Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' #=============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_coden_Cambridge 0222 #=========================================================================== _audit_creation_date 10-05-2004 # 1. SUBMISSION DETAILS _publ_contact_author_name 'Duncan Carmichael' _publ_contact_author_address ; CNRS UMR 7653 DCPH Ecole Polytechnique Palaiseau 91128 FRANCE ; _publ_contact_author_email DUNCAN.CARMICHAEL@POLYTECHNIQUE.FR _publ_contact_letter ; Please consider this CIF submission for publication as a new structure paper in Dalton Transactions. The figures, chemical structure diagram (scheme), Transfer of Copyright Agreement form and structure factors will be sent on receipt of your acknowledgement letter ; _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? #=============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis, structure and dynamics of methoxynaphtalene- substituted phospharuthenocenes and -ferrocenes. ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'D. Carmichael' ; Laboratoire Heteroelements et Coordination, CNRS UMR 7653, DCPH Ecole Polytechnique, F-91128 Palaiseau Cedex France ; L.Ricard ; Laboratoire Heteroelements et Coordination, CNRS UMR 7653, DCPH Ecole Polytechnique, F-91128 Palaiseau Cedex France ; N.Seeboth ; Laboratoire Heteroelements et Coordination, CNRS UMR 7653, DCPH Ecole Polytechnique, F-91128 Palaiseau Cedex France ; J.M.Brown ; Chemistry Research Laboratory, University of Oxford, Mansfield Road, OX1 3TA, United Kingdom ; T.D.W.Claridge ; Chemistry Research Laboratory, University of Oxford, Mansfield Road, OX1 3TA, United Kingdom ; ; B.Odell ; ; Chemistry Research Laboratory, University of Oxford, Mansfield Road, OX1 3TA, United Kingdom ; #=============================================================================== # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ; _publ_section_exptl_prep ;All structures were solved using SIR97 (Altomare et al.) and refined with SHELXL97 (Sheldrick). Figures were drawn with Platon (Spek, 1990). ; _publ_section_references ;Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993) J. Appl. Cryst. 26, 343-350. Sheldrick, G.M. SHELXL97. Program for crystal structure refinement. University of G\\"ottingen, Germany, 1997. Sluis, P. v.d., Spek, A.L. (1990). Acta Cryst. A46, 194-201. Spek, A.L. (1990). Acta Cryst. A46, C-34. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #=============================================================================== #=============================================================================== data_rumet _database_code_depnum_ccdc_archive 'CCDC 258042' #compound 5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H35 O P Ru' _chemical_formula_weight 579.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.992(5) _cell_length_b 11.740(5) _cell_length_c 12.042(5) _cell_angle_alpha 79.530(5) _cell_angle_beta 71.170(5) _cell_angle_gamma 89.490(5) _cell_volume 1312.9(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150.0(10) _cell_measurement_reflns_used 251 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 20.0 _exptl_crystal_description cube _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.466 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 600 _exptl_absorpt_coefficient_mu 0.683 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8755 _exptl_absorpt_correction_T_max 0.8755 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(10) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11067 _diffrn_reflns_av_R_equivalents 0.0243 _diffrn_reflns_av_sigmaI/netI 0.0556 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.47 _diffrn_reflns_theta_max 30.03 _reflns_number_total 7645 _reflns_number_gt 6403 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+0.6155P] 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 7645 _refine_ls_number_parameters 333 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0490 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.0874 _refine_ls_wR_factor_gt 0.0824 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru -0.126233(16) 0.791411(14) 0.847946(14) 0.01778(6) Uani 1 1 d . . . P1 P -0.09723(5) 0.59438(5) 0.81343(5) 0.01850(11) Uani 1 1 d . . . O1 O -0.21362(16) 0.61733(15) 0.53758(13) 0.0287(4) Uani 1 1 d . . . C1 C -0.2644(2) 0.63247(18) 0.90754(18) 0.0184(4) Uani 1 1 d . . . C2 C -0.3254(2) 0.72190(19) 0.84406(18) 0.0195(4) Uani 1 1 d . . . C3 C -0.2374(2) 0.76018(19) 0.72232(18) 0.0203(4) Uani 1 1 d . . . C4 C -0.1100(2) 0.69981(18) 0.69149(18) 0.0194(4) Uani 1 1 d . . . C5 C -0.3224(2) 0.57142(18) 1.03333(18) 0.0191(4) Uani 1 1 d . . . C6 C -0.2299(2) 0.51566(19) 1.08970(19) 0.0218(4) Uani 1 1 d . . . H6 H -0.1310 0.5228 1.0478 0.026 Uiso 1 1 calc R . . C7 C -0.2785(2) 0.4508(2) 1.20424(19) 0.0251(5) Uani 1 1 d . . . H7 H -0.2132 0.4137 1.2395 0.030 Uiso 1 1 calc R . . C8 C -0.4223(2) 0.4397(2) 1.2680(2) 0.0267(5) Uani 1 1 d . . . H8 H -0.4558 0.3949 1.3467 0.032 Uiso 1 1 calc R . . C9 C -0.5162(2) 0.4946(2) 1.21567(19) 0.0250(5) Uani 1 1 d . . . H9 H -0.6147 0.4882 1.2590 0.030 Uiso 1 1 calc R . . C10 C -0.4674(2) 0.55918(19) 1.09994(19) 0.0213(4) Uani 1 1 d . . . H10 H -0.5335 0.5957 1.0653 0.026 Uiso 1 1 calc R . . C11 C -0.4683(2) 0.7706(2) 0.8935(2) 0.0264(5) Uani 1 1 d . . . H11A H -0.4697 0.8483 0.8474 0.040 Uiso 1 1 calc R . . H11B H -0.4859 0.7753 0.9774 0.040 Uiso 1 1 calc R . . H11C H -0.5422 0.7198 0.8877 0.040 Uiso 1 1 calc R . . C12 C -0.2768(2) 0.8498(2) 0.6338(2) 0.0294(5) Uani 1 1 d . . . H12A H -0.1916 0.8799 0.5667 0.044 Uiso 1 1 calc R . . H12B H -0.3208 0.9135 0.6726 0.044 Uiso 1 1 calc R . . H12C H -0.3439 0.8145 0.6042 0.044 Uiso 1 1 calc R . . C13 C -0.0160(2) 0.70035(19) 0.56560(18) 0.0221(4) Uani 1 1 d . . . C14 C 0.1311(2) 0.7352(2) 0.52023(19) 0.0244(4) Uani 1 1 d . . . C15 C 0.2002(2) 0.7851(2) 0.5867(2) 0.0291(5) Uani 1 1 d . . . H15 H 0.1478 0.7970 0.6646 0.035 Uiso 1 1 calc R . . C16 C 0.3424(2) 0.8169(2) 0.5400(2) 0.0366(6) Uani 1 1 d . . . H16 H 0.3862 0.8515 0.5858 0.044 Uiso 1 1 calc R . . C17 C 0.4243(2) 0.7992(3) 0.4259(2) 0.0386(6) Uani 1 1 d . . . H17 H 0.5228 0.8204 0.3957 0.046 Uiso 1 1 calc R . . C18 C 0.3618(2) 0.7520(2) 0.3596(2) 0.0348(6) Uani 1 1 d . . . H18 H 0.4175 0.7407 0.2822 0.042 Uiso 1 1 calc R . . C19 C 0.2157(2) 0.7189(2) 0.4023(2) 0.0275(5) Uani 1 1 d . . . C20 C 0.1507(3) 0.6685(2) 0.3343(2) 0.0310(5) Uani 1 1 d . . . H20 H 0.2057 0.6565 0.2571 0.037 Uiso 1 1 calc R . . C21 C 0.0108(3) 0.6366(2) 0.37701(19) 0.0279(5) Uani 1 1 d . . . H21 H -0.0312 0.6036 0.3290 0.034 Uiso 1 1 calc R . . C22 C -0.0733(2) 0.6518(2) 0.49225(19) 0.0242(4) Uani 1 1 d . . . C23 C -0.2731(3) 0.5661(2) 0.4635(2) 0.0359(6) Uani 1 1 d . . . H23A H -0.2690 0.6236 0.3923 0.054 Uiso 1 1 calc R . . H23B H -0.3719 0.5401 0.5082 0.054 Uiso 1 1 calc R . . H23C H -0.2190 0.4996 0.4393 0.054 Uiso 1 1 calc R . . C24 C -0.0423(2) 0.83056(19) 0.98458(19) 0.0218(4) Uani 1 1 d . . . C25 C -0.1769(2) 0.88097(19) 0.99837(19) 0.0224(4) Uani 1 1 d . . . C26 C -0.1638(2) 0.96581(18) 0.89150(18) 0.0191(4) Uani 1 1 d . . . C27 C -0.0216(2) 0.96561(18) 0.81253(19) 0.0216(4) Uani 1 1 d . . . C28 C 0.0531(2) 0.88420(19) 0.87121(19) 0.0215(4) Uani 1 1 d . . . C29 C -0.0034(3) 0.7476(2) 1.0774(2) 0.0319(5) Uani 1 1 d . . . H29A H 0.0690 0.6976 1.0386 0.048 Uiso 1 1 calc R . . H29B H -0.0875 0.6997 1.1303 0.048 Uiso 1 1 calc R . . H29C H 0.0338 0.7910 1.1244 0.048 Uiso 1 1 calc R . . C30 C -0.3044(3) 0.8533(2) 1.1095(2) 0.0325(6) Uani 1 1 d . . . H30A H -0.3200 0.7689 1.1352 0.049 Uiso 1 1 calc R . . H30B H -0.3879 0.8858 1.0925 0.049 Uiso 1 1 calc R . . H30C H -0.2884 0.8870 1.1731 0.049 Uiso 1 1 calc R . . C31 C -0.2768(2) 1.0416(2) 0.8705(2) 0.0313(5) Uani 1 1 d . . . H31A H -0.2686 1.1154 0.8955 0.047 Uiso 1 1 calc R . . H31B H -0.3698 1.0031 0.9170 0.047 Uiso 1 1 calc R . . H31C H -0.2666 1.0562 0.7854 0.047 Uiso 1 1 calc R . . C32 C 0.0395(3) 1.0447(2) 0.6940(2) 0.0311(5) Uani 1 1 d . . . H32A H -0.0355 1.0645 0.6589 0.047 Uiso 1 1 calc R . . H32B H 0.1132 1.0056 0.6407 0.047 Uiso 1 1 calc R . . H32C H 0.0807 1.1156 0.7048 0.047 Uiso 1 1 calc R . . C33 C 0.2098(2) 0.8692(2) 0.8332(2) 0.0303(5) Uani 1 1 d . . . H33A H 0.2480 0.8907 0.8924 0.045 Uiso 1 1 calc R . . H33B H 0.2557 0.9191 0.7553 0.045 Uiso 1 1 calc R . . H33C H 0.2280 0.7880 0.8271 0.045 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01526(9) 0.01804(9) 0.01692(9) -0.00061(7) -0.00249(6) 0.00252(6) P1 0.0163(2) 0.0190(3) 0.0169(2) -0.0011(2) -0.00223(19) 0.0038(2) O1 0.0296(8) 0.0347(10) 0.0207(8) -0.0081(7) -0.0050(6) -0.0011(7) C1 0.0147(9) 0.0198(10) 0.0188(10) -0.0023(8) -0.0037(7) 0.0005(7) C2 0.0148(9) 0.0237(11) 0.0191(10) -0.0019(9) -0.0054(8) 0.0020(8) C3 0.0202(9) 0.0226(11) 0.0178(10) -0.0025(9) -0.0067(8) 0.0024(8) C4 0.0199(9) 0.0183(10) 0.0173(10) -0.0008(8) -0.0037(8) 0.0030(8) C5 0.0166(9) 0.0193(10) 0.0189(10) -0.0033(8) -0.0024(8) -0.0012(8) C6 0.0179(9) 0.0221(11) 0.0218(10) -0.0011(9) -0.0034(8) -0.0003(8) C7 0.0255(11) 0.0258(12) 0.0215(11) 0.0007(9) -0.0069(9) 0.0010(9) C8 0.0285(11) 0.0263(12) 0.0187(10) 0.0007(9) -0.0014(9) -0.0043(9) C9 0.0190(10) 0.0275(12) 0.0232(11) -0.0053(10) 0.0010(8) -0.0022(9) C10 0.0181(9) 0.0231(11) 0.0213(10) -0.0043(9) -0.0043(8) 0.0000(8) C11 0.0173(10) 0.0320(13) 0.0274(11) -0.0044(10) -0.0049(8) 0.0080(9) C12 0.0305(12) 0.0325(13) 0.0236(11) -0.0013(10) -0.0092(9) 0.0102(10) C13 0.0245(10) 0.0201(11) 0.0165(10) 0.0012(8) -0.0025(8) 0.0072(8) C14 0.0252(10) 0.0222(11) 0.0195(10) 0.0017(9) -0.0023(8) 0.0085(9) C15 0.0244(11) 0.0336(13) 0.0228(11) -0.0003(10) -0.0017(9) 0.0056(10) C16 0.0228(11) 0.0435(16) 0.0407(14) -0.0074(13) -0.0067(10) 0.0039(11) C17 0.0204(11) 0.0515(18) 0.0330(13) -0.0030(13) 0.0035(10) 0.0050(11) C18 0.0300(12) 0.0397(15) 0.0239(12) -0.0006(11) 0.0032(10) 0.0091(11) C19 0.0266(11) 0.0246(12) 0.0219(11) 0.0027(9) 0.0009(9) 0.0109(9) C20 0.0389(13) 0.0302(13) 0.0181(10) -0.0027(10) -0.0026(9) 0.0129(11) C21 0.0390(13) 0.0245(12) 0.0175(10) -0.0034(9) -0.0059(9) 0.0080(10) C22 0.0278(11) 0.0220(11) 0.0179(10) -0.0010(9) -0.0025(8) 0.0056(9) C23 0.0375(13) 0.0443(16) 0.0285(13) -0.0137(12) -0.0104(10) -0.0003(12) C24 0.0257(10) 0.0182(11) 0.0218(10) -0.0011(9) -0.0097(8) -0.0010(8) C25 0.0252(10) 0.0204(11) 0.0191(10) -0.0055(9) -0.0028(8) -0.0006(8) C26 0.0179(9) 0.0186(10) 0.0193(10) -0.0044(8) -0.0037(8) 0.0044(8) C27 0.0208(10) 0.0158(10) 0.0240(11) 0.0000(9) -0.0035(8) -0.0009(8) C28 0.0190(9) 0.0184(11) 0.0255(11) -0.0024(9) -0.0059(8) -0.0007(8) C29 0.0442(14) 0.0251(12) 0.0302(12) 0.0019(10) -0.0211(11) -0.0021(11) C30 0.0336(12) 0.0333(14) 0.0231(11) -0.0087(11) 0.0028(10) -0.0048(10) C31 0.0293(12) 0.0230(12) 0.0397(14) -0.0053(11) -0.0091(10) 0.0077(10) C32 0.0331(12) 0.0234(12) 0.0272(12) 0.0047(10) -0.0016(10) 0.0007(10) C33 0.0205(10) 0.0308(13) 0.0408(14) -0.0095(11) -0.0105(10) 0.0028(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C2 2.175(2) . ? Ru1 C25 2.176(2) . ? Ru1 C24 2.189(2) . ? Ru1 C1 2.196(2) . ? Ru1 C26 2.204(2) . ? Ru1 C27 2.212(2) . ? Ru1 C28 2.224(2) . ? Ru1 C3 2.225(2) . ? Ru1 C4 2.295(2) . ? Ru1 P1 2.4222(11) . ? P1 C4 1.778(2) . ? P1 C1 1.796(2) . ? O1 C22 1.365(3) . ? O1 C23 1.433(3) . ? C1 C2 1.434(3) . ? C1 C5 1.480(3) . ? C2 C3 1.435(3) . ? C2 C11 1.511(3) . ? C3 C4 1.427(3) . ? C3 C12 1.502(3) . ? C4 C13 1.502(3) . ? C5 C10 1.405(3) . ? C5 C6 1.406(3) . ? C6 C7 1.382(3) . ? C7 C8 1.387(3) . ? C8 C9 1.385(3) . ? C9 C10 1.392(3) . ? C13 C22 1.396(3) . ? C13 C14 1.428(3) . ? C14 C15 1.413(3) . ? C14 C19 1.445(3) . ? C15 C16 1.375(3) . ? C16 C17 1.405(3) . ? C17 C18 1.351(4) . ? C18 C19 1.414(3) . ? C19 C20 1.403(3) . ? C20 C21 1.354(3) . ? C21 C22 1.414(3) . ? C24 C28 1.424(3) . ? C24 C25 1.436(3) . ? C24 C29 1.493(3) . ? C25 C26 1.447(3) . ? C25 C30 1.506(3) . ? C26 C27 1.433(3) . ? C26 C31 1.489(3) . ? C27 C28 1.432(3) . ? C27 C32 1.496(3) . ? C28 C33 1.502(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 Ru1 C25 107.01(8) . . ? C2 Ru1 C24 136.46(8) . . ? C25 Ru1 C24 38.42(8) . . ? C2 Ru1 C1 38.29(8) . . ? C25 Ru1 C1 106.66(8) . . ? C24 Ru1 C1 113.16(8) . . ? C2 Ru1 C26 107.09(8) . . ? C25 Ru1 C26 38.57(8) . . ? C24 Ru1 C26 64.18(8) . . ? C1 Ru1 C26 131.01(8) . . ? C2 Ru1 C27 136.17(8) . . ? C25 Ru1 C27 63.83(8) . . ? C24 Ru1 C27 63.63(8) . . ? C1 Ru1 C27 168.84(7) . . ? C26 Ru1 C27 37.86(7) . . ? C2 Ru1 C28 169.61(7) . . ? C25 Ru1 C28 63.32(8) . . ? C24 Ru1 C28 37.63(8) . . ? C1 Ru1 C28 145.23(8) . . ? C26 Ru1 C28 63.17(8) . . ? C27 Ru1 C28 37.67(8) . . ? C2 Ru1 C3 38.05(8) . . ? C25 Ru1 C3 134.36(8) . . ? C24 Ru1 C3 172.66(7) . . ? C1 Ru1 C3 65.35(8) . . ? C26 Ru1 C3 110.89(8) . . ? C27 Ru1 C3 116.32(8) . . ? C28 Ru1 C3 146.45(8) . . ? C2 Ru1 C4 64.41(7) . . ? C25 Ru1 C4 170.87(7) . . ? C24 Ru1 C4 150.36(8) . . ? C1 Ru1 C4 68.88(8) . . ? C26 Ru1 C4 138.56(8) . . ? C27 Ru1 C4 119.61(8) . . ? C28 Ru1 C4 124.98(7) . . ? C3 Ru1 C4 36.76(7) . . ? C2 Ru1 P1 71.02(6) . . ? C25 Ru1 P1 138.09(6) . . ? C24 Ru1 P1 114.57(6) . . ? C1 Ru1 P1 45.43(5) . . ? C26 Ru1 P1 176.00(5) . . ? C27 Ru1 P1 145.63(6) . . ? C28 Ru1 P1 118.44(6) . . ? C3 Ru1 P1 69.95(6) . . ? C4 Ru1 P1 44.19(6) . . ? C4 P1 C1 90.65(10) . . ? C4 P1 Ru1 64.11(7) . . ? C1 P1 Ru1 60.62(7) . . ? C22 O1 C23 117.51(17) . . ? C2 C1 C5 128.65(17) . . ? C2 C1 P1 111.57(15) . . ? C5 C1 P1 119.78(15) . . ? C2 C1 Ru1 70.06(12) . . ? C5 C1 Ru1 124.20(13) . . ? P1 C1 Ru1 73.95(8) . . ? C1 C2 C3 112.65(17) . . ? C1 C2 C11 125.86(19) . . ? C3 C2 C11 121.45(19) . . ? C1 C2 Ru1 71.66(11) . . ? C3 C2 Ru1 72.87(11) . . ? C11 C2 Ru1 125.21(15) . . ? C4 C3 C2 112.85(19) . . ? C4 C3 C12 122.83(19) . . ? C2 C3 C12 124.26(18) . . ? C4 C3 Ru1 74.29(12) . . ? C2 C3 Ru1 69.08(11) . . ? C12 C3 Ru1 127.03(15) . . ? C3 C4 C13 124.26(19) . . ? C3 C4 P1 112.28(15) . . ? C13 C4 P1 121.59(15) . . ? C3 C4 Ru1 68.95(11) . . ? C13 C4 Ru1 139.87(15) . . ? P1 C4 Ru1 71.70(8) . . ? C10 C5 C6 116.6(2) . . ? C10 C5 C1 124.10(19) . . ? C6 C5 C1 119.21(17) . . ? C7 C6 C5 121.99(19) . . ? C6 C7 C8 120.3(2) . . ? C9 C8 C7 119.2(2) . . ? C8 C9 C10 120.49(19) . . ? C9 C10 C5 121.4(2) . . ? C22 C13 C14 117.78(18) . . ? C22 C13 C4 117.30(19) . . ? C14 C13 C4 124.54(18) . . ? C15 C14 C13 122.61(19) . . ? C15 C14 C19 117.4(2) . . ? C13 C14 C19 120.0(2) . . ? C16 C15 C14 120.8(2) . . ? C15 C16 C17 121.5(2) . . ? C18 C17 C16 119.4(2) . . ? C17 C18 C19 121.7(2) . . ? C20 C19 C18 121.9(2) . . ? C20 C19 C14 118.9(2) . . ? C18 C19 C14 119.2(2) . . ? C21 C20 C19 121.1(2) . . ? C20 C21 C22 120.7(2) . . ? O1 C22 C13 117.08(18) . . ? O1 C22 C21 121.36(19) . . ? C13 C22 C21 121.5(2) . . ? C28 C24 C25 107.71(19) . . ? C28 C24 C29 125.5(2) . . ? C25 C24 C29 126.4(2) . . ? C28 C24 Ru1 72.49(12) . . ? C25 C24 Ru1 70.28(11) . . ? C29 C24 Ru1 128.26(15) . . ? C24 C25 C26 108.11(18) . . ? C24 C25 C30 124.5(2) . . ? C26 C25 C30 127.3(2) . . ? C24 C25 Ru1 71.31(11) . . ? C26 C25 Ru1 71.77(11) . . ? C30 C25 Ru1 125.46(15) . . ? C27 C26 C25 107.34(18) . . ? C27 C26 C31 126.8(2) . . ? C25 C26 C31 125.78(19) . . ? C27 C26 Ru1 71.36(11) . . ? C25 C26 Ru1 69.66(11) . . ? C31 C26 Ru1 125.82(14) . . ? C28 C27 C26 108.12(19) . . ? C28 C27 C32 126.60(19) . . ? C26 C27 C32 125.1(2) . . ? C28 C27 Ru1 71.62(12) . . ? C26 C27 Ru1 70.78(12) . . ? C32 C27 Ru1 127.12(15) . . ? C24 C28 C27 108.69(18) . . ? C24 C28 C33 123.3(2) . . ? C27 C28 C33 127.3(2) . . ? C24 C28 Ru1 69.88(11) . . ? C27 C28 Ru1 70.71(12) . . ? C33 C28 Ru1 132.95(15) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.422 _refine_diff_density_min -0.917 _refine_diff_density_rms 0.091 #END==== data_fepo _database_code_depnum_ccdc_archive 'CCDC 258043' #compound 8 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H33 Fe O P' _chemical_formula_weight 520.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P21/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.4920(10) _cell_length_b 8.0130(10) _cell_length_c 31.1640(10) _cell_angle_alpha 90.00 _cell_angle_beta 93.3200(10) _cell_angle_gamma 90.00 _cell_volume 2615.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 251 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 20.0 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.322 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 0.661 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8792 _exptl_absorpt_correction_T_max 0.9490 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10129 _diffrn_reflns_av_R_equivalents 0.0223 _diffrn_reflns_av_sigmaI/netI 0.0422 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5924 _reflns_number_gt 4619 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+0.8001P] 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 5924 _refine_ls_number_parameters 323 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0579 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1270 _refine_ls_wR_factor_gt 0.1180 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe -0.30706(3) -0.37595(4) 0.100083(8) 0.03414(11) Uani 1 1 d . . . P1 P -0.31446(5) -0.14539(7) 0.143611(17) 0.03719(15) Uani 1 1 d . . . O1 O -0.0901(3) -0.1472(4) 0.04439(6) 0.1237(13) Uani 1 1 d . . . H1 H -0.0589 -0.1168 0.0214 0.186 Uiso 1 1 calc R . . C1 C -0.3496(2) -0.3469(3) 0.16496(6) 0.0343(4) Uani 1 1 d . . . C2 C -0.2480(2) -0.4629(3) 0.16091(7) 0.0403(5) Uani 1 1 d . . . C3 C -0.1421(2) -0.3896(3) 0.14102(7) 0.0394(5) Uani 1 1 d . . . C4 C -0.1626(2) -0.2187(3) 0.13019(6) 0.0364(4) Uani 1 1 d . . . C5 C -0.0568(2) -0.1045(3) 0.11925(7) 0.0398(5) Uani 1 1 d . . . C6 C -0.0250(3) -0.0744(4) 0.07815(8) 0.0664(8) Uani 1 1 d . . . C7 C 0.0766(3) 0.0320(5) 0.06857(9) 0.0843(11) Uani 1 1 d . . . H7 H 0.0970 0.0487 0.0396 0.101 Uiso 1 1 calc R . . C8 C 0.1444(3) 0.1096(4) 0.10051(9) 0.0691(9) Uani 1 1 d . . . H8 H 0.2122 0.1818 0.0938 0.083 Uiso 1 1 calc R . . C9 C 0.1171(2) 0.0861(3) 0.14391(8) 0.0466(5) Uani 1 1 d . . . C10 C 0.1867(2) 0.1678(3) 0.17809(9) 0.0591(7) Uani 1 1 d . . . H10 H 0.2553 0.2396 0.1719 0.071 Uiso 1 1 calc R . . C11 C 0.1575(3) 0.1459(4) 0.21931(9) 0.0622(7) Uani 1 1 d . . . H11 H 0.2058 0.2015 0.2417 0.075 Uiso 1 1 calc R . . C12 C 0.0562(2) 0.0413(4) 0.22905(8) 0.0581(7) Uani 1 1 d . . . H12 H 0.0352 0.0274 0.2581 0.070 Uiso 1 1 calc R . . C13 C -0.0125(2) -0.0409(3) 0.19706(7) 0.0447(5) Uani 1 1 d . . . H13 H -0.0802 -0.1126 0.2043 0.054 Uiso 1 1 calc R . . C14 C 0.01469(19) -0.0215(3) 0.15351(6) 0.0369(5) Uani 1 1 d . . . C15 C -0.4712(2) -0.3734(2) 0.18623(6) 0.0356(4) Uani 1 1 d . . . C16 C -0.4814(2) -0.4815(3) 0.22060(7) 0.0511(6) Uani 1 1 d . . . H16 H -0.4095 -0.5459 0.2304 0.061 Uiso 1 1 calc R . . C17 C -0.5951(3) -0.4969(4) 0.24085(8) 0.0623(7) Uani 1 1 d . . . H17 H -0.6004 -0.5735 0.2639 0.075 Uiso 1 1 calc R . . C18 C -0.6992(3) -0.4041(4) 0.22822(9) 0.0595(7) Uani 1 1 d . . . H18 H -0.7769 -0.4162 0.2421 0.071 Uiso 1 1 calc R . . C19 C -0.6903(2) -0.2927(4) 0.19505(9) 0.0579(6) Uani 1 1 d . . . H19 H -0.7618 -0.2259 0.1862 0.070 Uiso 1 1 calc R . . C20 C -0.5776(2) -0.2771(3) 0.17446(7) 0.0489(6) Uani 1 1 d . . . H20 H -0.5729 -0.1987 0.1517 0.059 Uiso 1 1 calc R . . C21 C -0.2453(3) -0.6410(3) 0.17668(9) 0.0604(7) Uani 1 1 d . . . H21A H -0.2159 -0.6435 0.2071 0.091 Uiso 1 1 calc R . . H21B H -0.1869 -0.7065 0.1599 0.091 Uiso 1 1 calc R . . H21C H -0.3313 -0.6886 0.1732 0.091 Uiso 1 1 calc R . . C22 C -0.0177(2) -0.4769(4) 0.13443(10) 0.0655(8) Uani 1 1 d . . . H22A H 0.0209 -0.4301 0.1092 0.098 Uiso 1 1 calc R . . H22B H -0.0334 -0.5964 0.1299 0.098 Uiso 1 1 calc R . . H22C H 0.0405 -0.4611 0.1599 0.098 Uiso 1 1 calc R . . C23 C -0.4706(3) -0.3707(5) 0.05974(8) 0.0737(10) Uani 1 1 d . . . C24 C -0.3653(3) -0.3330(4) 0.03564(7) 0.0534(6) Uani 1 1 d . . . C25 C -0.2795(3) -0.4685(3) 0.03818(7) 0.0520(6) Uani 1 1 d . . . C26 C -0.3315(4) -0.5932(4) 0.06430(9) 0.0769(10) Uani 1 1 d . . . C27 C -0.4514(3) -0.5316(5) 0.07729(9) 0.0877(13) Uani 1 1 d . . . C28 C -0.5881(3) -0.2629(9) 0.06158(11) 0.150(3) Uani 1 1 d . . . H28A H -0.5639 -0.1532 0.0733 0.225 Uiso 1 1 calc R . . H28B H -0.6487 -0.3160 0.0801 0.225 Uiso 1 1 calc R . . H28C H -0.6280 -0.2497 0.0326 0.225 Uiso 1 1 calc R . . C29 C -0.3620(4) -0.1825(5) 0.00657(9) 0.0836(10) Uani 1 1 d . . . H29A H -0.3706 -0.0807 0.0236 0.125 Uiso 1 1 calc R . . H29B H -0.4326 -0.1890 -0.0154 0.125 Uiso 1 1 calc R . . H29C H -0.2807 -0.1800 -0.0074 0.125 Uiso 1 1 calc R . . C30 C -0.1619(3) -0.4922(5) 0.01309(10) 0.0825(10) Uani 1 1 d . . . H30A H -0.1419 -0.3876 -0.0014 0.124 Uiso 1 1 calc R . . H30B H -0.1777 -0.5802 -0.0084 0.124 Uiso 1 1 calc R . . H30C H -0.0898 -0.5242 0.0328 0.124 Uiso 1 1 calc R . . C31 C -0.2730(7) -0.7621(4) 0.07191(13) 0.153(3) Uani 1 1 d . . . H31A H -0.3265 -0.8277 0.0904 0.230 Uiso 1 1 calc R . . H31B H -0.1875 -0.7495 0.0860 0.230 Uiso 1 1 calc R . . H31C H -0.2667 -0.8196 0.0444 0.230 Uiso 1 1 calc R . . C32 C -0.5440(5) -0.6301(7) 0.10315(12) 0.162(3) Uani 1 1 d . . . H32A H -0.6048 -0.6891 0.0835 0.243 Uiso 1 1 calc R . . H32B H -0.5903 -0.5536 0.1212 0.243 Uiso 1 1 calc R . . H32C H -0.4965 -0.7111 0.1214 0.243 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.03697(19) 0.03547(18) 0.03044(17) -0.00162(11) 0.00594(12) -0.00708(12) P1 0.0437(3) 0.0321(3) 0.0370(3) 0.0009(2) 0.0123(2) -0.0045(2) O1 0.153(2) 0.186(3) 0.0337(10) -0.0160(13) 0.0198(12) -0.124(2) C1 0.0377(11) 0.0368(11) 0.0287(9) 0.0028(8) 0.0047(8) -0.0053(8) C2 0.0429(12) 0.0386(11) 0.0395(11) 0.0095(9) 0.0025(9) -0.0014(9) C3 0.0347(11) 0.0457(12) 0.0379(11) 0.0067(9) 0.0018(9) 0.0003(9) C4 0.0393(11) 0.0389(11) 0.0310(10) -0.0010(8) 0.0041(8) -0.0090(9) C5 0.0377(11) 0.0434(12) 0.0391(11) 0.0003(9) 0.0099(9) -0.0105(9) C6 0.0758(19) 0.085(2) 0.0390(12) -0.0044(13) 0.0107(12) -0.0442(16) C7 0.091(2) 0.117(3) 0.0470(14) -0.0022(16) 0.0226(15) -0.063(2) C8 0.0646(17) 0.082(2) 0.0624(17) 0.0007(14) 0.0166(14) -0.0418(16) C9 0.0384(12) 0.0468(13) 0.0550(13) -0.0022(10) 0.0053(10) -0.0099(10) C10 0.0465(14) 0.0597(16) 0.0706(18) -0.0098(13) -0.0012(13) -0.0175(12) C11 0.0522(15) 0.0707(18) 0.0623(17) -0.0189(13) -0.0091(13) -0.0099(13) C12 0.0502(15) 0.0790(19) 0.0448(13) -0.0085(13) 0.0006(11) -0.0050(13) C13 0.0381(12) 0.0552(14) 0.0409(11) -0.0005(10) 0.0036(9) -0.0050(10) C14 0.0329(11) 0.0371(11) 0.0412(11) -0.0016(9) 0.0054(9) -0.0002(8) C15 0.0393(11) 0.0377(11) 0.0305(9) -0.0015(8) 0.0072(8) -0.0080(8) C16 0.0499(14) 0.0585(15) 0.0458(13) 0.0123(11) 0.0091(11) -0.0044(11) C17 0.0676(18) 0.0684(18) 0.0534(14) 0.0139(13) 0.0239(13) -0.0138(14) C18 0.0545(16) 0.0639(17) 0.0633(16) -0.0091(13) 0.0290(13) -0.0166(13) C19 0.0450(14) 0.0641(17) 0.0660(16) -0.0039(13) 0.0148(12) 0.0025(12) C20 0.0483(13) 0.0522(14) 0.0472(12) 0.0055(11) 0.0126(10) 0.0009(11) C21 0.0644(17) 0.0447(14) 0.0733(17) 0.0237(12) 0.0153(14) 0.0060(12) C22 0.0451(14) 0.0734(19) 0.0790(19) 0.0171(15) 0.0119(13) 0.0128(13) C23 0.0430(15) 0.140(3) 0.0374(13) -0.0157(16) -0.0001(11) -0.0211(17) C24 0.0552(15) 0.0740(18) 0.0306(11) -0.0073(11) 0.0001(10) -0.0108(13) C25 0.0647(16) 0.0526(15) 0.0400(11) -0.0147(10) 0.0155(11) -0.0168(12) C26 0.135(3) 0.0489(16) 0.0485(15) -0.0164(12) 0.0228(17) -0.0386(18) C27 0.095(2) 0.127(3) 0.0436(14) -0.0276(18) 0.0209(16) -0.081(2) C28 0.049(2) 0.338(8) 0.061(2) -0.009(3) -0.0120(16) 0.047(3) C29 0.112(3) 0.094(2) 0.0432(14) 0.0098(15) -0.0100(16) 0.012(2) C30 0.094(2) 0.089(2) 0.0688(18) -0.0226(17) 0.0374(17) 0.0008(19) C31 0.336(8) 0.0365(18) 0.093(3) -0.0179(18) 0.050(4) -0.015(3) C32 0.186(5) 0.234(6) 0.071(2) -0.056(3) 0.055(3) -0.183(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C27 2.057(3) . ? Fe1 C23 2.068(3) . ? Fe1 C26 2.076(3) . ? Fe1 C2 2.080(2) . ? Fe1 C3 2.093(2) . ? Fe1 C24 2.093(2) . ? Fe1 C25 2.102(2) . ? Fe1 C1 2.109(2) . ? Fe1 C4 2.145(2) . ? Fe1 P1 2.2959(6) . ? P1 C4 1.771(2) . ? P1 C1 1.793(2) . ? O1 C6 1.353(3) . ? C1 C2 1.426(3) . ? C1 C15 1.487(3) . ? C2 C3 1.429(3) . ? C2 C21 1.509(3) . ? C3 C4 1.423(3) . ? C3 C22 1.506(3) . ? C4 C5 1.494(3) . ? C5 C6 1.364(3) . ? C5 C14 1.432(3) . ? C6 C7 1.410(4) . ? C7 C8 1.342(4) . ? C8 C9 1.411(4) . ? C9 C10 1.417(3) . ? C9 C14 1.423(3) . ? C10 C11 1.349(4) . ? C11 C12 1.401(4) . ? C12 C13 1.365(3) . ? C13 C14 1.412(3) . ? C15 C16 1.387(3) . ? C15 C20 1.389(3) . ? C16 C17 1.387(3) . ? C17 C18 1.360(4) . ? C18 C19 1.373(4) . ? C19 C20 1.383(3) . ? C23 C24 1.404(4) . ? C23 C27 1.410(5) . ? C23 C28 1.509(5) . ? C24 C25 1.410(4) . ? C24 C29 1.510(4) . ? C25 C26 1.418(4) . ? C25 C30 1.510(4) . ? C26 C27 1.432(5) . ? C26 C31 1.499(5) . ? C27 C32 1.518(4) . ? 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 C27 Fe1 C23 39.98(15) . . ? C27 Fe1 C26 40.54(15) . . ? C23 Fe1 C26 67.54(15) . . ? C27 Fe1 C2 106.64(12) . . ? C23 Fe1 C2 138.92(11) . . ? C26 Fe1 C2 103.29(11) . . ? C27 Fe1 C3 138.20(15) . . ? C23 Fe1 C3 178.16(13) . . ? C26 Fe1 C3 110.86(13) . . ? C2 Fe1 C3 40.06(8) . . ? C27 Fe1 C24 66.43(12) . . ? C23 Fe1 C24 39.44(11) . . ? C26 Fe1 C24 66.57(12) . . ? C2 Fe1 C24 169.83(10) . . ? C3 Fe1 C24 141.13(9) . . ? C27 Fe1 C25 66.85(10) . . ? C23 Fe1 C25 66.60(11) . . ? C26 Fe1 C25 39.68(10) . . ? C2 Fe1 C25 131.95(10) . . ? C3 Fe1 C25 112.83(10) . . ? C24 Fe1 C25 39.27(11) . . ? C27 Fe1 C1 101.87(10) . . ? C23 Fe1 C1 111.49(10) . . ? C26 Fe1 C1 125.55(10) . . ? C2 Fe1 C1 39.79(8) . . ? C3 Fe1 C1 68.58(8) . . ? C24 Fe1 C1 146.66(10) . . ? C25 Fe1 C1 165.21(9) . . ? C27 Fe1 C4 174.25(9) . . ? C23 Fe1 C4 142.60(12) . . ? C26 Fe1 C4 142.20(13) . . ? C2 Fe1 C4 68.42(8) . . ? C3 Fe1 C4 39.23(8) . . ? C24 Fe1 C4 118.87(9) . . ? C25 Fe1 C4 118.52(9) . . ? C1 Fe1 C4 72.48(8) . . ? C27 Fe1 P1 129.98(12) . . ? C23 Fe1 P1 106.71(10) . . ? C26 Fe1 P1 170.09(11) . . ? C2 Fe1 P1 75.49(7) . . ? C3 Fe1 P1 74.74(6) . . ? C24 Fe1 P1 114.62(8) . . ? C25 Fe1 P1 146.84(7) . . ? C1 Fe1 P1 47.80(6) . . ? C4 Fe1 P1 46.85(6) . . ? C4 P1 C1 89.77(10) . . ? C4 P1 Fe1 62.08(7) . . ? C1 P1 Fe1 60.62(7) . . ? C2 C1 C15 127.73(18) . . ? C2 C1 P1 112.54(15) . . ? C15 C1 P1 119.64(15) . . ? C2 C1 Fe1 69.03(12) . . ? C15 C1 Fe1 130.26(14) . . ? P1 C1 Fe1 71.58(7) . . ? C1 C2 C3 112.00(18) . . ? C1 C2 C21 126.0(2) . . ? C3 C2 C21 122.0(2) . . ? C1 C2 Fe1 71.18(11) . . ? C3 C2 Fe1 70.45(12) . . ? C21 C2 Fe1 127.76(18) . . ? C4 C3 C2 112.78(19) . . ? C4 C3 C22 122.4(2) . . ? C2 C3 C22 124.7(2) . . ? C4 C3 Fe1 72.35(12) . . ? C2 C3 Fe1 69.49(12) . . ? C22 C3 Fe1 129.35(18) . . ? C3 C4 C5 122.6(2) . . ? C3 C4 P1 112.90(15) . . ? C5 C4 P1 122.78(16) . . ? C3 C4 Fe1 68.42(12) . . ? C5 C4 Fe1 140.89(14) . . ? P1 C4 Fe1 71.07(7) . . ? C6 C5 C14 118.2(2) . . ? C6 C5 C4 123.2(2) . . ? C14 C5 C4 118.56(18) . . ? O1 C6 C5 120.9(2) . . ? O1 C6 C7 116.7(2) . . ? C5 C6 C7 122.3(2) . . ? C8 C7 C6 119.9(2) . . ? C7 C8 C9 121.3(2) . . ? C8 C9 C10 122.3(2) . . ? C8 C9 C14 118.7(2) . . ? C10 C9 C14 119.0(2) . . ? C11 C10 C9 121.4(2) . . ? C10 C11 C12 120.1(2) . . ? C13 C12 C11 120.4(2) . . ? C12 C13 C14 121.4(2) . . ? C13 C14 C9 117.8(2) . . ? C13 C14 C5 122.65(19) . . ? C9 C14 C5 119.56(19) . . ? C16 C15 C20 117.0(2) . . ? C16 C15 C1 122.7(2) . . ? C20 C15 C1 120.02(18) . . ? C15 C16 C17 120.9(2) . . ? C18 C17 C16 121.1(2) . . ? C17 C18 C19 119.0(2) . . ? C18 C19 C20 120.4(3) . . ? C19 C20 C15 121.5(2) . . ? C24 C23 C27 107.7(3) . . ? C24 C23 C28 124.5(4) . . ? C27 C23 C28 127.4(4) . . ? C24 C23 Fe1 71.24(15) . . ? C27 C23 Fe1 69.57(17) . . ? C28 C23 Fe1 129.7(2) . . ? C23 C24 C25 108.9(3) . . ? C23 C24 C29 122.6(3) . . ? C25 C24 C29 127.7(3) . . ? C23 C24 Fe1 69.32(14) . . ? C25 C24 Fe1 70.71(14) . . ? C29 C24 Fe1 133.7(2) . . ? C24 C25 C26 108.0(3) . . ? C24 C25 C30 127.3(3) . . ? C26 C25 C30 124.2(3) . . ? C24 C25 Fe1 70.02(13) . . ? C26 C25 Fe1 69.14(14) . . ? C30 C25 Fe1 132.8(2) . . ? C25 C26 C27 107.0(3) . . ? C25 C26 C31 124.0(4) . . ? C27 C26 C31 128.7(4) . . ? C25 C26 Fe1 71.18(14) . . ? C27 C26 Fe1 69.03(16) . . ? C31 C26 Fe1 129.4(3) . . ? C23 C27 C26 108.3(2) . . ? C23 C27 C32 126.8(4) . . ? C26 C27 C32 124.8(4) . . ? C23 C27 Fe1 70.45(15) . . ? C26 C27 Fe1 70.43(15) . . ? C32 C27 Fe1 127.8(2) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.408 _refine_diff_density_min -0.360 _refine_diff_density_rms 0.052 #END==== data_ptru _database_code_depnum_ccdc_archive 'CCDC 258044' #compound 12 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H52 Cl8 O P2 Pt Ru' _chemical_formula_weight 1202.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P21/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.809(5) _cell_length_b 24.651(5) _cell_length_c 19.909(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 91.420(5) _cell_angle_gamma 90.000(5) _cell_volume 4813(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293.0(10) _cell_measurement_reflns_used 251 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 20.0 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.660 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2376 _exptl_absorpt_coefficient_mu 3.759 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2114 _exptl_absorpt_correction_T_max 0.7050 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293.0(10) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12590 _diffrn_reflns_av_R_equivalents 0.0499 _diffrn_reflns_av_sigmaI/netI 0.0734 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.46 _diffrn_reflns_theta_max 24.40 _reflns_number_total 7527 _reflns_number_gt 5943 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1269P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7527 _refine_ls_number_parameters 462 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0753 _refine_ls_R_factor_gt 0.0584 _refine_ls_wR_factor_ref 0.1796 _refine_ls_wR_factor_gt 0.1573 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.42187(3) 0.138799(14) 0.744004(16) 0.04379(17) Uani 1 1 d . . . Ru1 Ru 0.25248(6) 0.20457(3) 0.55825(3) 0.0427(2) Uani 1 1 d . . . Cl1 Cl 0.6108(2) 0.15835(12) 0.67579(13) 0.0617(6) Uani 1 1 d . . . Cl2 Cl 0.5776(3) 0.10665(13) 0.82589(13) 0.0722(8) Uani 1 1 d . . . P1 P 0.2782(2) 0.16918(9) 0.66541(10) 0.0410(5) Uani 1 1 d . . . P2 P 0.2567(3) 0.11748(12) 0.81526(13) 0.0568(6) Uani 1 1 d . . . O1 O -0.0348(7) 0.2519(3) 0.7413(4) 0.079(2) Uani 1 1 d . . . C1 C 0.1731(8) 0.2281(4) 0.6620(4) 0.045(2) Uani 1 1 d . . . C2 C 0.0651(8) 0.2202(4) 0.6150(4) 0.049(2) Uani 1 1 d . . . C3 C 0.0598(7) 0.1666(4) 0.5862(4) 0.047(2) Uani 1 1 d . . . C4 C 0.1673(8) 0.1325(3) 0.6102(4) 0.0390(19) Uani 1 1 d . . . C5 C 0.1841(9) 0.2748(4) 0.7087(4) 0.051(2) Uani 1 1 d . . . C6 C 0.3047(10) 0.3058(4) 0.7194(4) 0.053(2) Uani 1 1 d . . . C7 C 0.4304(9) 0.2944(4) 0.6889(5) 0.064(3) Uani 1 1 d . . . H7 H 0.4345 0.2658 0.6587 0.076 Uiso 1 1 calc R . . C8 C 0.5427(11) 0.3230(5) 0.7018(5) 0.069(3) Uani 1 1 d . . . H8 H 0.6225 0.3138 0.6803 0.083 Uiso 1 1 calc R . . C9 C 0.5444(18) 0.3665(5) 0.7467(7) 0.090(4) Uani 1 1 d . . . H9 H 0.6243 0.3858 0.7557 0.109 Uiso 1 1 calc R . . C10 C 0.4249(14) 0.3804(5) 0.7774(6) 0.080(3) Uani 1 1 d . . . H10 H 0.4241 0.4099 0.8064 0.096 Uiso 1 1 calc R . . C11 C 0.3047(13) 0.3509(4) 0.7657(5) 0.066(3) Uani 1 1 d . . . C12 C 0.1853(15) 0.3630(5) 0.7980(6) 0.082(4) Uani 1 1 d . . . H12 H 0.1818 0.3938 0.8249 0.099 Uiso 1 1 calc R . . C13 C 0.0735(12) 0.3312(5) 0.7914(6) 0.082(4) Uani 1 1 d . . . H13 H -0.0032 0.3388 0.8164 0.098 Uiso 1 1 calc R . . C14 C 0.0724(10) 0.2864(5) 0.7468(5) 0.065(3) Uani 1 1 d . . . C15 C -0.1503(12) 0.2584(7) 0.7836(7) 0.103(5) Uani 1 1 d . . . H15A H -0.1192 0.2641 0.8292 0.154 Uiso 1 1 calc R . . H15B H -0.2057 0.2263 0.7812 0.154 Uiso 1 1 calc R . . H15C H -0.2032 0.2891 0.7687 0.154 Uiso 1 1 calc R . . C16 C -0.0395(9) 0.2629(4) 0.5977(5) 0.062(3) Uani 1 1 d . . . H16A H -0.1217 0.2555 0.6213 0.094 Uiso 1 1 calc R . . H16B H -0.0586 0.2624 0.5502 0.094 Uiso 1 1 calc R . . H16C H -0.0050 0.2979 0.6107 0.094 Uiso 1 1 calc R . . C17 C -0.0539(10) 0.1495(4) 0.5403(5) 0.064(3) Uani 1 1 d . . . H17A H -0.0272 0.1179 0.5157 0.096 Uiso 1 1 calc R . . H17B H -0.0756 0.1783 0.5095 0.096 Uiso 1 1 calc R . . H17C H -0.1326 0.1411 0.5662 0.096 Uiso 1 1 calc R . . C18 C 0.1869(8) 0.0740(4) 0.5942(4) 0.0430(19) Uani 1 1 d . . . C19 C 0.3169(9) 0.0531(4) 0.5836(4) 0.050(2) Uani 1 1 d . . . H19 H 0.3923 0.0759 0.5865 0.060 Uiso 1 1 calc R . . C20 C 0.3344(10) -0.0006(4) 0.5690(5) 0.056(2) Uani 1 1 d . . . H20 H 0.4212 -0.0141 0.5615 0.068 Uiso 1 1 calc R . . C21 C 0.2217(9) -0.0348(4) 0.5653(4) 0.053(2) Uani 1 1 d . . . H21 H 0.2330 -0.0714 0.5553 0.063 Uiso 1 1 calc R . . C22 C 0.0955(10) -0.0147(4) 0.5762(5) 0.058(2) Uani 1 1 d . . . H22 H 0.0204 -0.0378 0.5736 0.070 Uiso 1 1 calc R . . C23 C 0.0772(8) 0.0386(4) 0.5908(4) 0.052(2) Uani 1 1 d . . . H23 H -0.0101 0.0516 0.5987 0.062 Uiso 1 1 calc R . . C24 C 0.4277(11) 0.2441(5) 0.5110(5) 0.067(3) Uani 1 1 d . . . C25 C 0.3094(12) 0.2733(4) 0.4912(5) 0.069(3) Uani 1 1 d . . . C26 C 0.2221(11) 0.2350(5) 0.4545(5) 0.068(3) Uani 1 1 d . . . C27 C 0.2852(9) 0.1841(4) 0.4531(4) 0.052(2) Uani 1 1 d . . . C28 C 0.4132(9) 0.1893(4) 0.4867(4) 0.055(2) Uani 1 1 d . . . C29 C 0.5570(13) 0.2680(7) 0.5384(7) 0.110(5) Uani 1 1 d . . . H29A H 0.6136 0.2785 0.5020 0.164 Uiso 1 1 calc R . . H29B H 0.6041 0.2416 0.5658 0.164 Uiso 1 1 calc R . . H29C H 0.5366 0.2993 0.5651 0.164 Uiso 1 1 calc R . . C30 C 0.2822(18) 0.3299(5) 0.5032(8) 0.129(6) Uani 1 1 d . . . H30A H 0.2314 0.3336 0.5436 0.193 Uiso 1 1 calc R . . H30B H 0.2302 0.3446 0.4660 0.193 Uiso 1 1 calc R . . H30C H 0.3668 0.3492 0.5082 0.193 Uiso 1 1 calc R . . C31 C 0.0869(14) 0.2489(8) 0.4190(7) 0.126(6) Uani 1 1 d . . . H31A H 0.1027 0.2570 0.3727 0.189 Uiso 1 1 calc R . . H31B H 0.0471 0.2799 0.4402 0.189 Uiso 1 1 calc R . . H31C H 0.0260 0.2185 0.4218 0.189 Uiso 1 1 calc R . . C32 C 0.2373(14) 0.1349(5) 0.4185(6) 0.087(4) Uani 1 1 d . . . H32A H 0.1423 0.1386 0.4066 0.130 Uiso 1 1 calc R . . H32B H 0.2498 0.1042 0.4477 0.130 Uiso 1 1 calc R . . H32C H 0.2885 0.1296 0.3785 0.130 Uiso 1 1 calc R . . C33 C 0.5261(12) 0.1476(5) 0.4892(6) 0.087(4) Uani 1 1 d . . . H33A H 0.5861 0.1535 0.4525 0.131 Uiso 1 1 calc R . . H33B H 0.4874 0.1119 0.4857 0.131 Uiso 1 1 calc R . . H33C H 0.5765 0.1508 0.5309 0.131 Uiso 1 1 calc R . . C34 C 0.2516(12) 0.2168(5) 0.8797(6) 0.082(3) Uani 1 1 d . . . H34A H 0.3154 0.2300 0.8477 0.124 Uiso 1 1 calc R . . H34B H 0.2644 0.2359 0.9214 0.124 Uiso 1 1 calc R . . H34C H 0.1603 0.2225 0.8627 0.124 Uiso 1 1 calc R . . C35 C 0.2744(11) 0.1577(6) 0.8910(5) 0.072(3) Uani 1 1 d . . . H35A H 0.2097 0.1447 0.9234 0.087 Uiso 1 1 calc R . . H35B H 0.3653 0.1524 0.9102 0.087 Uiso 1 1 calc R . . C36 C 0.2664(12) 0.0475(5) 0.8419(6) 0.080(3) Uani 1 1 d . . . H36A H 0.3569 0.0406 0.8607 0.097 Uiso 1 1 calc R . . H36B H 0.2018 0.0418 0.8773 0.097 Uiso 1 1 calc R . . C37 C 0.2370(13) 0.0061(6) 0.7860(8) 0.106(5) Uani 1 1 d . . . H37A H 0.1419 -0.0031 0.7853 0.159 Uiso 1 1 calc R . . H37B H 0.2904 -0.0259 0.7941 0.159 Uiso 1 1 calc R . . H37C H 0.2602 0.0215 0.7435 0.159 Uiso 1 1 calc R . . C38 C 0.0811(9) 0.1276(5) 0.7865(6) 0.068(3) Uani 1 1 d . . . H38A H 0.0715 0.1646 0.7702 0.081 Uiso 1 1 calc R . . H38B H 0.0624 0.1035 0.7489 0.081 Uiso 1 1 calc R . . C39 C -0.0265(10) 0.1177(7) 0.8402(6) 0.101(5) Uani 1 1 d . . . H39A H -0.0584 0.0809 0.8371 0.152 Uiso 1 1 calc R . . H39B H -0.1017 0.1421 0.8330 0.152 Uiso 1 1 calc R . . H39C H 0.0136 0.1239 0.8840 0.152 Uiso 1 1 calc R . . C40 C 0.6875(9) 0.0192(4) 0.6902(5) 0.065(3) Uani 1 1 d . . . H40 H 0.6485 0.0541 0.7035 0.078 Uiso 1 1 calc R . . Cl3 Cl 0.8487(3) 0.01095(16) 0.73068(18) 0.0977(10) Uani 1 1 d . . . Cl4 Cl 0.5805(4) -0.03357(18) 0.7165(2) 0.1102(12) Uani 1 1 d . . . Cl5 Cl 0.7035(3) 0.01813(14) 0.60347(15) 0.0801(8) 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 Pt1 0.0308(2) 0.0508(3) 0.0497(3) -0.00846(14) 0.00090(16) -0.00030(13) Ru1 0.0363(4) 0.0417(4) 0.0502(4) -0.0056(3) 0.0034(3) 0.0041(3) Cl1 0.0367(11) 0.0738(17) 0.0751(16) 0.0032(13) 0.0098(11) 0.0004(11) Cl2 0.0535(14) 0.098(2) 0.0644(15) -0.0027(14) -0.0134(12) 0.0121(13) P1 0.0330(10) 0.0426(13) 0.0473(12) -0.0090(9) 0.0021(9) -0.0002(9) P2 0.0440(13) 0.0704(18) 0.0562(14) -0.0055(12) 0.0062(11) -0.0063(12) O1 0.056(4) 0.090(6) 0.092(5) -0.041(4) 0.025(4) 0.002(4) C1 0.034(4) 0.048(5) 0.055(5) -0.005(4) 0.007(4) 0.003(4) C2 0.030(4) 0.058(6) 0.057(5) -0.010(4) -0.004(4) 0.010(4) C3 0.022(4) 0.061(6) 0.057(5) -0.005(4) 0.003(4) 0.006(4) C4 0.033(4) 0.049(5) 0.036(4) -0.008(3) 0.004(3) -0.002(3) C5 0.044(5) 0.053(6) 0.055(5) -0.014(4) 0.001(4) 0.013(4) C6 0.062(6) 0.041(5) 0.056(5) -0.007(4) -0.006(4) 0.008(4) C7 0.052(6) 0.063(7) 0.075(6) -0.017(5) -0.010(5) -0.005(5) C8 0.064(6) 0.069(8) 0.074(7) -0.013(6) 0.000(5) -0.007(5) C9 0.107(11) 0.062(9) 0.102(10) -0.007(6) -0.027(9) -0.023(7) C10 0.102(10) 0.055(7) 0.082(8) -0.024(6) -0.013(7) -0.012(7) C11 0.095(8) 0.044(6) 0.059(6) -0.011(5) -0.003(6) 0.010(5) C12 0.103(10) 0.062(8) 0.082(8) -0.035(6) -0.017(7) 0.022(7) C13 0.076(8) 0.097(10) 0.073(7) -0.042(7) 0.006(6) 0.021(7) C14 0.064(7) 0.062(7) 0.069(6) -0.022(5) 0.007(5) 0.013(5) C15 0.068(8) 0.141(14) 0.100(9) -0.039(9) 0.029(7) 0.007(8) C16 0.050(5) 0.057(7) 0.080(7) -0.013(5) -0.011(5) 0.018(4) C17 0.047(5) 0.074(7) 0.071(6) -0.012(5) -0.007(5) 0.005(5) C18 0.031(4) 0.050(5) 0.047(4) -0.004(4) -0.008(3) -0.004(4) C19 0.053(5) 0.041(5) 0.056(5) -0.007(4) 0.005(4) 0.000(4) C20 0.058(6) 0.048(6) 0.064(6) -0.009(4) 0.004(5) 0.008(4) C21 0.059(6) 0.038(5) 0.061(5) -0.003(4) -0.013(5) -0.003(4) C22 0.056(6) 0.042(6) 0.076(6) 0.006(5) -0.006(5) -0.014(4) C23 0.035(4) 0.061(7) 0.059(5) 0.001(4) 0.002(4) -0.003(4) C24 0.071(7) 0.067(7) 0.063(6) -0.003(5) 0.021(5) -0.019(5) C25 0.094(8) 0.044(6) 0.071(7) 0.009(5) 0.032(6) 0.009(6) C26 0.083(7) 0.068(8) 0.052(6) 0.014(5) 0.011(5) 0.018(6) C27 0.049(5) 0.067(7) 0.041(5) 0.003(4) 0.008(4) 0.001(5) C28 0.055(6) 0.057(6) 0.054(5) 0.009(4) 0.012(4) 0.011(4) C29 0.085(9) 0.145(14) 0.100(9) -0.017(9) 0.040(7) -0.059(9) C30 0.215(19) 0.050(9) 0.123(12) 0.026(8) 0.061(12) 0.012(10) C31 0.084(9) 0.197(18) 0.097(9) 0.076(11) 0.005(7) 0.053(10) C32 0.092(9) 0.102(11) 0.068(7) -0.020(6) 0.031(7) -0.028(7) C33 0.066(7) 0.122(11) 0.075(8) 0.011(7) 0.014(6) 0.043(7) C34 0.085(8) 0.094(10) 0.069(7) -0.022(6) 0.015(6) -0.015(7) C35 0.058(6) 0.103(10) 0.057(6) -0.005(6) 0.004(5) -0.004(6) C36 0.074(7) 0.091(9) 0.077(7) 0.015(6) 0.016(6) -0.016(6) C37 0.068(8) 0.084(10) 0.164(14) -0.020(9) -0.005(8) -0.006(7) C38 0.038(5) 0.094(9) 0.071(7) -0.014(6) 0.005(4) -0.011(5) C39 0.027(5) 0.195(15) 0.082(8) -0.008(9) 0.021(5) -0.012(7) C40 0.043(5) 0.068(7) 0.085(7) -0.006(5) 0.019(5) 0.006(5) Cl3 0.0659(18) 0.123(3) 0.104(2) 0.011(2) -0.0155(17) -0.0014(18) Cl4 0.082(2) 0.126(3) 0.124(3) 0.011(2) 0.0235(19) -0.037(2) Cl5 0.0566(15) 0.098(2) 0.0863(18) -0.0060(16) 0.0100(13) -0.0078(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P1 2.210(2) . ? Pt1 P2 2.242(3) . ? Pt1 Cl2 2.344(2) . ? Pt1 Cl1 2.374(2) . ? Ru1 C28 2.183(9) . ? Ru1 C27 2.185(8) . ? Ru1 C3 2.192(8) . ? Ru1 C24 2.207(10) . ? Ru1 C26 2.210(9) . ? Ru1 C2 2.215(8) . ? Ru1 C4 2.228(8) . ? Ru1 C25 2.237(10) . ? Ru1 C1 2.300(8) . ? Ru1 P1 2.313(2) . ? P1 C4 1.775(8) . ? P1 C1 1.782(8) . ? P2 C36 1.808(13) . ? P2 C35 1.809(11) . ? P2 C38 1.819(10) . ? O1 C14 1.354(13) . ? O1 C15 1.438(12) . ? C1 C2 1.410(11) . ? C1 C5 1.481(12) . ? C2 C3 1.440(13) . ? C2 C16 1.503(12) . ? C3 C4 1.422(11) . ? C3 C17 1.485(12) . ? C4 C18 1.491(12) . ? C5 C14 1.379(12) . ? C5 C6 1.420(13) . ? C6 C7 1.416(13) . ? C6 C11 1.444(13) . ? C7 C8 1.327(14) . ? C8 C9 1.396(16) . ? C9 C10 1.378(19) . ? C10 C11 1.400(17) . ? C11 C12 1.383(18) . ? C12 C13 1.351(17) . ? C13 C14 1.417(15) . ? C18 C23 1.385(11) . ? C18 C19 1.396(12) . ? C19 C20 1.366(12) . ? C20 C21 1.392(13) . ? C21 C22 1.356(13) . ? C22 C23 1.361(13) . ? C24 C25 1.413(15) . ? C24 C28 1.440(14) . ? C24 C29 1.490(15) . ? C25 C30 1.442(17) . ? C25 C26 1.458(16) . ? C26 C27 1.398(14) . ? C26 C31 1.526(15) . ? C27 C28 1.414(12) . ? C27 C32 1.468(14) . ? C28 C33 1.512(13) . ? C34 C35 1.490(17) . ? C36 C37 1.531(17) . ? C38 C39 1.541(14) . ? C40 Cl5 1.737(11) . ? C40 Cl4 1.760(11) . ? C40 Cl3 1.769(10) . ? 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 P1 Pt1 P2 93.99(9) . . ? P1 Pt1 Cl2 178.91(8) . . ? P2 Pt1 Cl2 87.09(10) . . ? P1 Pt1 Cl1 91.09(9) . . ? P2 Pt1 Cl1 174.92(9) . . ? Cl2 Pt1 Cl1 87.83(10) . . ? C28 Ru1 C27 37.8(3) . . ? C28 Ru1 C3 137.1(4) . . ? C27 Ru1 C3 107.0(3) . . ? C28 Ru1 C24 38.3(4) . . ? C27 Ru1 C24 63.8(4) . . ? C3 Ru1 C24 169.0(4) . . ? C28 Ru1 C26 62.1(4) . . ? C27 Ru1 C26 37.1(4) . . ? C3 Ru1 C26 106.5(4) . . ? C24 Ru1 C26 62.6(4) . . ? C28 Ru1 C2 169.9(3) . . ? C27 Ru1 C2 132.2(3) . . ? C3 Ru1 C2 38.1(3) . . ? C24 Ru1 C2 143.7(4) . . ? C26 Ru1 C2 108.8(4) . . ? C28 Ru1 C4 116.8(3) . . ? C27 Ru1 C4 109.1(3) . . ? C3 Ru1 C4 37.5(3) . . ? C24 Ru1 C4 148.7(4) . . ? C26 Ru1 C4 131.3(4) . . ? C2 Ru1 C4 65.0(3) . . ? C28 Ru1 C25 63.0(4) . . ? C27 Ru1 C25 63.7(4) . . ? C3 Ru1 C25 134.8(4) . . ? C24 Ru1 C25 37.1(4) . . ? C26 Ru1 C25 38.3(4) . . ? C2 Ru1 C25 113.3(4) . . ? C4 Ru1 C25 169.4(4) . . ? C28 Ru1 C1 153.5(3) . . ? C27 Ru1 C1 168.5(3) . . ? C3 Ru1 C1 64.3(3) . . ? C24 Ru1 C1 123.8(3) . . ? C26 Ru1 C1 135.5(3) . . ? C2 Ru1 C1 36.3(3) . . ? C4 Ru1 C1 69.2(3) . . ? C25 Ru1 C1 116.1(3) . . ? C28 Ru1 P1 118.2(2) . . ? C27 Ru1 P1 141.4(3) . . ? C3 Ru1 P1 71.4(2) . . ? C24 Ru1 P1 119.4(3) . . ? C26 Ru1 P1 177.3(3) . . ? C2 Ru1 P1 70.6(2) . . ? C4 Ru1 P1 46.0(2) . . ? C25 Ru1 P1 144.4(3) . . ? C1 Ru1 P1 45.4(2) . . ? C4 P1 C1 92.6(4) . . ? C4 P1 Pt1 129.5(3) . . ? C1 P1 Pt1 131.4(3) . . ? C4 P1 Ru1 64.5(3) . . ? C1 P1 Ru1 66.9(3) . . ? Pt1 P1 Ru1 146.51(10) . . ? C36 P2 C35 106.0(6) . . ? C36 P2 C38 105.4(6) . . ? C35 P2 C38 104.9(5) . . ? C36 P2 Pt1 112.1(4) . . ? C35 P2 Pt1 110.1(4) . . ? C38 P2 Pt1 117.5(4) . . ? C14 O1 C15 120.3(8) . . ? C2 C1 C5 124.5(7) . . ? C2 C1 P1 109.7(6) . . ? C5 C1 P1 125.2(6) . . ? C2 C1 Ru1 68.5(5) . . ? C5 C1 Ru1 137.6(6) . . ? P1 C1 Ru1 67.7(3) . . ? C1 C2 C3 114.2(7) . . ? C1 C2 C16 123.5(8) . . ? C3 C2 C16 122.2(7) . . ? C1 C2 Ru1 75.1(5) . . ? C3 C2 Ru1 70.1(4) . . ? C16 C2 Ru1 125.1(7) . . ? C4 C3 C2 112.9(7) . . ? C4 C3 C17 125.3(8) . . ? C2 C3 C17 121.7(7) . . ? C4 C3 Ru1 72.6(4) . . ? C2 C3 Ru1 71.8(5) . . ? C17 C3 Ru1 127.2(7) . . ? C3 C4 C18 126.8(7) . . ? C3 C4 P1 110.2(6) . . ? C18 C4 P1 123.0(6) . . ? C3 C4 Ru1 69.9(5) . . ? C18 C4 Ru1 128.4(5) . . ? P1 C4 Ru1 69.5(3) . . ? C14 C5 C6 118.4(8) . . ? C14 C5 C1 117.4(8) . . ? C6 C5 C1 124.1(8) . . ? C7 C6 C5 124.1(8) . . ? C7 C6 C11 116.1(9) . . ? C5 C6 C11 119.8(9) . . ? C8 C7 C6 122.6(10) . . ? C7 C8 C9 121.9(12) . . ? C10 C9 C8 118.5(12) . . ? C9 C10 C11 121.3(11) . . ? C12 C11 C10 122.0(10) . . ? C12 C11 C6 118.4(11) . . ? C10 C11 C6 119.5(11) . . ? C13 C12 C11 121.6(10) . . ? C12 C13 C14 120.4(10) . . ? O1 C14 C5 116.8(8) . . ? O1 C14 C13 122.3(9) . . ? C5 C14 C13 120.9(10) . . ? C23 C18 C19 118.2(8) . . ? C23 C18 C4 121.0(7) . . ? C19 C18 C4 120.8(7) . . ? C20 C19 C18 120.6(9) . . ? C19 C20 C21 119.7(9) . . ? C22 C21 C20 119.8(9) . . ? C21 C22 C23 120.9(8) . . ? C22 C23 C18 120.8(8) . . ? C25 C24 C28 108.1(9) . . ? C25 C24 C29 125.9(12) . . ? C28 C24 C29 124.7(11) . . ? C25 C24 Ru1 72.6(6) . . ? C28 C24 Ru1 70.0(5) . . ? C29 C24 Ru1 133.1(8) . . ? C24 C25 C30 126.9(13) . . ? C24 C25 C26 106.1(9) . . ? C30 C25 C26 126.9(12) . . ? C24 C25 Ru1 70.3(6) . . ? C30 C25 Ru1 125.7(8) . . ? C26 C25 Ru1 69.9(5) . . ? C27 C26 C25 109.6(9) . . ? C27 C26 C31 124.9(12) . . ? C25 C26 C31 125.4(12) . . ? C27 C26 Ru1 70.5(5) . . ? C25 C26 Ru1 71.8(5) . . ? C31 C26 Ru1 127.2(8) . . ? C26 C27 C28 107.3(9) . . ? C26 C27 C32 127.9(10) . . ? C28 C27 C32 124.6(10) . . ? C26 C27 Ru1 72.4(5) . . ? C28 C27 Ru1 71.0(5) . . ? C32 C27 Ru1 126.0(7) . . ? C27 C28 C24 108.8(9) . . ? C27 C28 C33 126.5(10) . . ? C24 C28 C33 124.2(10) . . ? C27 C28 Ru1 71.2(5) . . ? C24 C28 Ru1 71.8(5) . . ? C33 C28 Ru1 129.5(7) . . ? C34 C35 P2 113.5(8) . . ? C37 C36 P2 114.5(9) . . ? C39 C38 P2 114.8(8) . . ? Cl5 C40 Cl4 110.7(6) . . ? Cl5 C40 Cl3 110.5(5) . . ? Cl4 C40 Cl3 108.2(6) . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 24.40 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 2.506 _refine_diff_density_min -2.331 _refine_diff_density_rms 0.185 #END====