.044(5) 0.040(4) 0.024(4) 0.004(3) -0.002(3) -0.003(4) C24 0.039(5) 0.046(5) 0.078(7) -0.018(5) 0.001(4) 0.002(4) C26 0.049(5) 0.037(4) 0.025(4) 0.004(3) -0.007(3) -0.005(3) C3 0.063(5) 0.037(5) 0.038(5) -0.014(4) 0.009(4) -0.004(4) C28 0.069(6) 0.034(4) 0.035(4) -0.008(3) 0.014(4) -0.020(4) C23 0.041(5) 0.056(6) 0.110(10) -0.013(6) 0.019(6) 0.011(4) C21 0.054(5) 0.041(5) 0.076(7) -0.015(5) 0.007(5) 0.012(4) C22 0.045(5) 0.055(6) 0.105(9) -0.013(6) 0.017(6) 0.019(4) F11 0.031(5) 0.040(5) 0.22(2) 0.007(8) 0.026(8) -0.007(4) F10 0.099(12) 0.040(5) 0.036(4) 0.009(3) -0.012(5) -0.008(5) F8 0.158(18) 0.046(5) 0.028(4) 0.016(4) 0.001(7) 0.019(8) F7 0.045(6) 0.030(5) 0.173(18) 0.016(7) 0.039(7) 0.005(4) F11' 0.10(2) 0.054(12) 0.062(13) -0.001(10) 0.051(14) -0.010(13) F10' 0.046(13) 0.101(18) 0.041(10) -0.015(11) -0.026(8) 0.027(12) F8' 0.059(13) 0.078(18) 0.091(19) -0.050(15) -0.038(13) 0.029(13) F7' 0.09(2) 0.093(19) 0.10(2) -0.047(17) 0.080(19) -0.045(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 Ru1 N2 2.021(6) . ? Ru1 N1 2.026(6) . ? Ru1 O1 2.172(5) . ? Ru1 P2 2.264(3) . ? Ru1 S1 2.336(2) . ? Ru1 S2 2.344(3) . ? P2 C25 1.825(7) . ? P2 C19 1.829(8) . ? P2 C31 1.831(7) . ? S2 C15 1.825(8) . ? S2 C14 1.845(8) . ? P1 F6 1.585(5) . ? P1 F4 1.585(5) . ? P1 F3 1.588(6) . ? P1 F5 1.597(6) . ? P1 F2 1.595(5) . ? P1 F1 1.602(5) . ? P3 F8 1.542(7) . ? P3 F9 1.579(5) . ? P3 F12 1.592(6) . ? P3 F11 1.560(8) . ? P3 F7 1.591(8) . ? P3 F10 1.616(7) . ? P3 F10' 1.548(10) . ? P3 F7' 1.567(12) . ? P3 F11' 1.600(11) . ? P3 F8' 1.598(11) . ? S1 C18 1.820(8) . ? S1 C1 1.837(8) . ? C25 C26 1.389(10) . ? C25 C30 1.384(10) . ? N2 C13 1.320(9) . ? N2 C7 1.365(9) . ? N1 C2 1.323(9) . ? N1 C6 1.368(9) . ? C6 C5 1.409(10) . ? C6 C7 1.410(10) . ? O1 C17 1.440(9) . ? O1 C16 1.443(9) . ? C31 C32 1.390(10) . ? C31 C36 1.415(9) . ? C19 C24 1.384(12) . ? C19 C20 1.408(11) . ? C1 C2 1.503(10) . ? C36 C35 1.379(10) . ? C9 C10 1.349(13) . ? C9 C8 1.433(12) . ? C33 C34 1.374(12) . ? C33 C32 1.391(11) . ? C5 C4 1.398(13) . ? C5 C10 1.435(12) . ? C7 C8 1.388(10) . ? C13 C12 1.407(11) . ? C13 C14 1.508(11) . ? C30 C29 1.396(10) . ? C11 C12 1.363(12) . ? C11 C8 1.402(12) . ? C2 C3 1.389(11) . ? C20 C21 1.376(12) . ? C29 C28 1.372(12) . ? C34 C35 1.370(12) . ? C15 C16 1.510(11) . ? C4 C3 1.375(13) . ? C17 C18 1.503(12) . ? C27 C28 1.372(13) . ? C27 C26 1.378(11) . ? C24 C23 1.393(13) . ? C23 C22 1.373(15) . ? C21 C22 1.383(14) . ? C1S C2S 1.448(11) . ? C2S N3S 1.140(11) . ? 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 N2 Ru1 N1 80.9(2) . . ? N2 Ru1 O1 87.8(2) . . ? N1 Ru1 O1 86.8(2) . . ? N2 Ru1 P2 95.72(17) . . ? N1 Ru1 P2 97.93(19) . . ? O1 Ru1 P2 174.51(14) . . ? N2 Ru1 S1 161.60(17) . . ? N1 Ru1 S1 82.17(17) . . ? O1 Ru1 S1 83.99(16) . . ? P2 Ru1 S1 93.78(8) . . ? N2 Ru1 S2 82.71(18) . . ? N1 Ru1 S2 161.50(17) . . ? O1 Ru1 S2 84.05(17) . . ? P2 Ru1 S2 92.22(12) . . ? S1 Ru1 S2 112.66(8) . . ? C25 P2 C19 100.8(4) . . ? C25 P2 C31 103.9(3) . . ? C19 P2 C31 109.9(3) . . ? C25 P2 Ru1 116.9(3) . . ? C19 P2 Ru1 112.9(3) . . ? C31 P2 Ru1 111.6(2) . . ? C15 S2 C14 102.8(4) . . ? C15 S2 Ru1 99.0(3) . . ? C14 S2 Ru1 99.1(3) . . ? F6 P1 F4 90.3(3) . . ? F6 P1 F3 90.0(3) . . ? F4 P1 F3 179.8(4) . . ? F6 P1 F5 90.3(3) . . ? F4 P1 F5 89.4(3) . . ? F3 P1 F5 90.5(3) . . ? F6 P1 F2 90.0(3) . . ? F4 P1 F2 89.5(3) . . ? F3 P1 F2 90.6(3) . . ? F5 P1 F2 178.9(3) . . ? F6 P1 F1 179.7(4) . . ? F4 P1 F1 90.0(3) . . ? F3 P1 F1 89.7(3) . . ? F5 P1 F1 89.7(3) . . ? F2 P1 F1 89.9(3) . . ? F8 P3 F9 93.8(4) . . ? F8 P3 F12 86.8(4) . . ? F9 P3 F12 178.0(3) . . ? F8 P3 F11 94.3(7) . . ? F9 P3 F11 89.6(4) . . ? F12 P3 F11 92.3(5) . . ? F8 P3 F7 90.8(7) . . ? F9 P3 F7 88.3(5) . . ? F12 P3 F7 89.8(5) . . ? F11 P3 F7 174.6(6) . . ? F8 P3 F10 175.9(6) . . ? F9 P3 F10 83.1(4) . . ? F12 P3 F10 96.3(4) . . ? F11 P3 F10 88.4(6) . . ? F7 P3 F10 86.4(6) . . ? F8 P3 F10' 136.8(9) . . ? F9 P3 F10' 98.6(6) . . ? F12 P3 F10' 82.2(6) . . ? F11 P3 F10' 45.0(7) . . ? F7 P3 F10' 130.5(9) . . ? F10 P3 F10' 46.7(8) . . ? F8 P3 F7' 128.7(10) . . ? F9 P3 F7' 96.1(7) . . ? F12 P3 F7' 82.0(7) . . ? F11 P3 F7' 135.8(10) . . ? F7 P3 F7' 39.7(8) . . ? F10 P3 F7' 49.3(9) . . ? F10' P3 F7' 90.9(10) . . ? F8 P3 F11' 49.3(8) . . ? F9 P3 F11' 88.8(6) . . ? F12 P3 F11' 93.0(6) . . ? F11 P3 F11' 45.2(8) . . ? F7 P3 F11' 139.7(9) . . ? F10 P3 F11' 133.0(9) . . ? F10' P3 F11' 89.7(9) . . ? F7' P3 F11' 174.9(9) . . ? F8 P3 F8' 39.9(8) . . ? F9 P3 F8' 86.1(6) . . ? F12 P3 F8' 93.2(6) . . ? F11 P3 F8' 133.3(10) . . ? F7 P3 F8' 51.5(9) . . ? F10 P3 F8' 136.8(10) . . ? F10' P3 F8' 174.8(10) . . ? F7' P3 F8' 90.9(10) . . ? F11' P3 F8' 88.1(10) . . ? C18 S1 C1 102.6(4) . . ? C18 S1 Ru1 98.5(3) . . ? C1 S1 Ru1 99.6(2) . . ? C26 C25 C30 118.3(7) . . ? C26 C25 P2 120.0(6) . . ? C30 C25 P2 121.5(6) . . ? C13 N2 C7 119.6(6) . . ? C13 N2 Ru1 126.6(5) . . ? C7 N2 Ru1 113.6(5) . . ? C2 N1 C6 119.9(6) . . ? C2 N1 Ru1 127.3(5) . . ? C6 N1 Ru1 112.6(5) . . ? N1 C6 C5 122.2(7) . . ? N1 C6 C7 117.1(6) . . ? C5 C6 C7 120.7(7) . . ? C17 O1 C16 118.9(6) . . ? C17 O1 Ru1 115.0(4) . . ? C16 O1 Ru1 115.3(4) . . ? C32 C31 C36 117.6(6) . . ? C32 C31 P2 121.9(5) . . ? C36 C31 P2 119.7(5) . . ? C24 C19 C20 117.6(8) . . ? C24 C19 P2 122.6(6) . . ? C20 C19 P2 119.2(6) . . ? C2 C1 S1 114.3(5) . . ? C35 C36 C31 120.8(7) . . ? C10 C9 C8 121.3(7) . . ? C34 C33 C32 120.5(8) . . ? C4 C5 C6 116.2(8) . . ? C4 C5 C10 126.9(8) . . ? C6 C5 C10 116.8(8) . . ? N2 C7 C8 122.7(7) . . ? N2 C7 C6 115.8(6) . . ? C8 C7 C6 121.4(7) . . ? N2 C13 C12 120.6(7) . . ? N2 C13 C14 116.2(7) . . ? C12 C13 C14 123.1(7) . . ? C25 C30 C29 120.9(7) . . ? C12 C11 C8 120.2(7) . . ? N1 C2 C3 121.2(7) . . ? N1 C2 C1 115.3(6) . . ? C3 C2 C1 123.5(7) . . ? C7 C8 C11 116.8(7) . . ? C7 C8 C9 117.7(8) . . ? C11 C8 C9 125.6(7) . . ? C13 C14 S2 113.8(5) . . ? C21 C20 C19 121.2(8) . . ? C28 C29 C30 119.6(8) . . ? C33 C34 C35 120.1(7) . . ? C36 C35 C34 120.4(7) . . ? C11 C12 C13 119.9(8) . . ? C31 C32 C33 120.6(7) . . ? C16 C15 S2 112.9(5) . . ? C3 C4 C5 120.7(8) . . ? O1 C17 C18 111.1(6) . . ? C9 C10 C5 122.1(7) . . ? C17 C18 S1 112.6(5) . . ? C28 C27 C26 120.8(8) . . ? O1 C16 C15 111.8(6) . . ? C19 C24 C23 120.7(9) . . ? C25 C26 C27 120.5(7) . . ? C4 C3 C2 119.8(8) . . ? C27 C28 C29 119.8(8) . . ? C22 C23 C24 121.0(10) . . ? C20 C21 C22 120.4(9) . . ? C23 C22 C21 119.1(9) . . ? N3S C2S C1S 180.000(19) . . ? 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 C19 P2 C25 C26 60.2(7) . . . . ? C31 P2 C25 C26 -53.6(7) . . . . ? C19 P2 C25 C30 -115.4(7) . . . . ? C31 P2 C25 C30 130.8(6) . . . . ? C2 N1 C6 C5 2.3(10) . . . . ? C2 N1 C6 C7 -177.3(6) . . . . ? C25 P2 C31 C32 -22.3(7) . . . . ? C19 P2 C31 C32 -129.4(6) . . . . ? C25 P2 C31 C36 168.2(6) . . . . ? C19 P2 C31 C36 61.1(7) . . . . ? C25 P2 C19 C24 -162.5(8) . . . . ? C31 P2 C19 C24 -53.2(8) . . . . ? C25 P2 C19 C20 27.0(7) . . . . ? C31 P2 C19 C20 136.3(6) . . . . ? C18 S1 C1 C2 -89.2(6) . . . . ? C32 C31 C36 C35 -0.4(11) . . . . ? P2 C31 C36 C35 169.6(6) . . . . ? N1 C6 C5 C4 -1.2(11) . . . . ? C7 C6 C5 C4 178.4(7) . . . . ? N1 C6 C5 C10 179.7(6) . . . . ? C7 C6 C5 C10 -0.8(10) . . . . ? C13 N2 C7 C8 -2.4(10) . . . . ? C13 N2 C7 C6 175.5(6) . . . . ? N1 C6 C7 N2 1.6(9) . . . . ? C5 C6 C7 N2 -177.9(6) . . . . ? N1 C6 C7 C8 179.5(6) . . . . ? C5 C6 C7 C8 -0.1(10) . . . . ? C7 N2 C13 C12 3.8(10) . . . . ? C7 N2 C13 C14 -178.5(6) . . . . ? C26 C25 C30 C29 -0.2(11) . . . . ? P2 C25 C30 C29 175.5(6) . . . . ? C6 N1 C2 C3 -1.9(10) . . . . ? C6 N1 C2 C1 178.6(6) . . . . ? S1 C1 C2 N1 -11.1(9) . . . . ? S1 C1 C2 C3 169.4(7) . . . . ? N2 C7 C8 C11 -1.0(10) . . . . ? C6 C7 C8 C11 -178.7(6) . . . . ? N2 C7 C8 C9 178.6(6) . . . . ? C6 C7 C8 C9 0.9(10) . . . . ? C12 C11 C8 C7 2.9(10) . . . . ? C12 C11 C8 C9 -176.7(7) . . . . ? C10 C9 C8 C7 -0.9(11) . . . . ? C10 C9 C8 C11 178.7(7) . . . . ? N2 C13 C14 S2 11.2(9) . . . . ? C12 C13 C14 S2 -171.1(6) . . . . ? C15 S2 C14 C13 89.0(6) . . . . ? C24 C19 C20 C21 1.7(13) . . . . ? P2 C19 C20 C21 172.6(7) . . . . ? C25 C30 C29 C28 -1.8(12) . . . . ? C32 C33 C34 C35 0.3(14) . . . . ? C31 C36 C35 C34 0.8(12) . . . . ? C33 C34 C35 C36 -0.8(13) . . . . ? C8 C11 C12 C13 -1.6(11) . . . . ? N2 C13 C12 C11 -1.9(11) . . . . ? C14 C13 C12 C11 -179.4(7) . . . . ? C36 C31 C32 C33 0.0(11) . . . . ? P2 C31 C32 C33 -169.8(7) . . . . ? C34 C33 C32 C31 0.1(13) . . . . ? C14 S2 C15 C16 -71.0(7) . . . . ? C6 C5 C4 C3 -0.3(12) . . . . ? C10 C5 C4 C3 178.8(8) . . . . ? C16 O1 C17 C18 102.7(7) . . . . ? C8 C9 C10 C5 0.0(12) . . . . ? C4 C5 C10 C9 -178.2(8) . . . . ? C6 C5 C10 C9 0.8(11) . . . . ? O1 C17 C18 S1 49.7(8) . . . . ? C1 S1 C18 C17 68.5(6) . . . . ? C17 O1 C16 C15 -103.3(8) . . . . ? S2 C15 C16 O1 -47.1(8) . . . . ? C20 C19 C24 C23 -0.2(15) . . . . ? P2 C19 C24 C23 -170.8(9) . . . . ? C30 C25 C26 C27 2.0(12) . . . . ? P2 C25 C26 C27 -173.7(6) . . . . ? C28 C27 C26 C25 -1.8(13) . . . . ? C5 C4 C3 C2 0.6(14) . . . . ? N1 C2 C3 C4 0.5(13) . . . . ? C1 C2 C3 C4 179.9(8) . . . . ? C26 C27 C28 C29 -0.3(13) . . . . ? C30 C29 C28 C27 2.1(12) . . . . ? C19 C24 C23 C22 -0.9(18) . . . . ? C19 C20 C21 C22 -2.1(15) . . . . ? C24 C23 C22 C21 0.5(19) . . . . ? C20 C21 C22 C23 1.0(18) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.41 _refine_diff_density_min -1.07 _refine_diff_density_rms 0.12 #===END