# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2000 # CCDC Number: 440/180 data_4 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common - _chemical_formula_moiety 'C31 H27 N O P2 Se2' _chemical_formula_structural 'C31 H27 N O P2 Se2' _chemical_formula_analytical 'C31 H27 N O P2 Se2' _chemical_formula_sum 'C31 H27 N O P2 Se2' _chemical_formula_weight 649.40 _chemical_melting_point - _chemical_compound_source - 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.7749(3) _cell_length_b 18.8326(3) _cell_length_c 19.4901(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5790.2(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 140 _cell_measurement_theta_min 12 _cell_measurement_theta_max 168 _exptl_crystal_description block _exptl_crystal_colour clear _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.490 _exptl_crystal_density_method - _exptl_crystal_F_000 2608 _exptl_absorpt_coefficient_mu 2.689 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.610351 _exptl_absorpt_correction_T_max 1.000000 _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 SMART _diffrn_measurement_method CCD _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time - _diffrn_standards_decay_% - _diffrn_reflns_number 33146 _diffrn_reflns_av_R_equivalents 0.1059 _diffrn_reflns_av_sigmaI/netI 0.0853 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 28.78 _reflns_number_total 6966 _reflns_number_observed 3758 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 50 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0305P)^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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00113(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6916 _refine_ls_number_parameters 335 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0915 _refine_ls_R_factor_obs 0.0336 _refine_ls_wR_factor_all 0.0786 _refine_ls_wR_factor_obs 0.0611 _refine_ls_goodness_of_fit_all 0.830 _refine_ls_goodness_of_fit_obs 0.951 _refine_ls_restrained_S_all 0.885 _refine_ls_restrained_S_obs 0.951 _refine_ls_shift/esd_max 0.007 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Se1 Se 0.45332(2) 0.21358(2) 0.87908(2) 0.06664(12) Uani 1 d . . P1 P 0.32032(4) 0.20429(3) 0.87748(3) 0.0384(2) Uani 1 d . . N1 N 0.28039(10) 0.11916(10) 0.88373(8) 0.0331(4) Uani 1 d . . P2 P 0.29707(4) 0.05273(3) 0.82430(3) 0.0356(2) Uani 1 d . . Se2 Se 0.32922(2) 0.08835(2) 0.725930(13) 0.05744(10) Uani 1 d . . C1 C 0.2714(2) 0.24444(13) 0.80207(12) 0.0427(6) Uani 1 d . . C2 C 0.1899(2) 0.22585(14) 0.78180(13) 0.0490(7) Uani 1 d . . H2A H 0.1603(2) 0.19090(14) 0.80551(13) 0.059 Uiso 1 calc R . C3 C 0.1528(2) 0.2596(2) 0.72601(14) 0.0643(8) Uani 1 d . . H3A H 0.0984(2) 0.2473(2) 0.71217(14) 0.077 Uiso 1 calc R . C4 C 0.1972(3) 0.3116(2) 0.6912(2) 0.0803(10) Uani 1 d . . H4A H 0.1723(3) 0.3341(2) 0.6538(2) 0.096 Uiso 1 calc R . C5 C 0.2776(2) 0.3305(2) 0.71110(15) 0.0723(9) Uani 1 d . . H5A H 0.3067(2) 0.3658(2) 0.68757(15) 0.087 Uiso 1 calc R . C6 C 0.3150(2) 0.29662(13) 0.76651(13) 0.0540(7) Uani 1 d . . H6A H 0.3697(2) 0.30896(13) 0.77987(13) 0.065 Uiso 1 calc R . C7 C 0.2744(2) 0.24963(13) 0.95094(12) 0.0416(6) Uani 1 d . . C8 C 0.1951(2) 0.28147(15) 0.94833(14) 0.0570(7) Uani 1 d . . H8A H 0.1625(2) 0.27721(15) 0.90880(14) 0.068 Uiso 1 calc R . C9 C 0.1636(2) 0.3197(2) 1.00398(15) 0.0715(9) Uani 1 d . . H9A H 0.1103(2) 0.3407(2) 1.00141(15) 0.086 Uiso 1 calc R . C10 C 0.2104(3) 0.3262(2) 1.0617(2) 0.0763(10) Uani 1 d . . H10A H 0.1895(3) 0.3522(2) 1.0986(2) 0.092 Uiso 1 calc R . C11 C 0.2886(3) 0.2949(2) 1.0662(2) 0.0794(10) Uani 1 d . . H11A H 0.3199(3) 0.2991(2) 1.1065(2) 0.095 Uiso 1 calc R . C12 C 0.3214(2) 0.2570(2) 1.01136(14) 0.0609(8) Uani 1 d . . H12A H 0.3748(2) 0.2364(2) 1.01474(14) 0.073 Uiso 1 calc R . C13 C 0.37999(14) -0.00575(13) 0.85604(11) 0.0371(6) Uani 1 d . . C14 C 0.3829(2) -0.07618(13) 0.83395(13) 0.0480(7) Uani 1 d . . H14A H 0.3384(2) -0.09470(13) 0.80832(13) 0.058 Uiso 1 calc R . C15 C 0.4518(2) -0.11868(15) 0.84998(15) 0.0582(7) Uani 1 d . . H15A H 0.4537(2) -0.16545(15) 0.83477(15) 0.070 Uiso 1 calc R . C16 C 0.5181(2) -0.0914(2) 0.88880(14) 0.0590(8) Uani 1 d . . H16A H 0.5639(2) -0.1201(2) 0.90024(14) 0.071 Uiso 1 calc R . C17 C 0.5159(2) -0.0222(2) 0.91017(14) 0.0577(7) Uani 1 d . . H17A H 0.5605(2) -0.0041(2) 0.93596(14) 0.069 Uiso 1 calc R . C18 C 0.44805(15) 0.02082(15) 0.89380(12) 0.0469(6) Uani 1 d . . H18A H 0.44772(15) 0.06794(15) 0.90807(12) 0.056 Uiso 1 calc R . C19 C 0.19902(14) 0.00194(13) 0.82800(12) 0.0396(6) Uani 1 d . . C20 C 0.1355(2) 0.01709(15) 0.78051(13) 0.0566(7) Uani 1 d . . H20A H 0.1453(2) 0.04991(15) 0.74576(13) 0.068 Uiso 1 calc R . C21 C 0.0573(2) -0.0169(2) 0.7851(2) 0.0713(9) Uani 1 d . . H21A H 0.0144(2) -0.0061(2) 0.7540(2) 0.086 Uiso 1 calc R . C22 C 0.0434(2) -0.0665(2) 0.8355(2) 0.0783(10) Uani 1 d . . H22A H -0.0085(2) -0.0897(2) 0.8379(2) 0.094 Uiso 1 calc R . C23 C 0.1058(2) -0.0820(2) 0.8828(2) 0.0632(8) Uani 1 d . . H23A H 0.0958(2) -0.1156(2) 0.9169(2) 0.076 Uiso 1 calc R . C24 C 0.1839(2) -0.04733(13) 0.87950(13) 0.0471(6) Uani 1 d . . H24A H 0.2257(2) -0.05722(13) 0.91175(13) 0.056 Uiso 1 calc R . C25 C 0.23941(14) 0.09674(12) 0.94767(11) 0.0338(5) Uani 1 d . . C26 C 0.15117(14) 0.10212(12) 0.95559(12) 0.0399(6) Uani 1 d . . C27 C 0.1131(2) 0.07531(14) 1.01471(14) 0.0523(7) Uani 1 d . . H27A H 0.0547(2) 0.07897(14) 1.02045(14) 0.063 Uiso 1 calc R . C28 C 0.1617(2) 0.04341(15) 1.06463(14) 0.0584(8) Uani 1 d . . H28A H 0.1356(2) 0.02422(15) 1.10319(14) 0.070 Uiso 1 calc R . C29 C 0.2482(2) 0.03958(14) 1.05824(13) 0.0545(7) Uani 1 d . . H29A H 0.2807(2) 0.01927(14) 1.09285(13) 0.065 Uiso 1 calc R . C30 C 0.2867(2) 0.06627(13) 0.99971(12) 0.0427(6) Uani 1 d . . H30A H 0.3453(2) 0.06364(13) 0.99536(12) 0.051 Uiso 1 calc R . O26 O 0.10813(10) 0.13351(10) 0.90288(9) 0.0523(5) Uani 1 d . . C31 C 0.0183(2) 0.1399(2) 0.9079(2) 0.0935(12) Uani 1 d . . H31A H -0.0033(2) 0.1629(2) 0.8675(2) 0.140 Uiso 1 calc R . H31B H 0.0041(2) 0.1676(2) 0.9476(2) 0.140 Uiso 1 calc R . H31C H -0.0065(2) 0.0935(2) 0.9120(2) 0.140 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 Se1 0.0338(2) 0.0753(2) 0.0908(3) 0.0136(2) -0.00062(15) -0.00993(14) P1 0.0323(3) 0.0455(4) 0.0374(4) 0.0050(3) -0.0024(3) -0.0030(3) N1 0.0293(10) 0.0422(11) 0.0276(10) 0.0035(9) 0.0011(8) 0.0018(8) P2 0.0313(3) 0.0468(4) 0.0286(3) -0.0005(3) -0.0013(3) 0.0054(3) Se2 0.0687(2) 0.0719(2) 0.03180(15) 0.00657(14) 0.01038(13) 0.0165(2) C1 0.051(2) 0.0425(15) 0.0344(14) 0.0009(12) 0.0006(12) 0.0030(12) C2 0.050(2) 0.057(2) 0.040(2) 0.0040(13) -0.0061(12) 0.0046(13) C3 0.071(2) 0.076(2) 0.046(2) 0.002(2) -0.016(2) 0.013(2) C4 0.122(3) 0.078(2) 0.041(2) 0.016(2) -0.012(2) 0.024(2) C5 0.112(3) 0.059(2) 0.046(2) 0.017(2) 0.007(2) -0.002(2) C6 0.071(2) 0.049(2) 0.041(2) 0.0044(14) 0.0063(14) -0.0046(14) C7 0.050(2) 0.0401(15) 0.0349(14) 0.0025(12) -0.0066(12) -0.0077(12) C8 0.057(2) 0.072(2) 0.042(2) -0.0032(15) -0.0035(13) 0.0100(15) C9 0.086(2) 0.075(2) 0.053(2) -0.008(2) 0.008(2) 0.019(2) C10 0.109(3) 0.074(2) 0.046(2) -0.012(2) 0.013(2) 0.000(2) C11 0.110(3) 0.089(3) 0.039(2) -0.014(2) -0.013(2) -0.017(2) C12 0.063(2) 0.071(2) 0.049(2) 0.000(2) -0.0141(15) -0.008(2) C13 0.0319(13) 0.049(2) 0.0306(13) 0.0059(12) 0.0043(10) 0.0051(11) C14 0.0369(14) 0.050(2) 0.057(2) 0.0025(14) 0.0025(12) 0.0026(12) C15 0.054(2) 0.044(2) 0.076(2) 0.004(2) 0.009(2) 0.0108(14) C16 0.043(2) 0.073(2) 0.061(2) 0.016(2) 0.0009(14) 0.0198(14) C17 0.044(2) 0.074(2) 0.055(2) -0.006(2) -0.0140(13) 0.0162(14) C18 0.0406(15) 0.057(2) 0.043(2) -0.0040(13) -0.0048(12) 0.0077(13) C19 0.0309(13) 0.0458(15) 0.0422(15) -0.0136(13) -0.0036(11) 0.0040(11) C20 0.049(2) 0.067(2) 0.054(2) -0.011(2) -0.0144(14) 0.0076(14) C21 0.040(2) 0.092(3) 0.081(2) -0.030(2) -0.021(2) 0.007(2) C22 0.038(2) 0.090(3) 0.107(3) -0.046(2) 0.008(2) -0.012(2) C23 0.055(2) 0.060(2) 0.075(2) -0.016(2) 0.019(2) -0.0104(14) C24 0.0398(15) 0.048(2) 0.053(2) -0.0104(14) 0.0052(12) 0.0004(12) C25 0.0352(13) 0.0373(13) 0.0290(13) -0.0025(11) 0.0019(10) -0.0013(10) C26 0.0369(14) 0.045(2) 0.0377(14) -0.0038(12) 0.0015(11) 0.0038(11) C27 0.043(2) 0.062(2) 0.052(2) -0.0027(15) 0.0149(14) -0.0017(13) C28 0.069(2) 0.063(2) 0.042(2) 0.0087(15) 0.0213(15) -0.002(2) C29 0.072(2) 0.056(2) 0.036(2) 0.0072(14) 0.0004(14) 0.0077(15) C30 0.0400(14) 0.053(2) 0.0349(15) 0.0004(13) 0.0002(12) 0.0053(12) O26 0.0309(9) 0.0740(13) 0.0519(11) 0.0072(10) -0.0007(8) 0.0083(9) C31 0.035(2) 0.142(3) 0.103(3) 0.018(2) -0.001(2) 0.019(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 Se1 P1 2.1056(6) . ? P1 N1 1.727(2) . ? P1 C7 1.818(3) . ? P1 C1 1.824(2) . ? N1 C25 1.466(3) . ? N1 P2 1.725(2) . ? P2 C13 1.819(2) . ? P2 C19 1.820(2) . ? P2 Se2 2.0936(7) . ? C1 C6 1.386(3) . ? C1 C2 1.389(3) . ? C2 C3 1.389(3) . ? C3 C4 1.382(4) . ? C4 C5 1.374(4) . ? C5 C6 1.387(4) . ? C7 C8 1.387(3) . ? C7 C12 1.398(3) . ? C8 C9 1.394(4) . ? C9 C10 1.351(4) . ? C10 C11 1.369(5) . ? C11 C12 1.386(4) . ? C13 C18 1.394(3) . ? C13 C14 1.395(3) . ? C14 C15 1.385(3) . ? C15 C16 1.389(4) . ? C16 C17 1.367(4) . ? C17 C18 1.380(3) . ? C19 C24 1.388(3) . ? C19 C20 1.394(3) . ? C20 C21 1.393(4) . ? C21 C22 1.373(4) . ? C22 C23 1.379(4) . ? C23 C24 1.396(3) . ? C25 C30 1.383(3) . ? C25 C26 1.404(3) . ? C26 O26 1.366(3) . ? C26 C27 1.394(3) . ? C27 C28 1.377(4) . ? C28 C29 1.371(4) . ? C29 C30 1.387(3) . ? O26 C31 1.426(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 N1 P1 C7 103.60(10) . . ? N1 P1 C1 106.69(10) . . ? C7 P1 C1 105.73(11) . . ? N1 P1 Se1 116.08(6) . . ? C7 P1 Se1 110.28(8) . . ? C1 P1 Se1 113.53(9) . . ? C25 N1 P2 115.41(14) . . ? C25 N1 P1 119.22(14) . . ? P2 N1 P1 124.77(10) . . ? N1 P2 C13 108.70(10) . . ? N1 P2 C19 103.00(9) . . ? C13 P2 C19 106.23(11) . . ? N1 P2 Se2 114.80(7) . . ? C13 P2 Se2 109.35(7) . . ? C19 P2 Se2 114.24(8) . . ? C6 C1 C2 119.7(2) . . ? C6 C1 P1 119.1(2) . . ? C2 C1 P1 121.1(2) . . ? C1 C2 C3 119.8(3) . . ? C4 C3 C2 119.7(3) . . ? C5 C4 C3 120.8(3) . . ? C4 C5 C6 119.6(3) . . ? C5 C6 C1 120.3(3) . . ? C8 C7 C12 117.8(2) . . ? C8 C7 P1 122.2(2) . . ? C12 C7 P1 119.9(2) . . ? C7 C8 C9 121.1(3) . . ? C10 C9 C8 119.9(3) . . ? C9 C10 C11 120.5(3) . . ? C10 C11 C12 120.5(3) . . ? C11 C12 C7 120.2(3) . . ? C18 C13 C14 118.6(2) . . ? C18 C13 P2 121.1(2) . . ? C14 C13 P2 119.6(2) . . ? C13 C14 C15 120.4(2) . . ? C16 C15 C14 119.9(3) . . ? C17 C16 C15 120.0(2) . . ? C16 C17 C18 120.6(3) . . ? C17 C18 C13 120.5(3) . . ? C24 C19 C20 119.6(2) . . ? C24 C19 P2 121.8(2) . . ? C20 C19 P2 118.5(2) . . ? C19 C20 C21 120.0(3) . . ? C22 C21 C20 120.0(3) . . ? C21 C22 C23 120.6(3) . . ? C22 C23 C24 119.9(3) . . ? C19 C24 C23 119.9(3) . . ? C30 C25 C26 118.9(2) . . ? C30 C25 N1 120.3(2) . . ? C26 C25 N1 120.6(2) . . ? O26 C26 C27 124.3(2) . . ? O26 C26 C25 116.2(2) . . ? C27 C26 C25 119.5(2) . . ? C28 C27 C26 120.1(2) . . ? C29 C28 C27 120.9(2) . . ? C28 C29 C30 119.4(2) . . ? C25 C30 C29 121.2(2) . . ? C26 O26 C31 118.6(2) . . ? 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 P1 N1 C25 -13.5(2) . . . . ? C1 P1 N1 C25 -124.8(2) . . . . ? Se1 P1 N1 C25 107.53(15) . . . . ? C7 P1 N1 P2 175.76(12) . . . . ? C1 P1 N1 P2 64.43(15) . . . . ? Se1 P1 N1 P2 -63.21(13) . . . . ? C25 N1 P2 C13 -70.6(2) . . . . ? P1 N1 P2 C13 100.44(14) . . . . ? C25 N1 P2 C19 41.8(2) . . . . ? P1 N1 P2 C19 -147.16(13) . . . . ? C25 N1 P2 Se2 166.59(12) . . . . ? P1 N1 P2 Se2 -22.35(14) . . . . ? N1 P1 C1 C6 -151.5(2) . . . . ? C7 P1 C1 C6 98.7(2) . . . . ? Se1 P1 C1 C6 -22.3(2) . . . . ? N1 P1 C1 C2 31.5(2) . . . . ? C7 P1 C1 C2 -78.4(2) . . . . ? Se1 P1 C1 C2 160.6(2) . . . . ? C6 C1 C2 C3 0.1(4) . . . . ? P1 C1 C2 C3 177.1(2) . . . . ? C1 C2 C3 C4 -0.2(4) . . . . ? C2 C3 C4 C5 -0.1(5) . . . . ? C3 C4 C5 C6 0.5(5) . . . . ? C4 C5 C6 C1 -0.6(4) . . . . ? C2 C1 C6 C5 0.3(4) . . . . ? P1 C1 C6 C5 -176.8(2) . . . . ? N1 P1 C7 C8 -86.5(2) . . . . ? C1 P1 C7 C8 25.5(2) . . . . ? Se1 P1 C7 C8 148.7(2) . . . . ? N1 P1 C7 C12 97.4(2) . . . . ? C1 P1 C7 C12 -150.6(2) . . . . ? Se1 P1 C7 C12 -27.4(2) . . . . ? C12 C7 C8 C9 0.2(4) . . . . ? P1 C7 C8 C9 -175.9(2) . . . . ? C7 C8 C9 C10 0.0(5) . . . . ? C8 C9 C10 C11 -0.6(5) . . . . ? C9 C10 C11 C12 1.0(5) . . . . ? C10 C11 C12 C7 -0.8(5) . . . . ? C8 C7 C12 C11 0.1(4) . . . . ? P1 C7 C12 C11 176.4(2) . . . . ? N1 P2 C13 C18 -35.3(2) . . . . ? C19 P2 C13 C18 -145.5(2) . . . . ? Se2 P2 C13 C18 90.8(2) . . . . ? N1 P2 C13 C14 154.5(2) . . . . ? C19 P2 C13 C14 44.3(2) . . . . ? Se2 P2 C13 C14 -79.5(2) . . . . ? C18 C13 C14 C15 0.6(4) . . . . ? P2 C13 C14 C15 171.1(2) . . . . ? C13 C14 C15 C16 0.6(4) . . . . ? C14 C15 C16 C17 -1.1(4) . . . . ? C15 C16 C17 C18 0.3(4) . . . . ? C16 C17 C18 C13 1.0(4) . . . . ? C14 C13 C18 C17 -1.4(4) . . . . ? P2 C13 C18 C17 -171.8(2) . . . . ? N1 P2 C19 C24 -79.9(2) . . . . ? C13 P2 C19 C24 34.3(2) . . . . ? Se2 P2 C19 C24 154.9(2) . . . . ? N1 P2 C19 C20 95.4(2) . . . . ? C13 P2 C19 C20 -150.4(2) . . . . ? Se2 P2 C19 C20 -29.8(2) . . . . ? C24 C19 C20 C21 0.3(4) . . . . ? P2 C19 C20 C21 -175.1(2) . . . . ? C19 C20 C21 C22 -1.4(4) . . . . ? C20 C21 C22 C23 1.3(5) . . . . ? C21 C22 C23 C24 -0.1(4) . . . . ? C20 C19 C24 C23 0.9(3) . . . . ? P2 C19 C24 C23 176.1(2) . . . . ? C22 C23 C24 C19 -1.0(4) . . . . ? P2 N1 C25 C30 82.1(2) . . . . ? P1 N1 C25 C30 -89.5(2) . . . . ? P2 N1 C25 C26 -94.3(2) . . . . ? P1 N1 C25 C26 94.1(2) . . . . ? C30 C25 C26 O26 179.2(2) . . . . ? N1 C25 C26 O26 -4.4(3) . . . . ? C30 C25 C26 C27 -1.5(3) . . . . ? N1 C25 C26 C27 175.0(2) . . . . ? O26 C26 C27 C28 178.9(2) . . . . ? C25 C26 C27 C28 -0.4(4) . . . . ? C26 C27 C28 C29 2.2(4) . . . . ? C27 C28 C29 C30 -2.0(4) . . . . ? C26 C25 C30 C29 1.7(3) . . . . ? N1 C25 C30 C29 -174.8(2) . . . . ? C28 C29 C30 C25 0.0(4) . . . . ? C27 C26 O26 C31 0.2(4) . . . . ? C25 C26 O26 C31 179.5(2) . . . . ? _refine_diff_density_max 0.452 _refine_diff_density_min -0.536 _refine_diff_density_rms 0.069 #---end data_6 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common - _chemical_formula_moiety 'C31 H27 Cl2 N O P2 Pd.(C H Cl2)0.5(CH2Cl2)0.5' _chemical_formula_structural 'C32 H28.50 Cl4.50 N O P2 Pd' _chemical_formula_analytical 'C32 H28.50 Cl4.50 N O P2 Pd' _chemical_formula_sum 'C32 H28.50 Cl4.50 N O P2 Pd' _chemical_formula_weight 770.92 _chemical_melting_point - _chemical_compound_source - 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' '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' '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 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 11.8731(3) _cell_length_b 14.3704(3) _cell_length_c 21.5491(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.5020(10) _cell_angle_gamma 90.00 _cell_volume 3636.33(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 132 _cell_measurement_theta_min 12 _cell_measurement_theta_max 168 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max .31 _exptl_crystal_size_mid .26 _exptl_crystal_size_min .2 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.408 _exptl_crystal_density_method - _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 0.954 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.832801 _exptl_absorpt_correction_T_max 1.00000 _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 SMART _diffrn_measurement_method CCD _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time - _diffrn_standards_decay_% - _diffrn_reflns_number 22016 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0602 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 28.71 _reflns_number_total 8551 _reflns_number_observed 5354 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 50 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.1412P)^2^+4.9978P] 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 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8501 _refine_ls_number_parameters 392 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1063 _refine_ls_R_factor_obs 0.0559 _refine_ls_wR_factor_all 0.2341 _refine_ls_wR_factor_obs 0.1564 _refine_ls_goodness_of_fit_all 0.849 _refine_ls_goodness_of_fit_obs 0.840 _refine_ls_restrained_S_all 1.002 _refine_ls_restrained_S_obs 0.840 _refine_ls_shift/esd_max 2.204 _refine_ls_shift/esd_mean 0.107 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd -0.52035(3) 0.82392(3) 0.32335(2) 0.0389(2) Uani 1 d . . Cl1 Cl -0.67622(12) 0.87146(12) 0.24848(8) 0.0627(4) Uani 1 d . . P1 P -0.39173(11) 0.81954(9) 0.25841(6) 0.0374(3) Uani 1 d . . N1 N -0.2848(3) 0.7822(3) 0.3142(2) 0.0385(9) Uani 1 d . . C1 C -0.3568(4) 0.9308(4) 0.2279(2) 0.0437(11) Uani 1 d . . Cl2 Cl -0.61875(14) 0.82532(13) 0.41046(8) 0.0654(4) Uani 1 d . . C2 C -0.3980(5) 1.0115(4) 0.2530(3) 0.060(2) Uani 1 d . . H2A H -0.4443(5) 1.0069(4) 0.2841(3) 0.071 Uiso 1 calc R . C3 C -0.3701(6) 1.0975(5) 0.2318(4) 0.079(2) Uani 1 d . . H3A H -0.3960(6) 1.1510(5) 0.2495(4) 0.095 Uiso 1 calc R . C4 C -0.3043(6) 1.1049(5) 0.1848(4) 0.080(2) Uani 1 d . . H4A H -0.2876(6) 1.1632(5) 0.1697(4) 0.096 Uiso 1 calc R . C5 C -0.2630(7) 1.0254(6) 0.1600(4) 0.079(2) Uani 1 d . . H5A H -0.2175(7) 1.0301(6) 0.1285(4) 0.095 Uiso 1 calc R . C6 C -0.2891(6) 0.9388(4) 0.1819(3) 0.061(2) Uani 1 d . . H6A H -0.2606(6) 0.8856(4) 0.1653(3) 0.073 Uiso 1 calc R . C7 C -0.4057(5) 0.7405(4) 0.1926(2) 0.0434(11) Uani 1 d . . C8 C -0.4828(6) 0.7645(5) 0.1399(3) 0.062(2) Uani 1 d . . H8A H -0.5240(6) 0.8196(5) 0.1393(3) 0.075 Uiso 1 calc R . C9 C -0.4976(7) 0.7058(6) 0.0885(3) 0.076(2) Uani 1 d . . H9A H -0.5486(7) 0.7221(6) 0.0532(3) 0.092 Uiso 1 calc R . C10 C -0.4385(7) 0.6241(6) 0.0888(4) 0.078(2) Uani 1 d . . H10A H -0.4482(7) 0.5856(6) 0.0537(4) 0.093 Uiso 1 calc R . C11 C -0.3637(7) 0.5990(5) 0.1420(4) 0.078(2) Uani 1 d . . H11A H -0.3232(7) 0.5435(5) 0.1427(4) 0.093 Uiso 1 calc R . C12 C -0.3499(6) 0.6564(4) 0.1937(3) 0.065(2) Uani 1 d . . H12A H -0.3023(6) 0.6382(4) 0.2298(3) 0.078 Uiso 1 calc R . P2 P -0.35603(11) 0.78167(10) 0.37779(6) 0.0404(3) Uani 1 d . . C13 C -0.2856(5) 0.8611(4) 0.4348(2) 0.0478(12) Uani 1 d . . C14 C -0.3300(5) 0.9497(4) 0.4397(3) 0.0564(14) Uani 1 d . . H14A H -0.3994(5) 0.9653(4) 0.4160(3) 0.068 Uiso 1 calc R . C15 C -0.2725(7) 1.0149(5) 0.4792(4) 0.078(2) Uani 1 d . . H15A H -0.3024(7) 1.0744(5) 0.4816(4) 0.093 Uiso 1 calc R . C16 C -0.1745(8) 0.9928(7) 0.5140(4) 0.095(3) Uani 1 d . . H16A H -0.1372(8) 1.0369(7) 0.5412(4) 0.114 Uiso 1 calc R . C17 C -0.1266(7) 0.9056(7) 0.5106(4) 0.087(2) Uani 1 d . . H17A H -0.0573(7) 0.8916(7) 0.5349(4) 0.105 Uiso 1 calc R . C18 C -0.1831(6) 0.8388(6) 0.4706(4) 0.079(2) Uani 1 d . . H18A H -0.1519(6) 0.7799(6) 0.4680(4) 0.094 Uiso 1 calc R . C19 C -0.3496(5) 0.6683(4) 0.4128(3) 0.0515(13) Uani 1 d . . C20 C -0.3499(6) 0.5884(4) 0.3762(3) 0.063(2) Uani 1 d . . H20A H -0.3480(6) 0.5939(4) 0.3334(3) 0.075 Uiso 1 calc R . C21 C -0.3529(7) 0.5010(5) 0.4029(4) 0.080(2) Uani 1 d . . H21A H -0.3481(7) 0.4481(5) 0.3785(4) 0.096 Uiso 1 calc R . C22 C -0.3629(9) 0.4923(6) 0.4647(5) 0.100(3) Uani 1 d . . H22A H -0.3657(9) 0.4334(6) 0.4823(5) 0.120 Uiso 1 calc R . C23 C -0.3689(10) 0.5707(6) 0.5015(4) 0.113(4) Uani 1 d . . H23A H -0.3768(10) 0.5643(6) 0.5436(4) 0.135 Uiso 1 calc R . C24 C -0.3630(8) 0.6587(5) 0.4755(3) 0.080(2) Uani 1 d . . H24A H -0.3681(8) 0.7113(5) 0.5001(3) 0.096 Uiso 1 calc R . C25 C -0.1625(4) 0.7921(4) 0.3168(3) 0.0464(12) Uani 1 d . . C26 C -0.0931(5) 0.7136(5) 0.3166(4) 0.070(2) Uani 1 d . . C27 C 0.0249(6) 0.7262(7) 0.3237(5) 0.098(3) Uani 1 d . . H27A H 0.0727(6) 0.6748(7) 0.3244(5) 0.118 Uiso 1 calc R . C28 C 0.0704(6) 0.8138(6) 0.3297(5) 0.092(3) Uani 1 d . . H28A H 0.1490(6) 0.8213(6) 0.3340(5) 0.111 Uiso 1 calc R . C29 C 0.0026(6) 0.8902(6) 0.3294(4) 0.076(2) Uani 1 d . . H29A H 0.0355(6) 0.9491(6) 0.3329(4) 0.091 Uiso 1 calc R . C30 C -0.1148(5) 0.8814(5) 0.3239(3) 0.0583(15) Uani 1 d . . H30A H -0.1609(5) 0.9336(5) 0.3250(3) 0.070 Uiso 1 calc R . O26 O -0.1450(4) 0.6308(3) 0.3099(3) 0.088(2) Uani 1 d . . C31 C -0.0763(9) 0.5493(7) 0.3101(8) 0.163(6) Uani 1 d . . H31A H -0.1243(9) 0.4953(7) 0.3049(8) 0.244 Uiso 1 calc R . H31B H -0.0262(9) 0.5452(7) 0.3493(8) 0.244 Uiso 1 calc R . H31C H -0.0321(9) 0.5527(7) 0.2763(8) 0.244 Uiso 1 calc R . C40 C 0.1032(25) 0.7521(21) 0.6510(11) 0.186(14) Uani 0.50 d P . H40A H 0.1546(25) 0.7241(21) 0.6858(11) 0.223 Uiso 0.50 calc PR . Cl3 Cl -0.0186(7) 0.7038(5) 0.6486(4) 0.147(2) Uani 0.50 d P . Cl4 Cl 0.1149(8) 0.8658(4) 0.6578(4) 0.193(4) Uani 0.50 d P . Cl5 Cl 0.1636(7) 0.7332(7) 0.5808(6) 0.210(5) Uani 0.50 d P . C50 C -0.0128(70) 0.5620(45) 0.4904(34) 0.336(34) Uiso 0.50 d P . Cl6 Cl 0.0908(14) 0.6303(12) 0.4616(8) 0.296(6) Uiso 0.50 d P . Cl7 Cl -0.0913(9) 0.5599(7) 0.5134(5) 0.177(3) Uiso 0.50 d P . 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 0.0330(2) 0.0427(2) 0.0415(2) -0.0050(2) 0.00722(15) 0.0020(2) Cl1 0.0428(7) 0.0751(10) 0.0669(10) 0.0046(8) -0.0031(6) 0.0048(7) P1 0.0372(6) 0.0363(6) 0.0392(7) -0.0025(5) 0.0079(5) 0.0010(5) N1 0.032(2) 0.043(2) 0.041(2) 0.001(2) 0.006(2) 0.005(2) C1 0.043(3) 0.042(3) 0.045(3) 0.002(2) 0.003(2) -0.001(2) Cl2 0.0526(8) 0.0935(12) 0.0541(8) -0.0128(8) 0.0214(7) 0.0033(8) C2 0.059(4) 0.044(3) 0.077(4) 0.006(3) 0.018(3) 0.005(3) C3 0.064(4) 0.046(3) 0.129(7) 0.010(4) 0.020(4) 0.002(3) C4 0.064(4) 0.050(4) 0.128(7) 0.027(4) 0.019(4) -0.007(3) C5 0.080(5) 0.080(5) 0.083(5) 0.009(4) 0.024(4) -0.031(4) C6 0.073(4) 0.053(3) 0.061(4) -0.008(3) 0.025(3) -0.016(3) C7 0.050(3) 0.042(3) 0.040(3) -0.002(2) 0.013(2) -0.004(2) C8 0.078(4) 0.059(4) 0.048(3) -0.010(3) 0.003(3) 0.003(3) C9 0.093(5) 0.079(5) 0.054(4) -0.014(4) 0.003(4) -0.010(4) C10 0.101(6) 0.077(5) 0.063(4) -0.030(4) 0.036(4) -0.037(4) C11 0.108(6) 0.059(4) 0.072(5) -0.020(4) 0.032(4) 0.006(4) C12 0.077(4) 0.053(4) 0.066(4) -0.009(3) 0.014(3) 0.009(3) P2 0.0381(7) 0.0439(7) 0.0395(7) -0.0029(6) 0.0065(5) 0.0040(5) C13 0.050(3) 0.053(3) 0.040(3) -0.008(2) 0.008(2) 0.000(3) C14 0.057(3) 0.060(4) 0.051(3) -0.011(3) 0.007(3) 0.003(3) C15 0.092(5) 0.067(4) 0.071(5) -0.021(4) 0.004(4) -0.010(4) C16 0.111(7) 0.096(6) 0.078(5) -0.035(5) 0.009(5) -0.032(6) C17 0.071(5) 0.115(7) 0.067(5) -0.020(5) -0.019(4) -0.006(5) C18 0.066(4) 0.085(5) 0.076(5) -0.007(4) -0.017(4) 0.005(4) C19 0.051(3) 0.056(3) 0.048(3) 0.011(3) 0.009(2) 0.009(3) C20 0.075(4) 0.050(3) 0.064(4) -0.005(3) 0.013(3) -0.009(3) C21 0.095(5) 0.060(4) 0.087(5) -0.002(4) 0.022(4) -0.016(4) C22 0.132(8) 0.068(5) 0.106(7) 0.027(5) 0.034(6) 0.000(5) C23 0.200(11) 0.078(6) 0.066(5) 0.022(4) 0.040(6) 0.001(6) C24 0.120(7) 0.069(5) 0.054(4) 0.006(3) 0.028(4) 0.010(4) C25 0.032(2) 0.059(3) 0.049(3) 0.001(3) 0.010(2) -0.002(2) C26 0.037(3) 0.068(4) 0.107(6) -0.001(4) 0.016(3) 0.009(3) C27 0.042(4) 0.096(6) 0.158(9) 0.004(6) 0.024(4) 0.011(4) C28 0.038(4) 0.103(7) 0.136(8) 0.002(5) 0.015(4) -0.003(4) C29 0.054(4) 0.084(5) 0.087(5) -0.004(4) 0.001(3) -0.023(4) C30 0.048(3) 0.064(4) 0.060(4) 0.000(3) 0.000(3) -0.006(3) O26 0.050(3) 0.052(3) 0.162(5) -0.001(3) 0.015(3) 0.009(2) C31 0.097(7) 0.064(6) 0.324(20) -0.026(8) 0.019(9) 0.029(5) C40 0.202(25) 0.223(28) 0.109(16) 0.005(17) -0.062(16) 0.174(25) Cl3 0.128(5) 0.152(5) 0.155(6) 0.000(5) 0.004(4) -0.056(4) Cl4 0.236(9) 0.095(4) 0.202(7) 0.050(4) -0.115(7) -0.066(5) Cl5 0.143(6) 0.167(7) 0.326(14) 0.063(8) 0.055(8) 0.054(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 P2 2.2078(13) . ? Pd1 P1 2.2196(13) . ? Pd1 Cl2 2.3532(15) . ? Pd1 Cl1 2.3688(15) . ? P1 N1 1.701(4) . ? P1 C7 1.806(5) . ? P1 C1 1.800(5) . ? P1 P2 2.602(2) . ? N1 C25 1.452(6) . ? N1 P2 1.714(4) . ? C1 C6 1.369(8) . ? C1 C2 1.398(8) . ? C2 C3 1.375(9) . ? C3 C4 1.372(11) . ? C4 C5 1.383(11) . ? C5 C6 1.382(9) . ? C7 C12 1.375(8) . ? C7 C8 1.392(8) . ? C8 C9 1.383(9) . ? C9 C10 1.368(11) . ? C10 C11 1.390(11) . ? C11 C12 1.376(9) . ? P2 C13 1.792(6) . ? P2 C19 1.793(6) . ? C13 C18 1.378(9) . ? C13 C14 1.388(8) . ? C14 C15 1.377(9) . ? C15 C16 1.325(12) . ? C16 C17 1.382(12) . ? C17 C18 1.394(10) . ? C19 C24 1.391(9) . ? C19 C20 1.392(9) . ? C20 C21 1.384(10) . ? C21 C22 1.360(12) . ? C22 C23 1.386(13) . ? C23 C24 1.389(11) . ? C25 C30 1.402(8) . ? C25 C26 1.397(8) . ? C26 O26 1.337(8) . ? C26 C27 1.398(10) . ? C27 C28 1.369(12) . ? C28 C29 1.360(11) . ? C29 C30 1.388(9) . ? O26 C31 1.427(9) . ? C40 Cl4 1.65(3) . ? C40 Cl3 1.60(4) . ? C40 Cl5 1.79(3) . ? C50 Cl7 1.12(8) . ? C50 C50 1.85(13) 3_566 ? C50 Cl6 1.76(7) . ? C50 Cl7 2.15(7) 3_566 ? Cl7 C50 2.15(7) 3_566 ? 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 P2 Pd1 P1 71.99(5) . . ? P2 Pd1 Cl2 94.73(6) . . ? P1 Pd1 Cl2 166.46(6) . . ? P2 Pd1 Cl1 168.87(6) . . ? P1 Pd1 Cl1 96.88(5) . . ? Cl2 Pd1 Cl1 96.36(6) . . ? N1 P1 C7 109.2(2) . . ? N1 P1 C1 110.5(2) . . ? C7 P1 C1 105.7(2) . . ? N1 P1 Pd1 94.30(14) . . ? C7 P1 Pd1 121.4(2) . . ? C1 P1 Pd1 115.0(2) . . ? N1 P1 P2 40.55(14) . . ? C7 P1 P2 128.9(2) . . ? C1 P1 P2 122.3(2) . . ? Pd1 P1 P2 53.79(4) . . ? C25 N1 P1 129.4(4) . . ? C25 N1 P2 125.3(3) . . ? P1 N1 P2 99.3(2) . . ? C6 C1 C2 119.1(5) . . ? C6 C1 P1 122.1(4) . . ? C2 C1 P1 118.8(4) . . ? C3 C2 C1 120.1(6) . . ? C4 C3 C2 120.4(7) . . ? C5 C4 C3 119.7(6) . . ? C4 C5 C6 120.0(7) . . ? C1 C6 C5 120.6(6) . . ? C12 C7 C8 119.3(5) . . ? C12 C7 P1 123.4(5) . . ? C8 C7 P1 117.2(4) . . ? C9 C8 C7 119.5(6) . . ? C10 C9 C8 121.0(7) . . ? C9 C10 C11 119.4(6) . . ? C12 C11 C10 119.8(7) . . ? C11 C12 C7 120.9(7) . . ? N1 P2 C13 108.1(2) . . ? N1 P2 C19 110.2(2) . . ? C13 P2 C19 107.7(3) . . ? N1 P2 Pd1 94.34(14) . . ? C13 P2 Pd1 118.4(2) . . ? C19 P2 Pd1 116.9(2) . . ? N1 P2 P1 40.17(13) . . ? C13 P2 P1 122.4(2) . . ? C19 P2 P1 126.6(2) . . ? Pd1 P2 P1 54.21(4) . . ? C18 C13 C14 119.0(6) . . ? C18 C13 P2 121.3(5) . . ? C14 C13 P2 119.5(4) . . ? C15 C14 C13 120.7(6) . . ? C16 C15 C14 120.0(8) . . ? C15 C16 C17 121.4(7) . . ? C16 C17 C18 119.5(7) . . ? C13 C18 C17 119.3(7) . . ? C24 C19 C20 118.5(6) . . ? C24 C19 P2 119.7(5) . . ? C20 C19 P2 121.0(5) . . ? C21 C20 C19 120.7(6) . . ? C22 C21 C20 120.1(8) . . ? C21 C22 C23 120.4(8) . . ? C22 C23 C24 119.9(8) . . ? C19 C24 C23 120.1(7) . . ? C30 C25 C26 120.8(5) . . ? C30 C25 N1 118.6(5) . . ? C26 C25 N1 120.5(5) . . ? O26 C26 C27 124.4(6) . . ? O26 C26 C25 117.1(5) . . ? C27 C26 C25 118.4(7) . . ? C28 C27 C26 120.3(7) . . ? C29 C28 C27 121.2(7) . . ? C28 C29 C30 120.9(7) . . ? C29 C30 C25 118.4(6) . . ? C26 O26 C31 118.3(6) . . ? Cl4 C40 Cl3 119.8(13) . . ? Cl4 C40 Cl5 100.8(19) . . ? Cl3 C40 Cl5 112.4(16) . . ? Cl7 C50 C50 89.6(62) . 3_566 ? Cl7 C50 Cl6 147.6(55) . . ? C50 C50 Cl6 121.3(70) 3_566 . ? Cl7 C50 Cl7 121.0(47) . 3_566 ? C50 C50 Cl7 31.3(33) 3_566 3_566 ? Cl6 C50 Cl7 90.3(37) . 3_566 ? C50 Cl7 C50 59.0(47) . 3_566 ? 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 P2 Pd1 P1 N1 2.09(15) . . . . ? Cl2 Pd1 P1 N1 13.7(3) . . . . ? Cl1 Pd1 P1 N1 -178.3(2) . . . . ? P2 Pd1 P1 C7 117.7(2) . . . . ? Cl2 Pd1 P1 C7 129.3(3) . . . . ? Cl1 Pd1 P1 C7 -62.8(2) . . . . ? P2 Pd1 P1 C1 -112.9(2) . . . . ? Cl2 Pd1 P1 C1 -101.3(3) . . . . ? Cl1 Pd1 P1 C1 66.7(2) . . . . ? P2 Pd1 P1 P2 0.0 . . . . ? Cl2 Pd1 P1 P2 11.6(3) . . . . ? Cl1 Pd1 P1 P2 179.58(6) . . . . ? C7 P1 N1 C25 78.9(5) . . . . ? C1 P1 N1 C25 -37.0(5) . . . . ? Pd1 P1 N1 C25 -155.7(4) . . . . ? P2 P1 N1 C25 -153.1(6) . . . . ? C7 P1 N1 P2 -128.0(2) . . . . ? C1 P1 N1 P2 116.1(2) . . . . ? Pd1 P1 N1 P2 -2.6(2) . . . . ? P2 P1 N1 P2 0.0 . . . . ? N1 P1 C1 C6 82.4(5) . . . . ? C7 P1 C1 C6 -35.6(5) . . . . ? Pd1 P1 C1 C6 -172.4(4) . . . . ? P2 P1 C1 C6 126.1(4) . . . . ? N1 P1 C1 C2 -96.1(5) . . . . ? C7 P1 C1 C2 145.9(5) . . . . ? Pd1 P1 C1 C2 9.2(5) . . . . ? P2 P1 C1 C2 -52.4(5) . . . . ? C6 C1 C2 C3 -0.3(10) . . . . ? P1 C1 C2 C3 178.2(5) . . . . ? C1 C2 C3 C4 1.7(11) . . . . ? C2 C3 C4 C5 -2.0(12) . . . . ? C3 C4 C5 C6 0.8(12) . . . . ? C2 C1 C6 C5 -0.8(9) . . . . ? P1 C1 C6 C5 -179.3(5) . . . . ? C4 C5 C6 C1 0.6(11) . . . . ? N1 P1 C7 C12 9.6(6) . . . . ? C1 P1 C7 C12 128.5(5) . . . . ? Pd1 P1 C7 C12 -98.2(5) . . . . ? P2 P1 C7 C12 -31.5(6) . . . . ? N1 P1 C7 C8 -174.6(4) . . . . ? C1 P1 C7 C8 -55.7(5) . . . . ? Pd1 P1 C7 C8 77.6(5) . . . . ? P2 P1 C7 C8 144.3(4) . . . . ? C12 C7 C8 C9 -3.3(10) . . . . ? P1 C7 C8 C9 -179.3(5) . . . . ? C7 C8 C9 C10 0.6(11) . . . . ? C8 C9 C10 C11 1.1(12) . . . . ? C9 C10 C11 C12 -0.1(11) . . . . ? C10 C11 C12 C7 -2.7(11) . . . . ? C8 C7 C12 C11 4.3(10) . . . . ? P1 C7 C12 C11 -179.9(6) . . . . ? C25 N1 P2 C13 35.4(5) . . . . ? P1 N1 P2 C13 -119.2(3) . . . . ? C25 N1 P2 C19 -82.0(5) . . . . ? P1 N1 P2 C19 123.4(3) . . . . ? C25 N1 P2 Pd1 157.2(4) . . . . ? P1 N1 P2 Pd1 2.6(2) . . . . ? C25 N1 P2 P1 154.6(5) . . . . ? P1 N1 P2 P1 0.0 . . . . ? P1 Pd1 P2 N1 -2.07(15) . . . . ? Cl2 Pd1 P2 N1 -179.4(2) . . . . ? Cl1 Pd1 P2 N1 -4.3(4) . . . . ? P1 Pd1 P2 C13 111.2(2) . . . . ? Cl2 Pd1 P2 C13 -66.1(2) . . . . ? Cl1 Pd1 P2 C13 109.0(4) . . . . ? P1 Pd1 P2 C19 -117.3(2) . . . . ? Cl2 Pd1 P2 C19 65.4(2) . . . . ? Cl1 Pd1 P2 C19 -119.5(4) . . . . ? P1 Pd1 P2 P1 0.0 . . . . ? Cl2 Pd1 P2 P1 -177.29(6) . . . . ? Cl1 Pd1 P2 P1 -2.2(3) . . . . ? N1 P1 P2 N1 0.000(1) . . . . ? C7 P1 P2 N1 72.9(3) . . . . ? C1 P1 P2 N1 -84.2(3) . . . . ? Pd1 P1 P2 N1 176.8(2) . . . . ? N1 P1 P2 C13 79.5(3) . . . . ? C7 P1 P2 C13 152.4(3) . . . . ? C1 P1 P2 C13 -4.7(3) . . . . ? Pd1 P1 P2 C13 -103.7(2) . . . . ? N1 P1 P2 C19 -77.6(3) . . . . ? C7 P1 P2 C19 -4.7(3) . . . . ? C1 P1 P2 C19 -161.8(3) . . . . ? Pd1 P1 P2 C19 99.2(2) . . . . ? N1 P1 P2 Pd1 -176.8(2) . . . . ? C7 P1 P2 Pd1 -103.9(2) . . . . ? C1 P1 P2 Pd1 99.0(2) . . . . ? Pd1 P1 P2 Pd1 0.0 . . . . ? N1 P2 C13 C18 -74.8(6) . . . . ? C19 P2 C13 C18 44.2(6) . . . . ? Pd1 P2 C13 C18 179.7(5) . . . . ? P1 P2 C13 C18 -116.7(6) . . . . ? N1 P2 C13 C14 99.9(5) . . . . ? C19 P2 C13 C14 -141.1(5) . . . . ? Pd1 P2 C13 C14 -5.6(6) . . . . ? P1 P2 C13 C14 58.0(5) . . . . ? C18 C13 C14 C15 0.5(10) . . . . ? P2 C13 C14 C15 -174.3(5) . . . . ? C13 C14 C15 C16 -1.2(12) . . . . ? C14 C15 C16 C17 1.4(14) . . . . ? C15 C16 C17 C18 -0.9(14) . . . . ? C14 C13 C18 C17 0.0(11) . . . . ? P2 C13 C18 C17 174.7(6) . . . . ? C16 C17 C18 C13 0.2(13) . . . . ? N1 P2 C19 C24 156.5(6) . . . . ? C13 P2 C19 C24 38.8(7) . . . . ? Pd1 P2 C19 C24 -97.4(6) . . . . ? P1 P2 C19 C24 -161.3(5) . . . . ? N1 P2 C19 C20 -34.0(6) . . . . ? C13 P2 C19 C20 -151.7(5) . . . . ? Pd1 P2 C19 C20 72.1(5) . . . . ? P1 P2 C19 C20 8.2(6) . . . . ? C24 C19 C20 C21 -5.9(10) . . . . ? P2 C19 C20 C21 -175.5(6) . . . . ? C19 C20 C21 C22 4.1(12) . . . . ? C20 C21 C22 C23 -0.7(15) . . . . ? C21 C22 C23 C24 -0.9(17) . . . . ? C20 C19 C24 C23 4.2(12) . . . . ? P2 C19 C24 C23 174.0(8) . . . . ? C22 C23 C24 C19 -0.9(16) . . . . ? P1 N1 C25 C30 66.7(7) . . . . ? P2 N1 C25 C30 -80.1(6) . . . . ? P1 N1 C25 C26 -117.7(6) . . . . ? P2 N1 C25 C26 95.4(7) . . . . ? C30 C25 C26 O26 179.6(6) . . . . ? N1 C25 C26 O26 4.1(10) . . . . ? C30 C25 C26 C27 0.0(12) . . . . ? N1 C25 C26 C27 -175.5(7) . . . . ? O26 C26 C27 C28 179.4(9) . . . . ? C25 C26 C27 C28 -1.0(15) . . . . ? C26 C27 C28 C29 0.5(17) . . . . ? C27 C28 C29 C30 1.0(15) . . . . ? C28 C29 C30 C25 -1.9(11) . . . . ? C26 C25 C30 C29 1.4(10) . . . . ? N1 C25 C30 C29 177.0(6) . . . . ? C27 C26 O26 C31 0.1(15) . . . . ? C25 C26 O26 C31 -179.5(10) . . . . ? C50 C50 Cl7 C50 0.000(2) 3_566 . . 3_566 ? Cl6 C50 Cl7 C50 -163.2(149) . . . 3_566 ? Cl7 C50 Cl7 C50 0.002(10) 3_566 . . 3_566 ? _refine_diff_density_max 0.980 _refine_diff_density_min -0.582 _refine_diff_density_rms 0.106 #---end data_10 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common - _chemical_formula_moiety 'C31 H27 Cl2 N O P2 Pt S.(C H Cl3)0.5' _chemical_formula_structural 'C31.50 H27.50 Cl3.50 N O P2 Pt S' _chemical_formula_analytical 'C31.50 H27.50 Cl3.50 N O P2 Pt S' _chemical_formula_sum 'C31.50 H27.50 Cl3.50 N O P2 Pt S' _chemical_formula_weight 849.21 _chemical_melting_point - _chemical_compound_source - 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' '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' 'Cl' 'Cl' 0.1484 0.1585 '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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.0814(6) _cell_length_b 9.2086(4) _cell_length_c 25.0051(9) _cell_angle_alpha 90.00 _cell_angle_beta 98.3840(10) _cell_angle_gamma 90.00 _cell_volume 3435.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 54 _cell_measurement_theta_min 12 _cell_measurement_theta_max 168 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max .4 _exptl_crystal_size_mid .15 _exptl_crystal_size_min .02 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.642 _exptl_crystal_density_method - _exptl_crystal_F_000 1660 _exptl_absorpt_coefficient_mu 4.536 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.616813 _exptl_absorpt_correction_T_max 1.000000 _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 SMART _diffrn_measurement_method CCD _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time - _diffrn_standards_decay_% - _diffrn_reflns_number 14656 _diffrn_reflns_av_R_equivalents 0.0283 _diffrn_reflns_av_sigmaI/netI 0.0316 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 23.23 _reflns_number_total 4931 _reflns_number_observed 4212 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 50 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0796P)^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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00105(15) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4881 _refine_ls_number_parameters 389 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0364 _refine_ls_R_factor_obs 0.0261 _refine_ls_wR_factor_all 0.1131 _refine_ls_wR_factor_obs 0.0752 _refine_ls_goodness_of_fit_all 0.787 _refine_ls_goodness_of_fit_obs 0.806 _refine_ls_restrained_S_all 1.123 _refine_ls_restrained_S_obs 0.806 _refine_ls_shift/esd_max 0.314 _refine_ls_shift/esd_mean 0.013 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt 0.746625(10) -0.85575(2) 0.232956(6) 0.02982(11) Uani 1 d . . Cl1 Cl 0.76698(9) -0.63912(13) 0.28304(6) 0.0480(3) Uani 1 d . . Cl2 Cl 0.74177(9) -0.98414(15) 0.31214(5) 0.0523(3) Uani 1 d . . S1 S 0.76316(9) -0.72466(14) 0.15699(5) 0.0446(3) Uani 1 d . . P1 P 0.68156(9) -0.84496(13) 0.10365(5) 0.0341(3) Uani 1 d . . N1 N 0.6988(2) -1.0219(4) 0.11950(14) 0.0324(8) Uani 1 d . . P2 P 0.72932(7) -1.06127(12) 0.18754(5) 0.0293(3) Uani 1 d . . C1 C 0.5661(3) -0.8005(5) 0.1060(2) 0.0395(11) Uani 1 d . . C2 C 0.4970(4) -0.8888(6) 0.0798(2) 0.0501(13) Uani 1 d . . H2A H 0.5108(4) -0.9705(6) 0.0607(2) 0.060 Uiso 1 calc R . C3 C 0.4085(4) -0.8541(7) 0.0823(3) 0.064(2) Uani 1 d . . H3A H 0.3628(4) -0.9126(7) 0.0651(3) 0.076 Uiso 1 calc R . C4 C 0.3881(4) -0.7328(9) 0.1105(3) 0.075(2) Uani 1 d . . H4A H 0.3286(4) -0.7104(9) 0.1127(3) 0.090 Uiso 1 calc R . C5 C 0.4547(5) -0.6460(8) 0.1351(3) 0.080(2) Uani 1 d . . H5A H 0.4406(5) -0.5629(8) 0.1532(3) 0.095 Uiso 1 calc R . C6 C 0.5428(4) -0.6808(7) 0.1334(2) 0.058(2) Uani 1 d . . H6A H 0.5877(4) -0.6217(7) 0.1512(2) 0.070 Uiso 1 calc R . C7 C 0.7037(4) -0.8109(6) 0.0358(2) 0.0446(13) Uani 1 d . . C8 C 0.6370(4) -0.7888(7) -0.0066(2) 0.059(2) Uani 1 d . . H8A H 0.5775(4) -0.7949(7) -0.0010(2) 0.071 Uiso 1 calc R . C9 C 0.6563(6) -0.7580(9) -0.0571(3) 0.086(2) Uani 1 d . . H9A H 0.6097(6) -0.7432(9) -0.0853(3) 0.103 Uiso 1 calc R . C10 C 0.7425(7) -0.7486(8) -0.0666(3) 0.091(2) Uani 1 d . . H10A H 0.7552(7) -0.7308(8) -0.1013(3) 0.109 Uiso 1 calc R . C11 C 0.8105(6) -0.7658(9) -0.0243(3) 0.094(3) Uani 1 d . . H11A H 0.8697(6) -0.7586(9) -0.0304(3) 0.113 Uiso 1 calc R . C12 C 0.7921(5) -0.7938(8) 0.0277(3) 0.074(2) Uani 1 d . . H12A H 0.8385(5) -0.8009(8) 0.0565(3) 0.089 Uiso 1 calc R . C13 C 0.6415(3) -1.1785(5) 0.2044(2) 0.0330(10) Uani 1 d . . C14 C 0.5514(3) -1.1386(5) 0.1878(2) 0.0378(12) Uani 1 d . . H14A H 0.5382(3) -1.0553(5) 0.1672(2) 0.045 Uiso 1 calc R . C15 C 0.4831(3) -1.2221(6) 0.2020(2) 0.0413(12) Uani 1 d . . H15A H 0.4238(3) -1.1962(6) 0.1904(2) 0.050 Uiso 1 calc R . C16 C 0.5019(4) -1.3436(6) 0.2333(2) 0.0518(15) Uani 1 d . . H16A H 0.4555(4) -1.3998(6) 0.2430(2) 0.062 Uiso 1 calc R . C17 C 0.5904(4) -1.3827(6) 0.2505(3) 0.061(2) Uani 1 d . . H17A H 0.6032(4) -1.4651(6) 0.2718(3) 0.073 Uiso 1 calc R . C18 C 0.6590(3) -1.3005(6) 0.2363(2) 0.0439(12) Uani 1 d . . H18A H 0.7180(3) -1.3271(6) 0.2483(2) 0.053 Uiso 1 calc R . C19 C 0.8303(3) -1.1695(5) 0.1907(2) 0.0359(11) Uani 1 d . . C20 C 0.8302(3) -1.3139(6) 0.1747(2) 0.0453(12) Uani 1 d . . H20A H 0.7764(3) -1.3624(6) 0.1642(2) 0.054 Uiso 1 calc R . C21 C 0.9111(4) -1.3849(7) 0.1745(3) 0.063(2) Uani 1 d . . H21A H 0.9112(4) -1.4813(7) 0.1634(3) 0.075 Uiso 1 calc R . C22 C 0.9908(4) -1.3157(7) 0.1904(3) 0.062(2) Uani 1 d . . H22A H 1.0447(4) -1.3645(7) 0.1898(3) 0.074 Uiso 1 calc R . C23 C 0.9908(4) -1.1750(7) 0.2068(3) 0.063(2) Uani 1 d . . H23A H 1.0450(4) -1.1280(7) 0.2179(3) 0.075 Uiso 1 calc R . C24 C 0.9113(3) -1.1013(6) 0.2073(2) 0.0474(13) Uani 1 d . . H24A H 0.9122(3) -1.0053(6) 0.2188(2) 0.057 Uiso 1 calc R . C25 C 0.6979(4) -1.1387(5) 0.0810(2) 0.0406(12) Uani 1 d . . C26 C 0.7756(4) -1.1705(6) 0.0592(2) 0.0515(14) Uani 1 d . . C27 C 0.7759(5) -1.2953(8) 0.0258(2) 0.070(2) Uani 1 d . . H27A H 0.8265(5) -1.3175(8) 0.0100(2) 0.083 Uiso 1 calc R . C28 C 0.7026(6) -1.3821(7) 0.0168(3) 0.074(2) Uani 1 d . . H28A H 0.7051(6) -1.4642(7) -0.0046(3) 0.089 Uiso 1 calc R . C29 C 0.6260(6) -1.3550(7) 0.0374(3) 0.072(2) Uani 1 d . . H29A H 0.5766(6) -1.4160(7) 0.0300(3) 0.087 Uiso 1 calc R . C30 C 0.6238(4) -1.2303(5) 0.0706(2) 0.0463(12) Uani 1 d . . H30A H 0.5723(4) -1.2095(5) 0.0856(2) 0.056 Uiso 1 calc R . O26 O 0.8454(2) -1.0808(5) 0.0725(2) 0.0641(11) Uani 1 d . . C31 C 0.9297(5) -1.1161(11) 0.0560(4) 0.105(3) Uani 1 d . . H31A H 0.9727(5) -1.0421(11) 0.0683(4) 0.157 Uiso 1 calc R . H31B H 0.9227(5) -1.1222(11) 0.0173(4) 0.157 Uiso 1 calc R . H31C H 0.9502(5) -1.2078(11) 0.0713(4) 0.157 Uiso 1 calc R . C40 C 0.8918(14) -0.2264(44) -0.1359(8) 0.230(19) Uani 0.50 d P . H40A H 0.8492(14) -0.2715(44) -0.1645(8) 0.276 Uiso 0.50 calc PR . Cl3 Cl 0.9480(5) -0.3892(7) -0.0731(2) 0.140(2) Uani 0.50 d P . Cl4 Cl 0.9989(3) -0.2240(4) -0.1526(2) 0.0899(11) Uani 0.50 d P . Cl5 Cl 0.8470(2) -0.1244(4) -0.1038(2) 0.0793(10) Uani 0.50 d P . 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 0.02578(14) 0.02979(15) 0.03337(14) -0.00272(7) 0.00255(8) -0.00111(7) Cl1 0.0436(7) 0.0403(8) 0.0595(8) -0.0170(6) 0.0051(6) -0.0024(5) Cl2 0.0708(9) 0.0512(8) 0.0351(7) 0.0032(6) 0.0087(6) -0.0039(7) S1 0.0543(7) 0.0344(7) 0.0432(7) 0.0024(6) 0.0013(6) -0.0154(6) P1 0.0398(7) 0.0313(7) 0.0310(7) 0.0018(5) 0.0046(5) -0.0013(5) N1 0.036(2) 0.029(2) 0.032(2) -0.002(2) 0.005(2) 0.000(2) P2 0.0267(6) 0.0283(6) 0.0329(6) 0.0018(5) 0.0041(5) -0.0012(5) C1 0.048(3) 0.037(3) 0.033(3) 0.003(2) 0.005(2) 0.004(2) C2 0.047(3) 0.046(3) 0.055(3) 0.001(3) -0.002(3) 0.006(3) C3 0.043(3) 0.074(5) 0.069(4) 0.005(3) -0.004(3) 0.002(3) C4 0.049(3) 0.099(6) 0.077(4) -0.010(4) 0.012(3) 0.024(4) C5 0.062(4) 0.092(6) 0.084(5) -0.033(4) 0.011(4) 0.024(4) C6 0.058(4) 0.060(4) 0.056(4) -0.018(3) 0.003(3) 0.011(3) C7 0.065(3) 0.036(3) 0.035(3) 0.006(2) 0.016(3) 0.004(3) C8 0.076(4) 0.065(4) 0.035(3) 0.001(3) 0.001(3) -0.019(3) C9 0.116(6) 0.097(6) 0.040(4) 0.004(4) -0.002(4) -0.025(5) C10 0.162(8) 0.071(5) 0.047(4) 0.013(3) 0.039(5) -0.005(5) C11 0.111(6) 0.095(6) 0.090(6) 0.032(5) 0.060(5) 0.022(5) C12 0.082(5) 0.089(5) 0.058(4) 0.023(4) 0.030(3) 0.015(4) C13 0.030(2) 0.034(3) 0.035(3) -0.006(2) 0.003(2) -0.001(2) C14 0.038(3) 0.035(3) 0.041(3) -0.001(2) 0.009(2) 0.002(2) C15 0.027(2) 0.047(3) 0.051(3) -0.010(3) 0.009(2) -0.002(2) C16 0.042(3) 0.050(3) 0.066(4) 0.006(3) 0.018(3) -0.010(2) C17 0.049(3) 0.054(4) 0.083(4) 0.029(3) 0.017(3) -0.002(3) C18 0.031(2) 0.040(3) 0.061(3) 0.015(3) 0.006(2) 0.003(2) C19 0.031(3) 0.041(3) 0.036(3) 0.004(2) 0.004(2) 0.001(2) C20 0.039(3) 0.038(3) 0.059(3) 0.000(3) 0.008(2) 0.001(2) C21 0.057(4) 0.048(3) 0.085(5) 0.001(3) 0.016(3) 0.017(3) C22 0.044(3) 0.065(4) 0.077(4) 0.009(3) 0.009(3) 0.018(3) C23 0.028(3) 0.077(5) 0.080(4) -0.005(4) -0.001(3) 0.000(3) C24 0.031(3) 0.050(3) 0.062(3) -0.003(3) 0.005(2) -0.001(2) C25 0.050(3) 0.038(3) 0.034(3) 0.000(2) 0.006(2) 0.007(2) C26 0.057(3) 0.056(3) 0.042(3) 0.002(3) 0.007(3) 0.009(3) C27 0.082(4) 0.074(4) 0.053(4) -0.014(3) 0.013(3) 0.022(4) C28 0.098(6) 0.057(4) 0.065(4) -0.024(3) 0.007(4) 0.014(4) C29 0.098(6) 0.053(4) 0.061(4) -0.012(3) -0.007(4) -0.009(3) C30 0.057(3) 0.034(3) 0.045(3) -0.009(2) -0.001(2) -0.001(2) O26 0.049(2) 0.083(3) 0.065(3) -0.012(2) 0.022(2) -0.003(2) C31 0.059(4) 0.163(9) 0.101(6) -0.023(6) 0.042(4) -0.003(5) C40 0.120(16) 0.482(51) 0.090(14) -0.106(23) 0.025(12) -0.223(26) Cl3 0.201(6) 0.140(4) 0.089(3) 0.022(3) 0.054(4) 0.067(4) Cl4 0.096(2) 0.079(2) 0.106(3) -0.004(2) 0.053(2) 0.002(2) Cl5 0.053(2) 0.089(3) 0.097(3) 0.002(2) 0.015(2) 0.006(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 Pt1 P2 2.2029(12) . ? Pt1 S1 2.2948(12) . ? Pt1 Cl2 2.3164(13) . ? Pt1 Cl1 2.3515(12) . ? S1 P1 2.010(2) . ? P1 N1 1.688(4) . ? P1 C1 1.798(5) . ? P1 C7 1.803(5) . ? N1 C25 1.441(6) . ? N1 P2 1.735(4) . ? P2 C13 1.805(5) . ? P2 C19 1.811(5) . ? C1 C6 1.371(7) . ? C1 C2 1.406(7) . ? C2 C3 1.383(8) . ? C3 C4 1.380(9) . ? C4 C5 1.359(10) . ? C5 C6 1.374(9) . ? C7 C8 1.366(7) . ? C7 C12 1.388(8) . ? C8 C9 1.367(9) . ? C9 C10 1.358(10) . ? C10 C11 1.372(11) . ? C11 C12 1.392(9) . ? C13 C18 1.380(7) . ? C13 C14 1.410(6) . ? C14 C15 1.373(7) . ? C15 C16 1.371(8) . ? C16 C17 1.389(8) . ? C17 C18 1.369(7) . ? C19 C24 1.382(7) . ? C19 C20 1.389(7) . ? C20 C21 1.385(7) . ? C21 C22 1.367(9) . ? C22 C23 1.359(9) . ? C23 C24 1.380(8) . ? C25 C26 1.395(8) . ? C25 C30 1.394(7) . ? C26 O26 1.341(7) . ? C26 C27 1.422(8) . ? C27 C28 1.356(10) . ? C28 C29 1.355(10) . ? C29 C30 1.421(8) . ? O26 C31 1.431(7) . ? C40 Cl5 1.46(3) . ? C40 Cl4 1.73(2) . ? C40 Cl3 2.25(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 P2 Pt1 S1 92.53(4) . . ? P2 Pt1 Cl2 89.20(4) . . ? S1 Pt1 Cl2 175.45(4) . . ? P2 Pt1 Cl1 178.73(5) . . ? S1 Pt1 Cl1 88.46(5) . . ? Cl2 Pt1 Cl1 89.76(5) . . ? P1 S1 Pt1 97.43(6) . . ? N1 P1 C1 109.2(2) . . ? N1 P1 C7 110.2(2) . . ? C1 P1 C7 107.7(2) . . ? N1 P1 S1 108.52(14) . . ? C1 P1 S1 110.8(2) . . ? C7 P1 S1 110.4(2) . . ? C25 N1 P1 125.2(3) . . ? C25 N1 P2 118.3(3) . . ? P1 N1 P2 116.2(2) . . ? N1 P2 C13 104.8(2) . . ? N1 P2 C19 105.0(2) . . ? C13 P2 C19 107.5(2) . . ? N1 P2 Pt1 108.70(13) . . ? C13 P2 Pt1 115.41(15) . . ? C19 P2 Pt1 114.5(2) . . ? C6 C1 C2 118.2(5) . . ? C6 C1 P1 121.2(4) . . ? C2 C1 P1 120.6(4) . . ? C3 C2 C1 120.0(5) . . ? C4 C3 C2 120.0(6) . . ? C3 C4 C5 120.2(6) . . ? C6 C5 C4 120.2(6) . . ? C5 C6 C1 121.5(6) . . ? C8 C7 C12 119.0(5) . . ? C8 C7 P1 122.7(4) . . ? C12 C7 P1 118.1(4) . . ? C7 C8 C9 121.1(6) . . ? C10 C9 C8 120.9(7) . . ? C9 C10 C11 119.0(6) . . ? C10 C11 C12 120.9(7) . . ? C7 C12 C11 119.0(7) . . ? C18 C13 C14 118.4(4) . . ? C18 C13 P2 122.5(3) . . ? C14 C13 P2 118.9(4) . . ? C15 C14 C13 120.4(5) . . ? C14 C15 C16 120.2(5) . . ? C15 C16 C17 119.9(5) . . ? C18 C17 C16 120.3(5) . . ? C17 C18 C13 120.8(5) . . ? C24 C19 C20 119.0(5) . . ? C24 C19 P2 117.7(4) . . ? C20 C19 P2 123.3(4) . . ? C19 C20 C21 119.3(5) . . ? C22 C21 C20 121.1(6) . . ? C23 C22 C21 119.6(5) . . ? C22 C23 C24 120.6(6) . . ? C19 C24 C23 120.4(5) . . ? C26 C25 C30 119.8(5) . . ? C26 C25 N1 119.4(5) . . ? C30 C25 N1 120.4(4) . . ? O26 C26 C25 116.5(5) . . ? O26 C26 C27 125.1(6) . . ? C25 C26 C27 118.4(6) . . ? C28 C27 C26 120.1(6) . . ? C27 C28 C29 123.3(6) . . ? C28 C29 C30 117.8(6) . . ? C25 C30 C29 120.7(6) . . ? C26 O26 C31 119.1(5) . . ? Cl5 C40 Cl4 130.3(15) . . ? Cl5 C40 Cl3 101.7(11) . . ? Cl4 C40 Cl3 84.6(15) . . ? 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 P2 Pt1 S1 P1 32.43(6) . . . . ? Cl2 Pt1 S1 P1 144.7(6) . . . . ? Cl1 Pt1 S1 P1 -148.36(7) . . . . ? Pt1 S1 P1 N1 -40.84(15) . . . . ? Pt1 S1 P1 C1 79.1(2) . . . . ? Pt1 S1 P1 C7 -161.7(2) . . . . ? C1 P1 N1 C25 96.4(4) . . . . ? C7 P1 N1 C25 -21.7(4) . . . . ? S1 P1 N1 C25 -142.7(3) . . . . ? C1 P1 N1 P2 -89.3(3) . . . . ? C7 P1 N1 P2 152.6(2) . . . . ? S1 P1 N1 P2 31.6(2) . . . . ? C25 N1 P2 C13 -65.9(4) . . . . ? P1 N1 P2 C13 119.4(2) . . . . ? C25 N1 P2 C19 47.3(4) . . . . ? P1 N1 P2 C19 -127.4(2) . . . . ? C25 N1 P2 Pt1 170.2(3) . . . . ? P1 N1 P2 Pt1 -4.5(2) . . . . ? S1 Pt1 P2 N1 -19.73(13) . . . . ? Cl2 Pt1 P2 N1 164.48(14) . . . . ? Cl1 Pt1 P2 N1 -161.0(18) . . . . ? S1 Pt1 P2 C13 -137.1(2) . . . . ? Cl2 Pt1 P2 C13 47.1(2) . . . . ? Cl1 Pt1 P2 C13 81.6(18) . . . . ? S1 Pt1 P2 C19 97.3(2) . . . . ? Cl2 Pt1 P2 C19 -78.5(2) . . . . ? Cl1 Pt1 P2 C19 -44.0(19) . . . . ? N1 P1 C1 C6 131.1(4) . . . . ? C7 P1 C1 C6 -109.3(5) . . . . ? S1 P1 C1 C6 11.6(5) . . . . ? N1 P1 C1 C2 -48.6(5) . . . . ? C7 P1 C1 C2 71.1(5) . . . . ? S1 P1 C1 C2 -168.1(4) . . . . ? C6 C1 C2 C3 -0.3(8) . . . . ? P1 C1 C2 C3 179.4(4) . . . . ? C1 C2 C3 C4 0.1(9) . . . . ? C2 C3 C4 C5 1.0(11) . . . . ? C3 C4 C5 C6 -1.8(12) . . . . ? C4 C5 C6 C1 1.6(11) . . . . ? C2 C1 C6 C5 -0.5(9) . . . . ? P1 C1 C6 C5 179.8(5) . . . . ? N1 P1 C7 C8 105.5(5) . . . . ? C1 P1 C7 C8 -13.6(6) . . . . ? S1 P1 C7 C8 -134.7(5) . . . . ? N1 P1 C7 C12 -80.5(5) . . . . ? C1 P1 C7 C12 160.5(5) . . . . ? S1 P1 C7 C12 39.4(5) . . . . ? C12 C7 C8 C9 3.5(10) . . . . ? P1 C7 C8 C9 177.6(6) . . . . ? C7 C8 C9 C10 0.1(12) . . . . ? C8 C9 C10 C11 -2.2(12) . . . . ? C9 C10 C11 C12 0.6(13) . . . . ? C8 C7 C12 C11 -5.0(11) . . . . ? P1 C7 C12 C11 -179.3(6) . . . . ? C10 C11 C12 C7 3.0(12) . . . . ? N1 P2 C13 C18 137.4(4) . . . . ? C19 P2 C13 C18 26.0(5) . . . . ? Pt1 P2 C13 C18 -103.1(4) . . . . ? N1 P2 C13 C14 -47.4(4) . . . . ? C19 P2 C13 C14 -158.8(4) . . . . ? Pt1 P2 C13 C14 72.1(4) . . . . ? C18 C13 C14 C15 -1.8(7) . . . . ? P2 C13 C14 C15 -177.2(4) . . . . ? C13 C14 C15 C16 1.2(8) . . . . ? C14 C15 C16 C17 -0.3(8) . . . . ? C15 C16 C17 C18 -0.1(10) . . . . ? C16 C17 C18 C13 -0.6(9) . . . . ? C14 C13 C18 C17 1.5(8) . . . . ? P2 C13 C18 C17 176.7(5) . . . . ? N1 P2 C19 C24 101.8(4) . . . . ? C13 P2 C19 C24 -147.0(4) . . . . ? Pt1 P2 C19 C24 -17.3(5) . . . . ? N1 P2 C19 C20 -74.6(5) . . . . ? C13 P2 C19 C20 36.6(5) . . . . ? Pt1 P2 C19 C20 166.3(4) . . . . ? C24 C19 C20 C21 -1.4(8) . . . . ? P2 C19 C20 C21 174.9(4) . . . . ? C19 C20 C21 C22 0.7(9) . . . . ? C20 C21 C22 C23 0.3(10) . . . . ? C21 C22 C23 C24 -0.5(11) . . . . ? C20 C19 C24 C23 1.3(8) . . . . ? P2 C19 C24 C23 -175.3(5) . . . . ? C22 C23 C24 C19 -0.3(10) . . . . ? P1 N1 C25 C26 85.0(5) . . . . ? P2 N1 C25 C26 -89.2(5) . . . . ? P1 N1 C25 C30 -102.8(5) . . . . ? P2 N1 C25 C30 83.0(5) . . . . ? C30 C25 C26 O26 -177.6(5) . . . . ? N1 C25 C26 O26 -5.3(7) . . . . ? C30 C25 C26 C27 1.3(8) . . . . ? N1 C25 C26 C27 173.5(5) . . . . ? O26 C26 C27 C28 177.2(6) . . . . ? C25 C26 C27 C28 -1.6(9) . . . . ? C26 C27 C28 C29 1.4(11) . . . . ? C27 C28 C29 C30 -0.9(11) . . . . ? C26 C25 C30 C29 -0.9(8) . . . . ? N1 C25 C30 C29 -173.0(5) . . . . ? C28 C29 C30 C25 0.6(9) . . . . ? C25 C26 O26 C31 173.6(6) . . . . ? C27 C26 O26 C31 -5.2(9) . . . . ? _refine_diff_density_max 1.200 _refine_diff_density_min -0.573 _refine_diff_density_rms 0.104 #---end data_11 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 'C35 H27 Mo N O5 P2' _chemical_formula_moiety 'C35 H27 Mo N O5 P2' _chemical_formula_structural 'C35 H27 Mo N O5 P2' _chemical_formula_analytical 'C35 H27 Mo N O5 P2' _chemical_formula_sum 'C35 H27 Mo N O5 P2' _chemical_formula_weight 699.46 _chemical_melting_point - _chemical_compound_source - 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 9.07320(10) _cell_length_b 18.9395(2) _cell_length_c 19.28230(10) _cell_angle_alpha 90.00 _cell_angle_beta 96.8620(10) _cell_angle_gamma 90.00 _cell_volume 3289.77(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 61 _cell_measurement_theta_min 12 _cell_measurement_theta_max 168 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max .3 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .1 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.412 _exptl_crystal_density_method - _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 0.538 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.840270 _exptl_absorpt_correction_T_max 1.0000 _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 SMART _diffrn_measurement_method CCD _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time - _diffrn_standards_decay_% - _diffrn_reflns_number 13779 _diffrn_reflns_av_R_equivalents 0.0173 _diffrn_reflns_av_sigmaI/netI 0.0207 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 23.22 _reflns_number_total 4677 _reflns_number_observed 4060 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 50 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0451P)^2^+0.1631P] 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 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0030(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4627 _refine_ls_number_parameters 398 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0289 _refine_ls_R_factor_obs 0.0209 _refine_ls_wR_factor_all 0.0736 _refine_ls_wR_factor_obs 0.0563 _refine_ls_goodness_of_fit_all 0.943 _refine_ls_goodness_of_fit_obs 0.966 _refine_ls_restrained_S_all 1.174 _refine_ls_restrained_S_obs 0.966 _refine_ls_shift/esd_max 0.003 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo 0.22207(2) 0.130952(8) 0.450290(8) 0.03230(9) Uani 1 d . . P1 P 0.05176(5) 0.13769(2) 0.33789(3) 0.03261(13) Uani 1 d . . N1 N 0.0156(2) 0.22681(8) 0.34568(8) 0.0337(4) Uani 1 d . . P2 P 0.09530(5) 0.24681(2) 0.42930(2) 0.03303(13) Uani 1 d . . C1 C 0.1313(2) 0.12187(10) 0.25598(10) 0.0395(5) Uani 1 d . . C2 C 0.1272(3) 0.05344(13) 0.22985(13) 0.0641(7) Uani 1 d . . H2A H 0.0774(3) 0.01849(13) 0.25166(13) 0.077 Uiso 1 calc R . C3 C 0.1963(3) 0.0366(2) 0.17176(15) 0.0777(8) Uani 1 d . . H3A H 0.1933(3) -0.0096(2) 0.15529(15) 0.093 Uiso 1 calc R . C4 C 0.2687(3) 0.0873(2) 0.13841(14) 0.0729(8) Uani 1 d . . H4A H 0.3131(3) 0.0761(2) 0.09876(14) 0.087 Uiso 1 calc R . C5 C 0.2750(3) 0.1544(2) 0.1641(2) 0.0774(8) Uani 1 d . . H5A H 0.3246(3) 0.1890(2) 0.1418(2) 0.093 Uiso 1 calc R . C6 C 0.2083(3) 0.17179(13) 0.22309(13) 0.0609(6) Uani 1 d . . H6A H 0.2160(3) 0.21762(13) 0.24047(13) 0.073 Uiso 1 calc R . C7 C -0.1297(2) 0.09457(10) 0.31927(10) 0.0361(4) Uani 1 d . . C8 C -0.2164(2) 0.10371(12) 0.25518(11) 0.0500(5) Uani 1 d . . H8A H -0.1799(2) 0.13011(12) 0.22031(11) 0.060 Uiso 1 calc R . C9 C -0.3567(2) 0.07369(13) 0.24299(13) 0.0606(6) Uani 1 d . . H9A H -0.4140(2) 0.08028(13) 0.20018(13) 0.073 Uiso 1 calc R . C10 C -0.4114(2) 0.03390(13) 0.29458(14) 0.0595(6) Uani 1 d . . H10A H -0.5056(2) 0.01398(13) 0.28649(14) 0.071 Uiso 1 calc R . C11 C -0.3264(2) 0.02396(12) 0.35762(13) 0.0543(6) Uani 1 d . . H11A H -0.3629(2) -0.00297(12) 0.39211(13) 0.065 Uiso 1 calc R . C12 C -0.1859(2) 0.05399(10) 0.37012(11) 0.0430(5) Uani 1 d . . H12A H -0.1290(2) 0.04685(10) 0.41294(11) 0.052 Uiso 1 calc R . C13 C -0.0575(2) 0.26842(10) 0.47987(10) 0.0384(5) Uani 1 d . . C14 C -0.0506(3) 0.32329(14) 0.52717(13) 0.0668(7) Uani 1 d . . H14A H 0.0282(3) 0.35492(14) 0.52987(13) 0.080 Uiso 1 calc R . C15 C -0.1608(4) 0.3317(2) 0.5709(2) 0.0934(10) Uani 1 d . . H15A H -0.1557(4) 0.3694(2) 0.6019(2) 0.112 Uiso 1 calc R . C16 C -0.2767(3) 0.2850(2) 0.56886(15) 0.0794(8) Uani 1 d . . H16A H -0.3483(3) 0.2900(2) 0.59923(15) 0.095 Uiso 1 calc R . C17 C -0.2853(3) 0.23138(15) 0.52181(14) 0.0654(7) Uani 1 d . . H17A H -0.3649(3) 0.20020(15) 0.51926(14) 0.078 Uiso 1 calc R . C18 C -0.1777(2) 0.22243(12) 0.47774(11) 0.0502(5) Uani 1 d . . H18A H -0.1855(2) 0.18513(12) 0.44615(11) 0.060 Uiso 1 calc R . C19 C 0.1915(2) 0.33151(10) 0.42613(11) 0.0424(5) Uani 1 d . . C20 C 0.3438(3) 0.33372(13) 0.44499(13) 0.0591(6) Uani 1 d . . H20A H 0.3950(3) 0.29251(13) 0.45857(13) 0.071 Uiso 1 calc R . C21 C 0.4205(3) 0.3975(2) 0.4437(2) 0.0812(9) Uani 1 d . . H21A H 0.5227(3) 0.3987(2) 0.4562(2) 0.097 Uiso 1 calc R . C22 C 0.3451(4) 0.4580(2) 0.4241(2) 0.0945(10) Uani 1 d . . H22A H 0.3962(4) 0.5005(2) 0.4236(2) 0.113 Uiso 1 calc R . C23 C 0.1942(4) 0.45656(13) 0.4051(2) 0.0907(10) Uani 1 d . . H23A H 0.1440(4) 0.49796(13) 0.3913(2) 0.109 Uiso 1 calc R . C24 C 0.1171(3) 0.39395(12) 0.40662(13) 0.0630(7) Uani 1 d . . H24A H 0.0148(3) 0.39346(12) 0.39452(13) 0.076 Uiso 1 calc R . C25 C -0.0839(2) 0.27108(10) 0.30034(10) 0.0382(4) Uani 1 d . . C26 C -0.0263(2) 0.32031(10) 0.25628(10) 0.0438(5) Uani 1 d . . C27 C -0.1233(3) 0.36128(12) 0.21122(12) 0.0611(7) Uani 1 d . . H27A H -0.0860(3) 0.39326(12) 0.18115(12) 0.073 Uiso 1 calc R . C28 C -0.2742(3) 0.35427(15) 0.2114(2) 0.0759(8) Uani 1 d . . H28A H -0.3383(3) 0.38147(15) 0.1810(2) 0.091 Uiso 1 calc R . C29 C -0.3312(3) 0.30797(14) 0.2554(2) 0.0737(8) Uani 1 d . . H29A H -0.4334(3) 0.30432(14) 0.2554(2) 0.088 Uiso 1 calc R . C30 C -0.2368(2) 0.26639(12) 0.30019(12) 0.0538(6) Uani 1 d . . H30A H -0.2761(2) 0.23513(12) 0.33034(12) 0.065 Uiso 1 calc R . O26 O 0.1249(2) 0.32499(7) 0.26142(8) 0.0556(4) Uani 1 d . . C261 C 0.1904(4) 0.3781(2) 0.2225(2) 0.0931(11) Uani 1 d . . H26A H 0.2966(4) 0.3749(2) 0.2314(2) 0.140 Uiso 1 calc R . H26B H 0.1589(4) 0.4239(2) 0.2364(2) 0.140 Uiso 1 calc R . H26C H 0.1598(4) 0.3714(2) 0.1736(2) 0.140 Uiso 1 calc R . C31 C 0.0693(2) 0.09711(10) 0.51200(11) 0.0393(5) Uani 1 d . . O31 O -0.0099(2) 0.07784(9) 0.55008(8) 0.0589(4) Uani 1 d . . C32 C 0.3458(2) 0.15395(12) 0.54022(11) 0.0442(5) Uani 1 d . . O32 O 0.4117(2) 0.16885(11) 0.59277(9) 0.0721(5) Uani 1 d . . C33 C 0.2978(2) 0.03129(12) 0.44411(12) 0.0479(5) Uani 1 d . . O33 O 0.3425(2) -0.02487(9) 0.43934(11) 0.0795(6) Uani 1 d . . C34 C 0.3889(2) 0.16329(11) 0.39516(11) 0.0461(5) Uani 1 d . . O34 O 0.4839(2) 0.18150(10) 0.36579(10) 0.0776(5) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.02684(11) 0.03383(12) 0.03551(12) 0.00380(7) 0.00076(7) -0.00103(6) P1 0.0296(3) 0.0337(3) 0.0340(3) 0.0019(2) 0.0018(2) -0.0022(2) N1 0.0310(8) 0.0342(8) 0.0353(9) 0.0045(7) 0.0010(6) -0.0003(7) P2 0.0296(3) 0.0322(3) 0.0366(3) 0.0023(2) 0.0011(2) -0.0034(2) C1 0.0325(11) 0.0460(12) 0.0392(11) 0.0001(9) 0.0016(8) 0.0024(9) C2 0.063(2) 0.0597(15) 0.074(2) -0.0206(13) 0.0228(12) -0.0119(12) C3 0.063(2) 0.089(2) 0.082(2) -0.043(2) 0.0171(14) -0.002(2) C4 0.052(2) 0.116(2) 0.052(2) -0.012(2) 0.0128(12) 0.020(2) C5 0.075(2) 0.087(2) 0.078(2) 0.024(2) 0.0396(15) 0.016(2) C6 0.064(2) 0.0530(14) 0.071(2) 0.0075(12) 0.0316(13) 0.0054(12) C7 0.0334(10) 0.0345(10) 0.0399(11) -0.0028(8) 0.0022(8) -0.0029(8) C8 0.0428(12) 0.0627(14) 0.0435(13) 0.0002(10) 0.0007(9) -0.0054(11) C9 0.0424(13) 0.077(2) 0.0582(15) -0.0139(13) -0.0113(11) 0.0023(12) C10 0.0346(12) 0.0595(14) 0.084(2) -0.0171(13) 0.0067(12) -0.0084(10) C11 0.0485(13) 0.0466(12) 0.069(2) -0.0008(11) 0.0133(11) -0.0124(10) C12 0.0421(12) 0.0388(11) 0.0469(12) -0.0001(9) 0.0004(9) -0.0044(9) C13 0.0393(11) 0.0411(11) 0.0342(11) 0.0006(8) 0.0015(8) 0.0025(9) C14 0.075(2) 0.069(2) 0.059(2) -0.0192(13) 0.0173(13) -0.0167(13) C15 0.131(3) 0.085(2) 0.072(2) -0.035(2) 0.046(2) -0.009(2) C16 0.081(2) 0.094(2) 0.071(2) 0.000(2) 0.041(2) 0.010(2) C17 0.0469(14) 0.081(2) 0.071(2) 0.0016(14) 0.0204(12) -0.0007(13) C18 0.0427(12) 0.0560(13) 0.0532(14) -0.0082(10) 0.0118(10) -0.0043(10) C19 0.0461(12) 0.0375(11) 0.0424(12) 0.0004(9) -0.0001(9) -0.0091(9) C20 0.0492(14) 0.0532(14) 0.074(2) -0.0033(12) 0.0028(11) -0.0158(11) C21 0.065(2) 0.073(2) 0.104(2) -0.004(2) 0.001(2) -0.035(2) C22 0.118(3) 0.062(2) 0.098(2) 0.014(2) -0.009(2) -0.051(2) C23 0.117(3) 0.0403(15) 0.105(2) 0.0162(14) -0.028(2) -0.021(2) C24 0.070(2) 0.0424(13) 0.072(2) 0.0050(12) -0.0133(13) -0.0099(11) C25 0.0395(11) 0.0373(10) 0.0363(11) 0.0001(8) -0.0020(8) 0.0029(9) C26 0.0533(13) 0.0398(11) 0.0382(11) 0.0035(9) 0.0048(9) 0.0040(10) C27 0.085(2) 0.0481(13) 0.0485(14) 0.0125(10) 0.0013(12) 0.0108(12) C28 0.077(2) 0.068(2) 0.074(2) 0.0091(14) -0.0259(15) 0.0236(15) C29 0.0441(14) 0.075(2) 0.096(2) 0.004(2) -0.0174(13) 0.0121(13) C30 0.0399(13) 0.0546(13) 0.066(2) 0.0050(11) 0.0005(10) 0.0020(10) O26 0.0571(10) 0.0481(9) 0.0643(10) 0.0190(7) 0.0185(7) -0.0014(7) C261 0.090(2) 0.082(2) 0.116(3) 0.050(2) 0.046(2) 0.001(2) C31 0.0386(11) 0.0371(11) 0.0408(12) 0.0022(9) -0.0015(9) -0.0027(9) O31 0.0565(10) 0.0697(10) 0.0532(10) 0.0087(8) 0.0174(8) -0.0089(8) C32 0.0339(11) 0.0553(12) 0.0435(13) 0.0063(10) 0.0045(9) -0.0068(10) O32 0.0538(10) 0.1102(15) 0.0490(10) -0.0032(9) -0.0070(8) -0.0207(10) C33 0.0400(12) 0.0473(13) 0.0566(14) 0.0019(10) 0.0063(9) -0.0018(10) O33 0.0722(12) 0.0439(10) 0.125(2) -0.0051(10) 0.0203(11) 0.0125(9) C34 0.0381(12) 0.0470(12) 0.0528(13) -0.0036(10) 0.0040(10) -0.0039(10) O34 0.0587(11) 0.0909(13) 0.0901(13) -0.0094(10) 0.0370(10) -0.0230(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 Mo1 C32 1.998(2) . ? Mo1 C33 2.017(2) . ? Mo1 C31 2.035(2) . ? Mo1 C34 2.045(2) . ? Mo1 P2 2.4880(5) . ? Mo1 P1 2.5102(5) . ? P1 N1 1.729(2) . ? P1 C7 1.835(2) . ? P1 C1 1.838(2) . ? N1 C25 1.447(2) . ? N1 P2 1.7285(15) . ? P2 C19 1.831(2) . ? P2 C13 1.834(2) . ? C1 C6 1.375(3) . ? C1 C2 1.389(3) . ? C2 C3 1.384(3) . ? C3 C4 1.366(4) . ? C4 C5 1.363(4) . ? C5 C6 1.390(4) . ? C7 C12 1.390(3) . ? C7 C8 1.394(3) . ? C8 C9 1.389(3) . ? C9 C10 1.386(4) . ? C10 C11 1.373(3) . ? C11 C12 1.390(3) . ? C13 C14 1.379(3) . ? C13 C18 1.392(3) . ? C14 C15 1.391(4) . ? C15 C16 1.371(4) . ? C16 C17 1.358(4) . ? C17 C18 1.379(3) . ? C19 C20 1.387(3) . ? C19 C24 1.391(3) . ? C20 C21 1.395(3) . ? C21 C22 1.364(4) . ? C22 C23 1.374(4) . ? C23 C24 1.379(3) . ? C25 C30 1.390(3) . ? C25 C26 1.404(3) . ? C26 O26 1.367(3) . ? C26 C27 1.396(3) . ? C27 C28 1.376(4) . ? C28 C29 1.365(4) . ? C29 C30 1.386(3) . ? O26 C261 1.426(3) . ? C31 O31 1.147(2) . ? C32 O32 1.149(2) . ? C33 O33 1.146(3) . ? C34 O34 1.139(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 C32 Mo1 C33 95.47(9) . . ? C32 Mo1 C31 84.97(8) . . ? C33 Mo1 C31 90.02(8) . . ? C32 Mo1 C34 90.68(8) . . ? C33 Mo1 C34 88.34(8) . . ? C31 Mo1 C34 175.19(8) . . ? C32 Mo1 P2 98.61(6) . . ? C33 Mo1 P2 165.88(6) . . ? C31 Mo1 P2 92.24(5) . . ? C34 Mo1 P2 90.45(6) . . ? C32 Mo1 P1 164.23(6) . . ? C33 Mo1 P1 100.10(6) . . ? C31 Mo1 P1 97.41(5) . . ? C34 Mo1 P1 87.34(6) . . ? P2 Mo1 P1 65.78(2) . . ? N1 P1 C7 106.04(8) . . ? N1 P1 C1 109.38(8) . . ? C7 P1 C1 101.22(9) . . ? N1 P1 Mo1 94.49(5) . . ? C7 P1 Mo1 126.29(6) . . ? C1 P1 Mo1 117.99(6) . . ? C25 N1 P2 126.73(12) . . ? C25 N1 P1 128.62(12) . . ? P2 N1 P1 103.43(8) . . ? N1 P2 C19 107.98(8) . . ? N1 P2 C13 106.63(8) . . ? C19 P2 C13 102.47(9) . . ? N1 P2 Mo1 95.29(5) . . ? C19 P2 Mo1 124.42(7) . . ? C13 P2 Mo1 118.33(6) . . ? C6 C1 C2 117.9(2) . . ? C6 C1 P1 123.9(2) . . ? C2 C1 P1 117.9(2) . . ? C3 C2 C1 120.9(2) . . ? C4 C3 C2 120.6(3) . . ? C3 C4 C5 119.0(2) . . ? C4 C5 C6 121.0(3) . . ? C1 C6 C5 120.6(2) . . ? C12 C7 C8 118.6(2) . . ? C12 C7 P1 120.29(14) . . ? C8 C7 P1 121.07(15) . . ? C9 C8 C7 120.5(2) . . ? C10 C9 C8 120.1(2) . . ? C11 C10 C9 119.9(2) . . ? C10 C11 C12 120.3(2) . . ? C7 C12 C11 120.7(2) . . ? C14 C13 C18 117.7(2) . . ? C14 C13 P2 122.8(2) . . ? C18 C13 P2 118.93(15) . . ? C13 C14 C15 120.5(2) . . ? C16 C15 C14 120.9(3) . . ? C17 C16 C15 118.9(2) . . ? C16 C17 C18 121.0(2) . . ? C17 C18 C13 121.0(2) . . ? C20 C19 C24 118.8(2) . . ? C20 C19 P2 118.8(2) . . ? C24 C19 P2 122.4(2) . . ? C19 C20 C21 120.3(2) . . ? C22 C21 C20 119.8(3) . . ? C21 C22 C23 120.5(2) . . ? C22 C23 C24 120.2(3) . . ? C23 C24 C19 120.4(2) . . ? C30 C25 C26 119.0(2) . . ? C30 C25 N1 121.0(2) . . ? C26 C25 N1 120.0(2) . . ? O26 C26 C27 124.2(2) . . ? O26 C26 C25 116.2(2) . . ? C27 C26 C25 119.6(2) . . ? C28 C27 C26 119.9(2) . . ? C29 C28 C27 120.9(2) . . ? C28 C29 C30 120.0(2) . . ? C29 C30 C25 120.5(2) . . ? C26 O26 C261 119.0(2) . . ? O31 C31 Mo1 175.8(2) . . ? O32 C32 Mo1 177.0(2) . . ? O33 C33 Mo1 178.4(2) . . ? O34 C34 Mo1 178.5(2) . . ? 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 C32 Mo1 P1 N1 -2.1(2) . . . . ? C33 Mo1 P1 N1 -173.02(8) . . . . ? C31 Mo1 P1 N1 95.63(7) . . . . ? C34 Mo1 P1 N1 -85.18(8) . . . . ? P2 Mo1 P1 N1 6.51(5) . . . . ? C32 Mo1 P1 C7 -115.8(2) . . . . ? C33 Mo1 P1 C7 73.31(10) . . . . ? C31 Mo1 P1 C7 -18.04(9) . . . . ? C34 Mo1 P1 C7 161.15(10) . . . . ? P2 Mo1 P1 C7 -107.16(8) . . . . ? C32 Mo1 P1 C1 112.6(2) . . . . ? C33 Mo1 P1 C1 -58.28(9) . . . . ? C31 Mo1 P1 C1 -149.62(9) . . . . ? C34 Mo1 P1 C1 29.56(9) . . . . ? P2 Mo1 P1 C1 121.26(7) . . . . ? C7 P1 N1 C25 -46.9(2) . . . . ? C1 P1 N1 C25 61.5(2) . . . . ? Mo1 P1 N1 C25 -176.70(15) . . . . ? C7 P1 N1 P2 121.01(9) . . . . ? C1 P1 N1 P2 -130.58(9) . . . . ? Mo1 P1 N1 P2 -8.80(7) . . . . ? C25 N1 P2 C19 -54.1(2) . . . . ? P1 N1 P2 C19 137.72(9) . . . . ? C25 N1 P2 C13 55.4(2) . . . . ? P1 N1 P2 C13 -112.78(9) . . . . ? C25 N1 P2 Mo1 177.10(14) . . . . ? P1 N1 P2 Mo1 8.89(7) . . . . ? C32 Mo1 P2 N1 171.12(8) . . . . ? C33 Mo1 P2 N1 -4.6(3) . . . . ? C31 Mo1 P2 N1 -103.64(7) . . . . ? C34 Mo1 P2 N1 80.36(8) . . . . ? P1 Mo1 P2 N1 -6.52(5) . . . . ? C32 Mo1 P2 C19 55.05(10) . . . . ? C33 Mo1 P2 C19 -120.7(3) . . . . ? C31 Mo1 P2 C19 140.30(10) . . . . ? C34 Mo1 P2 C19 -35.71(10) . . . . ? P1 Mo1 P2 C19 -122.59(8) . . . . ? C32 Mo1 P2 C13 -76.77(9) . . . . ? C33 Mo1 P2 C13 107.5(3) . . . . ? C31 Mo1 P2 C13 8.48(9) . . . . ? C34 Mo1 P2 C13 -167.53(9) . . . . ? P1 Mo1 P2 C13 105.59(7) . . . . ? N1 P1 C1 C6 26.0(2) . . . . ? C7 P1 C1 C6 137.6(2) . . . . ? Mo1 P1 C1 C6 -80.3(2) . . . . ? N1 P1 C1 C2 -161.2(2) . . . . ? C7 P1 C1 C2 -49.6(2) . . . . ? Mo1 P1 C1 C2 92.4(2) . . . . ? C6 C1 C2 C3 -1.2(4) . . . . ? P1 C1 C2 C3 -174.4(2) . . . . ? C1 C2 C3 C4 -0.7(4) . . . . ? C2 C3 C4 C5 1.5(4) . . . . ? C3 C4 C5 C6 -0.4(4) . . . . ? C2 C1 C6 C5 2.3(4) . . . . ? P1 C1 C6 C5 175.1(2) . . . . ? C4 C5 C6 C1 -1.6(4) . . . . ? N1 P1 C7 C12 -107.5(2) . . . . ? C1 P1 C7 C12 138.3(2) . . . . ? Mo1 P1 C7 C12 0.7(2) . . . . ? N1 P1 C7 C8 70.2(2) . . . . ? C1 P1 C7 C8 -44.0(2) . . . . ? Mo1 P1 C7 C8 178.34(14) . . . . ? C12 C7 C8 C9 1.0(3) . . . . ? P1 C7 C8 C9 -176.7(2) . . . . ? C7 C8 C9 C10 -0.4(3) . . . . ? C8 C9 C10 C11 -0.3(4) . . . . ? C9 C10 C11 C12 0.4(3) . . . . ? C8 C7 C12 C11 -0.9(3) . . . . ? P1 C7 C12 C11 176.9(2) . . . . ? C10 C11 C12 C7 0.2(3) . . . . ? N1 P2 C13 C14 -139.0(2) . . . . ? C19 P2 C13 C14 -25.7(2) . . . . ? Mo1 P2 C13 C14 115.3(2) . . . . ? N1 P2 C13 C18 49.7(2) . . . . ? C19 P2 C13 C18 163.1(2) . . . . ? Mo1 P2 C13 C18 -55.9(2) . . . . ? C18 C13 C14 C15 0.0(4) . . . . ? P2 C13 C14 C15 -171.3(2) . . . . ? C13 C14 C15 C16 1.2(5) . . . . ? C14 C15 C16 C17 -2.1(5) . . . . ? C15 C16 C17 C18 1.7(4) . . . . ? C16 C17 C18 C13 -0.4(4) . . . . ? C14 C13 C18 C17 -0.4(3) . . . . ? P2 C13 C18 C17 171.3(2) . . . . ? N1 P2 C19 C20 -118.3(2) . . . . ? C13 P2 C19 C20 129.4(2) . . . . ? Mo1 P2 C19 C20 -8.4(2) . . . . ? N1 P2 C19 C24 62.8(2) . . . . ? C13 P2 C19 C24 -49.5(2) . . . . ? Mo1 P2 C19 C24 172.7(2) . . . . ? C24 C19 C20 C21 -0.6(4) . . . . ? P2 C19 C20 C21 -179.5(2) . . . . ? C19 C20 C21 C22 0.3(4) . . . . ? C20 C21 C22 C23 -0.5(5) . . . . ? C21 C22 C23 C24 0.9(5) . . . . ? C22 C23 C24 C19 -1.1(5) . . . . ? C20 C19 C24 C23 1.0(4) . . . . ? P2 C19 C24 C23 179.9(2) . . . . ? P2 N1 C25 C30 -91.2(2) . . . . ? P1 N1 C25 C30 74.1(2) . . . . ? P2 N1 C25 C26 88.0(2) . . . . ? P1 N1 C25 C26 -106.8(2) . . . . ? C30 C25 C26 O26 176.7(2) . . . . ? N1 C25 C26 O26 -2.5(3) . . . . ? C30 C25 C26 C27 -2.7(3) . . . . ? N1 C25 C26 C27 178.1(2) . . . . ? O26 C26 C27 C28 -178.0(2) . . . . ? C25 C26 C27 C28 1.4(3) . . . . ? C26 C27 C28 C29 0.4(4) . . . . ? C27 C28 C29 C30 -1.0(4) . . . . ? C28 C29 C30 C25 -0.4(4) . . . . ? C26 C25 C30 C29 2.2(3) . . . . ? N1 C25 C30 C29 -178.6(2) . . . . ? C27 C26 O26 C261 4.7(3) . . . . ? C25 C26 O26 C261 -174.7(2) . . . . ? C32 Mo1 C31 O31 -18.4(24) . . . . ? C33 Mo1 C31 O31 77.1(24) . . . . ? C34 Mo1 C31 O31 7.0(30) . . . . ? P2 Mo1 C31 O31 -116.8(24) . . . . ? P1 Mo1 C31 O31 177.3(1000) . . . . ? C33 Mo1 C32 O32 -142.5(37) . . . . ? C31 Mo1 C32 O32 -52.9(37) . . . . ? C34 Mo1 C32 O32 129.1(37) . . . . ? P2 Mo1 C32 O32 38.6(37) . . . . ? P1 Mo1 C32 O32 46.5(38) . . . . ? C32 Mo1 C33 O33 -109.9(72) . . . . ? C31 Mo1 C33 O33 165.2(72) . . . . ? C34 Mo1 C33 O33 -19.3(72) . . . . ? P2 Mo1 C33 O33 65.9(72) . . . . ? P1 Mo1 C33 O33 67.7(72) . . . . ? C32 Mo1 C34 O34 6.1(75) . . . . ? C33 Mo1 C34 O34 -89.4(75) . . . . ? C31 Mo1 C34 O34 -19.2(81) . . . . ? P2 Mo1 C34 O34 104.7(75) . . . . ? P1 Mo1 C34 O34 170.4(1000) . . . . ? _refine_diff_density_max 0.242 _refine_diff_density_min -0.199 _refine_diff_density_rms 0.036 #---end data_12 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common - _chemical_formula_moiety 'C62 H54 Cu N2 O2 P4'.F6 P' _chemical_formula_structural 'C62 H54 Cu F6 N2 O2 P5' _chemical_formula_analytical 'C62 H54 Cu F6 N2 O2 P5' _chemical_formula_sum 'C62 H54 Cu F6 N2 O2 P5' _chemical_formula_weight 1191.46 _chemical_melting_point - _chemical_compound_source - 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' 'Cu' 'Cu' 0.3201 1.2651 '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 11.1500(2) _cell_length_b 30.8735(4) _cell_length_c 17.2571(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.3930(10) _cell_angle_gamma 90.00 _cell_volume 5923.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 75 _cell_measurement_theta_min 12 _cell_measurement_theta_max 168 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.336 _exptl_crystal_density_method - _exptl_crystal_F_000 2456 _exptl_absorpt_coefficient_mu 0.567 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.619494 _exptl_absorpt_correction_T_max 1.000000 _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 SMART _diffrn_measurement_method CCD _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time - _diffrn_standards_decay_% - _diffrn_reflns_number 35606 _diffrn_reflns_av_R_equivalents 0.0718 _diffrn_reflns_av_sigmaI/netI 0.1236 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 28.27 _reflns_number_total 13891 _reflns_number_observed 5978 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 51 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0872P)^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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0016(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 13840 _refine_ls_number_parameters 704 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1745 _refine_ls_R_factor_obs 0.0578 _refine_ls_wR_factor_all 0.2015 _refine_ls_wR_factor_obs 0.1269 _refine_ls_goodness_of_fit_all 0.963 _refine_ls_goodness_of_fit_obs 1.010 _refine_ls_restrained_S_all 1.032 _refine_ls_restrained_S_obs 1.010 _refine_ls_shift/esd_max 0.049 _refine_ls_shift/esd_mean 0.003 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.37321(5) 0.11599(2) 0.78278(3) 0.0461(2) Uani 1 d . . P1 P 0.42116(10) 0.07151(4) 0.68272(6) 0.0430(3) Uani 1 d . . N1 N 0.2712(3) 0.06630(10) 0.6529(2) 0.0422(8) Uani 1 d . . P2 P 0.19409(10) 0.10045(4) 0.70994(7) 0.0460(3) Uani 1 d . . C1 C 0.4820(4) 0.01729(13) 0.7006(2) 0.0450(10) Uani 1 d . . C2 C 0.6036(4) 0.0101(2) 0.6977(3) 0.0711(15) Uani 1 d . . H2A H 0.6528(4) 0.0322(2) 0.6818(3) 0.085 Uiso 1 calc R . C3 C 0.6532(5) -0.0301(2) 0.7185(3) 0.088(2) Uani 1 d . . H3A H 0.7354(5) -0.0346(2) 0.7165(3) 0.105 Uiso 1 calc R . C4 C 0.5819(6) -0.0631(2) 0.7417(3) 0.078(2) Uani 1 d . . H4A H 0.6150(6) -0.0900(2) 0.7545(3) 0.094 Uiso 1 calc R . C5 C 0.4638(5) -0.0561(2) 0.7457(3) 0.0739(15) Uani 1 d . . H5A H 0.4152(5) -0.0784(2) 0.7614(3) 0.089 Uiso 1 calc R . C6 C 0.4133(4) -0.01616(15) 0.7270(3) 0.0613(13) Uani 1 d . . H6A H 0.3318(4) -0.01173(15) 0.7322(3) 0.074 Uiso 1 calc R . C7 C 0.4950(4) 0.08939(14) 0.5980(3) 0.0508(11) Uani 1 d . . C8 C 0.5207(5) 0.0614(2) 0.5388(3) 0.0682(14) Uani 1 d . . H8A H 0.5050(5) 0.0319(2) 0.5435(3) 0.082 Uiso 1 calc R . C9 C 0.5694(5) 0.0768(2) 0.4730(3) 0.083(2) Uani 1 d . . H9A H 0.5844(5) 0.0578(2) 0.4330(3) 0.100 Uiso 1 calc R . C10 C 0.5959(6) 0.1201(2) 0.4663(4) 0.098(2) Uani 1 d . . H10A H 0.6302(6) 0.1303(2) 0.4223(4) 0.118 Uiso 1 calc R . C11 C 0.5717(6) 0.1482(2) 0.5243(4) 0.095(2) Uani 1 d . . H11A H 0.5895(6) 0.1775(2) 0.5201(4) 0.114 Uiso 1 calc R . C12 C 0.5200(5) 0.1325(2) 0.5899(3) 0.0730(15) Uani 1 d . . H12A H 0.5022(5) 0.1517(2) 0.6288(3) 0.088 Uiso 1 calc R . C13 C 0.0737(4) 0.0691(2) 0.7481(3) 0.0562(12) Uani 1 d . . C14 C 0.0831(5) 0.0254(2) 0.7627(4) 0.087(2) Uani 1 d . . H14A H 0.1502(5) 0.0106(2) 0.7478(4) 0.104 Uiso 1 calc R . C15 C -0.0036(7) 0.0027(2) 0.7989(4) 0.119(3) Uani 1 d . . H15A H 0.0041(7) -0.0270(2) 0.8060(4) 0.143 Uiso 1 calc R . C16 C -0.0994(7) 0.0238(3) 0.8238(5) 0.131(3) Uani 1 d . . H16A H -0.1568(7) 0.0087(3) 0.8494(5) 0.157 Uiso 1 calc R . C17 C -0.1115(6) 0.0668(3) 0.8114(5) 0.122(3) Uani 1 d . . H17A H -0.1777(6) 0.0812(3) 0.8286(5) 0.146 Uiso 1 calc R . C18 C -0.0263(5) 0.0900(2) 0.7731(4) 0.087(2) Uani 1 d . . H18A H -0.0367(5) 0.1195(2) 0.7644(4) 0.104 Uiso 1 calc R . C19 C 0.1084(4) 0.1390(2) 0.6483(3) 0.0603(12) Uani 1 d . . C20 C 0.0110(5) 0.1272(2) 0.5979(3) 0.080(2) Uani 1 d . . H20A H -0.0143(5) 0.0985(2) 0.5953(3) 0.096 Uiso 1 calc R . C21 C -0.0488(6) 0.1582(3) 0.5513(4) 0.115(2) Uani 1 d . . H21A H -0.1122(6) 0.1501(3) 0.5161(4) 0.138 Uiso 1 calc R . C22 C -0.0150(9) 0.2008(3) 0.5568(5) 0.141(3) Uani 1 d . . H22A H -0.0564(9) 0.2215(3) 0.5262(5) 0.169 Uiso 1 calc R . C23 C 0.0781(9) 0.2127(2) 0.6067(5) 0.132(3) Uani 1 d . . H23A H 0.1004(9) 0.2417(2) 0.6102(5) 0.159 Uiso 1 calc R . C24 C 0.1409(6) 0.1822(2) 0.6527(3) 0.087(2) Uani 1 d . . H24A H 0.2053(6) 0.1908(2) 0.6867(3) 0.104 Uiso 1 calc R . C25 C 0.2255(3) 0.04695(15) 0.5799(2) 0.0466(10) Uani 1 d . . C26 C 0.2162(4) 0.0717(2) 0.5125(3) 0.0575(12) Uani 1 d . . C27 C 0.1702(5) 0.0527(2) 0.4427(3) 0.078(2) Uani 1 d . . H27A H 0.1605(5) 0.0692(2) 0.3977(3) 0.094 Uiso 1 calc R . C28 C 0.1396(5) 0.0099(2) 0.4407(4) 0.084(2) Uani 1 d . . H28A H 0.1103(5) -0.0025(2) 0.3939(4) 0.101 Uiso 1 calc R . C29 C 0.1513(5) -0.0152(2) 0.5067(4) 0.080(2) Uani 1 d . . H29A H 0.1313(5) -0.0444(2) 0.5045(4) 0.096 Uiso 1 calc R . C30 C 0.1929(4) 0.0036(2) 0.5763(3) 0.0591(12) Uani 1 d . . H30A H 0.1993(4) -0.0131(2) 0.6214(3) 0.071 Uiso 1 calc R . O26 O 0.2526(3) 0.11347(12) 0.5203(2) 0.0771(10) Uani 1 d . . C261 C 0.2431(7) 0.1407(2) 0.4518(4) 0.116(2) Uani 1 d . . H26A H 0.2718(7) 0.1693(2) 0.4653(4) 0.173 Uiso 1 calc R . H26B H 0.1606(7) 0.1423(2) 0.4316(4) 0.173 Uiso 1 calc R . H26C H 0.2907(7) 0.1287(2) 0.4131(4) 0.173 Uiso 1 calc R . P3 P 0.45004(11) 0.18116(3) 0.82701(6) 0.0466(3) Uani 1 d . . N3 N 0.4560(3) 0.16300(11) 0.9205(2) 0.0498(9) Uani 1 d . . P4 P 0.40738(11) 0.11010(4) 0.91744(6) 0.0479(3) Uani 1 d . . C31 C 0.3488(5) 0.2275(2) 0.8231(3) 0.0698(15) Uani 1 d . . C32 C 0.2390(6) 0.2232(2) 0.8544(4) 0.104(2) Uani 1 d . . H32A H 0.2218(6) 0.1986(2) 0.8827(4) 0.125 Uiso 1 calc R . C33 C 0.1545(8) 0.2562(4) 0.8428(6) 0.169(5) Uani 1 d . . H33A H 0.0814(8) 0.2535(4) 0.8650(6) 0.202 Uiso 1 calc R . C34 C 0.1751(14) 0.2918(5) 0.8006(9) 0.213(9) Uani 1 d . . H34A H 0.1169(14) 0.3133(5) 0.7928(9) 0.256 Uiso 1 calc R . C35 C 0.2798(12) 0.2953(3) 0.7708(6) 0.181(6) Uani 1 d . . H35A H 0.2944(12) 0.3198(3) 0.7417(6) 0.218 Uiso 1 calc R . C36 C 0.3708(7) 0.2639(2) 0.7806(4) 0.106(2) Uani 1 d . . H36A H 0.4439(7) 0.2676(2) 0.7589(4) 0.128 Uiso 1 calc R . C37 C 0.5970(5) 0.2027(2) 0.8115(3) 0.0608(13) Uani 1 d . . C38 C 0.6703(5) 0.1783(2) 0.7670(3) 0.075(2) Uani 1 d . . H38A H 0.6439(5) 0.1516(2) 0.7477(3) 0.090 Uiso 1 calc R . C39 C 0.7837(6) 0.1938(3) 0.7509(5) 0.121(3) Uani 1 d . . H39A H 0.8318(6) 0.1782(3) 0.7191(5) 0.145 Uiso 1 calc R . C40 C 0.8224(8) 0.2325(4) 0.7831(7) 0.159(5) Uani 1 d . . H40A H 0.8980(8) 0.2429(4) 0.7733(7) 0.191 Uiso 1 calc R . C41 C 0.7525(10) 0.2560(3) 0.8291(6) 0.150(4) Uani 1 d . . H41A H 0.7810(10) 0.2819(3) 0.8506(6) 0.180 Uiso 1 calc R . C42 C 0.6404(6) 0.2415(2) 0.8437(4) 0.094(2) Uani 1 d . . H42A H 0.5932(6) 0.2576(2) 0.8752(4) 0.112 Uiso 1 calc R . C43 C 0.5256(4) 0.07562(14) 0.9628(3) 0.0520(11) Uani 1 d . . C44 C 0.5828(5) 0.0812(2) 1.0359(3) 0.081(2) Uani 1 d . . H44A H 0.5602(5) 0.1040(2) 1.0668(3) 0.097 Uiso 1 calc R . C45 C 0.6730(6) 0.0534(2) 1.0637(4) 0.096(2) Uani 1 d . . H45A H 0.7121(6) 0.0579(2) 1.1126(4) 0.115 Uiso 1 calc R . C46 C 0.7047(5) 0.0193(2) 1.0188(4) 0.086(2) Uani 1 d . . H46A H 0.7661(5) 0.0007(2) 1.0371(4) 0.103 Uiso 1 calc R . C47 C 0.6470(5) 0.0126(2) 0.9481(4) 0.080(2) Uani 1 d . . H47A H 0.6672(5) -0.0112(2) 0.9186(4) 0.096 Uiso 1 calc R . C48 C 0.5588(4) 0.0406(2) 0.9195(3) 0.0608(13) Uani 1 d . . H48A H 0.5209(4) 0.0359(2) 0.8703(3) 0.073 Uiso 1 calc R . C49 C 0.2863(4) 0.10694(14) 0.9824(3) 0.0542(12) Uani 1 d . . C50 C 0.2924(5) 0.1148(2) 1.0598(3) 0.093(2) Uani 1 d . . H50A H 0.3663(5) 0.1222(2) 1.0851(3) 0.111 Uiso 1 calc R . C51 C 0.1928(7) 0.1123(2) 1.1027(4) 0.101(2) Uani 1 d . . H51A H 0.1998(7) 0.1205(2) 1.1547(4) 0.121 Uiso 1 calc R . C52 C 0.0875(6) 0.0986(2) 1.0711(4) 0.100(2) Uani 1 d . . H52A H 0.0210(6) 0.0972(2) 1.1004(4) 0.120 Uiso 1 calc R . C53 C 0.0784(6) 0.0865(3) 0.9949(4) 0.119(3) Uani 1 d . . H53A H 0.0067(6) 0.0752(3) 0.9723(4) 0.143 Uiso 1 calc R . C54 C 0.1784(5) 0.0913(2) 0.9506(3) 0.097(2) Uani 1 d . . H54A H 0.1712(5) 0.0836(2) 0.8983(3) 0.116 Uiso 1 calc R . C55 C 0.5012(5) 0.18806(14) 0.9867(3) 0.0576(12) Uani 1 d . . C56 C 0.6221(5) 0.1871(2) 1.0111(3) 0.0687(14) Uani 1 d . . C57 C 0.6636(7) 0.2118(2) 1.0764(4) 0.102(2) Uani 1 d . . H57A H 0.7442(7) 0.2106(2) 1.0946(4) 0.122 Uiso 1 calc R . C58 C 0.5874(9) 0.2370(2) 1.1122(4) 0.118(3) Uani 1 d . . H58A H 0.6165(9) 0.2534(2) 1.1548(4) 0.142 Uiso 1 calc R . C59 C 0.4683(8) 0.2392(2) 1.0880(4) 0.109(2) Uani 1 d . . H59A H 0.4173(8) 0.2572(2) 1.1134(4) 0.131 Uiso 1 calc R . C60 C 0.4231(5) 0.2143(2) 1.0248(3) 0.076(2) Uani 1 d . . H60A H 0.3417(5) 0.2152(2) 1.0084(3) 0.091 Uiso 1 calc R . O56 O 0.6929(3) 0.16235(13) 0.9692(2) 0.0881(12) Uani 1 d . . C561 C 0.8186(6) 0.1603(3) 0.9913(5) 0.168(4) Uani 1 d . . H56A H 0.8567(6) 0.1414(3) 0.9564(5) 0.252 Uiso 1 calc R . H56B H 0.8310(6) 0.1492(3) 1.0433(5) 0.252 Uiso 1 calc R . H56C H 0.8528(6) 0.1887(3) 0.9891(5) 0.252 Uiso 1 calc R . P5 P 0.88500(14) 0.12143(5) 1.27792(10) 0.0786(5) Uani 1 d . . F1 F 0.9259(4) 0.15329(15) 1.3436(3) 0.149(2) Uani 1 d . . F2 F 1.0202(3) 0.10699(12) 1.2735(3) 0.1275(14) Uani 1 d . . F3 F 0.9074(4) 0.1590(2) 1.2214(3) 0.180(2) Uani 1 d . . F4 F 0.7530(3) 0.1373(2) 1.2805(3) 0.166(2) Uani 1 d . . F5 F 0.8485(4) 0.0911(2) 1.2087(4) 0.225(3) Uani 1 d . . F6 F 0.8639(6) 0.0853(2) 1.3329(5) 0.257(4) Uani 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 Cu1 0.0527(3) 0.0495(3) 0.0354(3) -0.0087(2) -0.0015(2) -0.0009(2) P1 0.0459(7) 0.0484(6) 0.0347(6) -0.0064(5) 0.0017(5) -0.0017(5) N1 0.041(2) 0.051(2) 0.034(2) -0.008(2) -0.004(2) 0.004(2) P2 0.0446(7) 0.0523(7) 0.0401(6) -0.0079(5) -0.0029(5) 0.0050(5) C1 0.048(3) 0.057(3) 0.030(2) -0.008(2) 0.000(2) 0.004(2) C2 0.058(3) 0.073(3) 0.084(4) 0.005(3) 0.014(3) 0.011(3) C3 0.068(4) 0.109(5) 0.086(4) 0.007(4) 0.012(3) 0.036(4) C4 0.100(5) 0.071(4) 0.063(4) 0.008(3) 0.000(3) 0.029(3) C5 0.086(4) 0.068(3) 0.065(4) 0.019(3) -0.008(3) 0.000(3) C6 0.054(3) 0.063(3) 0.066(3) 0.014(3) -0.003(2) -0.001(2) C7 0.052(3) 0.059(3) 0.042(3) -0.004(2) 0.007(2) 0.000(2) C8 0.093(4) 0.064(3) 0.049(3) -0.004(3) 0.017(3) 0.004(3) C9 0.100(5) 0.093(4) 0.059(4) -0.001(3) 0.029(3) 0.016(4) C10 0.109(5) 0.121(6) 0.070(4) 0.021(4) 0.041(4) -0.005(4) C11 0.129(5) 0.085(4) 0.075(4) 0.008(4) 0.024(4) -0.034(4) C12 0.091(4) 0.070(3) 0.060(3) -0.012(3) 0.018(3) -0.018(3) C13 0.047(3) 0.072(3) 0.050(3) -0.011(2) 0.006(2) -0.002(2) C14 0.079(4) 0.081(4) 0.107(5) -0.010(4) 0.048(4) -0.004(3) C15 0.134(6) 0.097(5) 0.137(7) -0.014(5) 0.081(5) -0.028(5) C16 0.113(6) 0.140(7) 0.147(8) -0.023(6) 0.061(5) -0.050(6) C17 0.060(4) 0.181(8) 0.129(7) -0.021(6) 0.033(4) -0.003(5) C18 0.056(4) 0.105(4) 0.102(5) -0.001(4) 0.017(3) 0.015(3) C19 0.065(3) 0.066(3) 0.048(3) -0.010(2) -0.007(2) 0.012(3) C20 0.072(4) 0.096(4) 0.067(4) -0.017(3) -0.026(3) 0.020(3) C21 0.100(5) 0.145(7) 0.091(5) 0.003(5) -0.041(4) 0.044(5) C22 0.159(8) 0.130(7) 0.125(7) 0.023(6) -0.042(6) 0.062(6) C23 0.187(9) 0.092(5) 0.112(6) 0.014(5) -0.029(6) 0.045(5) C24 0.111(5) 0.072(4) 0.074(4) 0.006(3) -0.022(3) 0.013(3) C25 0.036(2) 0.066(3) 0.037(2) -0.011(2) -0.001(2) 0.004(2) C26 0.053(3) 0.075(3) 0.043(3) -0.007(3) 0.000(2) 0.001(2) C27 0.072(4) 0.124(5) 0.038(3) -0.011(3) -0.003(3) 0.013(3) C28 0.062(4) 0.128(6) 0.062(4) -0.042(4) -0.006(3) -0.004(4) C29 0.068(4) 0.098(4) 0.073(4) -0.039(4) -0.003(3) -0.015(3) C30 0.049(3) 0.072(3) 0.055(3) -0.018(3) -0.003(2) -0.003(2) O26 0.100(3) 0.080(2) 0.050(2) 0.015(2) -0.004(2) 0.003(2) C261 0.150(6) 0.124(5) 0.071(4) 0.046(4) -0.001(4) 0.009(5) P3 0.0566(7) 0.0420(6) 0.0397(6) -0.0038(5) -0.0068(5) 0.0031(5) N3 0.063(2) 0.050(2) 0.036(2) -0.009(2) -0.004(2) -0.006(2) P4 0.0581(7) 0.0504(7) 0.0344(6) -0.0038(5) -0.0011(5) -0.0033(5) C31 0.083(4) 0.069(3) 0.053(3) -0.020(3) -0.022(3) 0.027(3) C32 0.078(4) 0.130(5) 0.100(5) -0.054(4) -0.022(4) 0.042(4) C33 0.112(6) 0.227(11) 0.155(9) -0.115(9) -0.070(6) 0.102(8) C34 0.237(15) 0.182(11) 0.197(14) -0.114(10) -0.133(12) 0.161(12) C35 0.284(15) 0.101(6) 0.144(9) -0.011(6) -0.084(9) 0.118(9) C36 0.162(6) 0.065(4) 0.087(5) 0.003(3) -0.025(4) 0.041(4) C37 0.069(3) 0.059(3) 0.052(3) 0.019(2) -0.013(3) -0.008(3) C38 0.055(3) 0.081(4) 0.088(4) 0.030(3) -0.001(3) 0.006(3) C39 0.064(5) 0.163(8) 0.136(7) 0.066(6) 0.015(4) 0.017(5) C40 0.076(6) 0.208(13) 0.187(12) 0.088(10) -0.037(6) -0.061(7) C41 0.144(9) 0.134(8) 0.163(10) 0.042(7) -0.044(7) -0.080(7) C42 0.104(5) 0.078(4) 0.094(5) 0.013(3) -0.019(4) -0.037(4) C43 0.064(3) 0.051(3) 0.040(3) 0.006(2) -0.001(2) -0.004(2) C44 0.111(5) 0.072(4) 0.056(3) -0.007(3) -0.018(3) 0.018(3) C45 0.113(5) 0.099(5) 0.071(4) 0.018(4) -0.028(4) 0.014(4) C46 0.073(4) 0.092(5) 0.091(5) 0.024(4) 0.002(4) 0.016(3) C47 0.082(4) 0.073(4) 0.089(5) 0.006(3) 0.028(4) 0.013(3) C48 0.064(3) 0.067(3) 0.052(3) -0.003(3) 0.009(2) 0.004(3) C49 0.058(3) 0.062(3) 0.042(3) -0.005(2) 0.002(2) 0.003(2) C50 0.082(4) 0.146(6) 0.051(3) -0.010(4) 0.011(3) -0.033(4) C51 0.113(6) 0.140(6) 0.052(4) -0.011(4) 0.027(4) -0.023(4) C52 0.079(5) 0.152(6) 0.073(5) 0.002(4) 0.024(4) 0.019(4) C53 0.065(4) 0.199(8) 0.093(6) -0.017(5) 0.010(4) 0.001(4) C54 0.073(4) 0.163(6) 0.055(4) -0.012(4) 0.009(3) 0.012(4) C55 0.080(4) 0.053(3) 0.038(3) -0.004(2) -0.009(3) -0.012(3) C56 0.083(4) 0.067(3) 0.053(3) -0.003(3) -0.011(3) -0.011(3) C57 0.113(5) 0.112(5) 0.073(4) -0.009(4) -0.037(4) -0.024(4) C58 0.165(8) 0.108(6) 0.076(5) -0.038(4) -0.021(5) -0.025(6) C59 0.166(7) 0.096(5) 0.065(4) -0.035(4) 0.010(5) 0.001(5) C60 0.109(4) 0.066(3) 0.053(3) -0.020(3) 0.006(3) 0.002(3) O56 0.072(3) 0.106(3) 0.082(3) -0.002(2) -0.019(2) 0.014(2) C561 0.080(5) 0.249(11) 0.167(8) -0.025(8) -0.042(5) 0.041(6) P5 0.0822(11) 0.0756(10) 0.0786(11) -0.0122(9) 0.0104(8) -0.0219(8) F1 0.157(4) 0.157(4) 0.130(4) -0.072(3) -0.017(3) 0.008(3) F2 0.091(3) 0.137(3) 0.153(4) -0.036(3) 0.002(2) 0.011(2) F3 0.170(4) 0.221(5) 0.147(4) 0.094(4) 0.007(3) -0.003(4) F4 0.083(3) 0.154(4) 0.264(6) -0.055(4) 0.029(3) -0.009(3) F5 0.128(4) 0.263(6) 0.276(8) -0.185(6) -0.039(4) -0.002(4) F6 0.300(8) 0.149(4) 0.342(10) 0.123(6) 0.139(7) -0.027(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 Cu1 P3 2.2944(12) . ? Cu1 P1 2.3010(12) . ? Cu1 P2 2.3268(12) . ? Cu1 P4 2.3330(12) . ? P1 N1 1.719(3) . ? P1 C7 1.817(4) . ? P1 C1 1.823(4) . ? N1 C25 1.451(5) . ? N1 P2 1.717(3) . ? P2 C19 1.817(5) . ? P2 C13 1.818(5) . ? C1 C2 1.379(6) . ? C1 C6 1.383(6) . ? C2 C3 1.395(7) . ? C3 C4 1.370(8) . ? C4 C5 1.341(7) . ? C5 C6 1.384(6) . ? C7 C12 1.370(6) . ? C7 C8 1.385(6) . ? C8 C9 1.381(7) . ? C9 C10 1.378(8) . ? C10 C11 1.366(8) . ? C11 C12 1.395(7) . ? C13 C14 1.376(7) . ? C13 C18 1.386(6) . ? C14 C15 1.380(7) . ? C15 C16 1.348(9) . ? C16 C17 1.351(9) . ? C17 C18 1.395(9) . ? C19 C24 1.383(7) . ? C19 C20 1.387(6) . ? C20 C21 1.389(8) . ? C21 C22 1.367(10) . ? C22 C23 1.348(10) . ? C23 C24 1.388(8) . ? C25 C30 1.388(6) . ? C25 C26 1.389(6) . ? C26 O26 1.356(5) . ? C26 C27 1.401(7) . ? C27 C28 1.362(8) . ? C28 C29 1.376(8) . ? C29 C30 1.382(6) . ? O26 C261 1.447(6) . ? P3 N3 1.705(3) . ? P3 C37 1.808(5) . ? P3 C31 1.821(5) . ? N3 C55 1.439(5) . ? N3 P4 1.720(3) . ? P4 C43 1.823(4) . ? P4 C49 1.823(5) . ? C31 C36 1.375(8) . ? C31 C32 1.381(8) . ? C32 C33 1.391(10) . ? C33 C34 1.35(2) . ? C34 C35 1.32(2) . ? C35 C36 1.403(10) . ? C37 C38 1.386(7) . ? C37 C42 1.390(7) . ? C38 C39 1.400(8) . ? C39 C40 1.373(13) . ? C40 C41 1.363(13) . ? C41 C42 1.368(10) . ? C43 C48 1.382(6) . ? C43 C44 1.379(6) . ? C44 C45 1.379(7) . ? C45 C46 1.370(8) . ? C46 C47 1.352(8) . ? C47 C48 1.372(7) . ? C49 C50 1.355(7) . ? C49 C54 1.371(7) . ? C50 C51 1.383(8) . ? C51 C52 1.326(8) . ? C52 C53 1.363(9) . ? C53 C54 1.407(8) . ? C55 C56 1.381(7) . ? C55 C60 1.391(6) . ? C56 O56 1.346(6) . ? C56 C57 1.410(8) . ? C57 C58 1.337(9) . ? C58 C59 1.364(9) . ? C59 C60 1.396(8) . ? O56 C561 1.426(7) . ? P5 F6 1.495(5) . ? P5 F1 1.543(4) . ? P5 F3 1.548(5) . ? P5 F5 1.548(5) . ? P5 F4 1.555(4) . ? P5 F2 1.580(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 P3 Cu1 P1 132.12(5) . . ? P3 Cu1 P2 130.06(5) . . ? P1 Cu1 P2 73.19(4) . . ? P3 Cu1 P4 73.06(4) . . ? P1 Cu1 P4 132.18(5) . . ? P2 Cu1 P4 126.16(5) . . ? N1 P1 C7 106.1(2) . . ? N1 P1 C1 107.8(2) . . ? C7 P1 C1 103.3(2) . . ? N1 P1 Cu1 90.21(11) . . ? C7 P1 Cu1 124.60(15) . . ? C1 P1 Cu1 121.73(13) . . ? C25 N1 P2 126.4(3) . . ? C25 N1 P1 124.5(3) . . ? P2 N1 P1 106.8(2) . . ? N1 P2 C19 109.3(2) . . ? N1 P2 C13 107.2(2) . . ? C19 P2 C13 101.0(2) . . ? N1 P2 Cu1 89.41(11) . . ? C19 P2 Cu1 124.9(2) . . ? C13 P2 Cu1 122.7(2) . . ? C2 C1 C6 117.5(4) . . ? C2 C1 P1 119.7(3) . . ? C6 C1 P1 122.2(3) . . ? C1 C2 C3 120.4(5) . . ? C4 C3 C2 120.5(5) . . ? C5 C4 C3 119.4(5) . . ? C4 C5 C6 120.9(5) . . ? C5 C6 C1 121.1(5) . . ? C12 C7 C8 118.4(4) . . ? C12 C7 P1 119.1(4) . . ? C8 C7 P1 122.4(4) . . ? C9 C8 C7 120.5(5) . . ? C10 C9 C8 120.3(5) . . ? C11 C10 C9 119.9(5) . . ? C10 C11 C12 119.5(5) . . ? C7 C12 C11 121.4(5) . . ? C14 C13 C18 116.8(5) . . ? C14 C13 P2 122.7(4) . . ? C18 C13 P2 120.0(4) . . ? C13 C14 C15 122.3(5) . . ? C16 C15 C14 120.0(7) . . ? C15 C16 C17 119.6(7) . . ? C16 C17 C18 121.1(7) . . ? C13 C18 C17 120.2(6) . . ? C24 C19 C20 118.4(5) . . ? C24 C19 P2 118.4(4) . . ? C20 C19 P2 123.2(4) . . ? C19 C20 C21 120.1(6) . . ? C22 C21 C20 120.3(7) . . ? C23 C22 C21 120.2(7) . . ? C22 C23 C24 120.6(7) . . ? C19 C24 C23 120.4(6) . . ? C30 C25 C26 119.4(4) . . ? C30 C25 N1 120.6(4) . . ? C26 C25 N1 120.0(4) . . ? O26 C26 C27 124.8(5) . . ? O26 C26 C25 116.0(4) . . ? C27 C26 C25 119.2(5) . . ? C28 C27 C26 120.2(5) . . ? C27 C28 C29 121.1(5) . . ? C28 C29 C30 119.2(5) . . ? C29 C30 C25 120.8(5) . . ? C26 O26 C261 118.0(4) . . ? N3 P3 C37 106.9(2) . . ? N3 P3 C31 105.8(2) . . ? C37 P3 C31 105.8(3) . . ? N3 P3 Cu1 90.75(12) . . ? C37 P3 Cu1 126.4(2) . . ? C31 P3 Cu1 117.5(2) . . ? C55 N3 P3 124.1(3) . . ? C55 N3 P4 128.7(3) . . ? P3 N3 P4 107.1(2) . . ? N3 P4 C43 109.0(2) . . ? N3 P4 C49 106.2(2) . . ? C43 P4 C49 104.5(2) . . ? N3 P4 Cu1 89.08(12) . . ? C43 P4 Cu1 122.06(15) . . ? C49 P4 Cu1 123.0(2) . . ? C36 C31 C32 119.2(5) . . ? C36 C31 P3 121.8(5) . . ? C32 C31 P3 118.4(5) . . ? C31 C32 C33 118.9(8) . . ? C34 C33 C32 122.3(12) . . ? C35 C34 C33 118.0(10) . . ? C34 C35 C36 123.5(12) . . ? C31 C36 C35 118.2(8) . . ? C38 C37 C42 119.1(5) . . ? C38 C37 P3 117.5(4) . . ? C42 C37 P3 123.3(5) . . ? C37 C38 C39 120.3(6) . . ? C40 C39 C38 118.5(9) . . ? C39 C40 C41 121.5(9) . . ? C40 C41 C42 120.3(10) . . ? C41 C42 C37 120.2(8) . . ? C48 C43 C44 117.9(4) . . ? C48 C43 P4 116.1(3) . . ? C44 C43 P4 126.0(4) . . ? C45 C44 C43 121.0(5) . . ? C46 C45 C44 119.6(6) . . ? C47 C46 C45 120.2(5) . . ? C46 C47 C48 120.4(5) . . ? C47 C48 C43 120.9(5) . . ? C50 C49 C54 115.8(5) . . ? C50 C49 P4 127.8(4) . . ? C54 C49 P4 116.2(4) . . ? C49 C50 C51 122.4(6) . . ? C52 C51 C50 121.3(6) . . ? C51 C52 C53 118.8(6) . . ? C52 C53 C54 119.5(7) . . ? C49 C54 C53 121.8(6) . . ? C56 C55 C60 120.1(5) . . ? C56 C55 N3 120.3(4) . . ? C60 C55 N3 119.6(5) . . ? O56 C56 C55 116.6(4) . . ? O56 C56 C57 124.5(6) . . ? C55 C56 C57 118.9(6) . . ? C58 C57 C56 120.3(7) . . ? C57 C58 C59 121.7(6) . . ? C58 C59 C60 119.8(6) . . ? C55 C60 C59 119.2(6) . . ? C56 O56 C561 119.1(5) . . ? F6 P5 F1 93.5(4) . . ? F6 P5 F3 179.6(4) . . ? F1 P5 F3 86.2(3) . . ? F6 P5 F5 89.6(4) . . ? F1 P5 F5 176.5(4) . . ? F3 P5 F5 90.7(4) . . ? F6 P5 F4 91.3(3) . . ? F1 P5 F4 90.3(3) . . ? F3 P5 F4 88.9(3) . . ? F5 P5 F4 91.1(3) . . ? F6 P5 F2 91.0(3) . . ? F1 P5 F2 89.2(2) . . ? F3 P5 F2 88.9(3) . . ? F5 P5 F2 89.3(2) . . ? F4 P5 F2 177.7(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P3 Cu1 P1 N1 -133.33(12) . . . . ? P2 Cu1 P1 N1 -4.04(11) . . . . ? P4 Cu1 P1 N1 119.87(12) . . . . ? P3 Cu1 P1 C7 -23.4(2) . . . . ? P2 Cu1 P1 C7 105.8(2) . . . . ? P4 Cu1 P1 C7 -130.2(2) . . . . ? P3 Cu1 P1 C1 115.5(2) . . . . ? P2 Cu1 P1 C1 -115.2(2) . . . . ? P4 Cu1 P1 C1 8.7(2) . . . . ? C7 P1 N1 C25 42.8(4) . . . . ? C1 P1 N1 C25 -67.3(4) . . . . ? Cu1 P1 N1 C25 169.1(3) . . . . ? C7 P1 N1 P2 -120.8(2) . . . . ? C1 P1 N1 P2 129.1(2) . . . . ? Cu1 P1 N1 P2 5.5(2) . . . . ? C25 N1 P2 C19 -41.6(4) . . . . ? P1 N1 P2 C19 121.7(2) . . . . ? C25 N1 P2 C13 67.0(4) . . . . ? P1 N1 P2 C13 -129.7(2) . . . . ? C25 N1 P2 Cu1 -168.7(3) . . . . ? P1 N1 P2 Cu1 -5.4(2) . . . . ? P3 Cu1 P2 N1 135.44(12) . . . . ? P1 Cu1 P2 N1 4.04(12) . . . . ? P4 Cu1 P2 N1 -126.34(12) . . . . ? P3 Cu1 P2 C19 22.1(2) . . . . ? P1 Cu1 P2 C19 -109.3(2) . . . . ? P4 Cu1 P2 C19 120.3(2) . . . . ? P3 Cu1 P2 C13 -114.3(2) . . . . ? P1 Cu1 P2 C13 114.3(2) . . . . ? P4 Cu1 P2 C13 -16.1(2) . . . . ? N1 P1 C1 C2 156.7(4) . . . . ? C7 P1 C1 C2 44.7(4) . . . . ? Cu1 P1 C1 C2 -101.6(4) . . . . ? N1 P1 C1 C6 -31.9(4) . . . . ? C7 P1 C1 C6 -143.9(4) . . . . ? Cu1 P1 C1 C6 69.8(4) . . . . ? C6 C1 C2 C3 2.1(7) . . . . ? P1 C1 C2 C3 173.9(4) . . . . ? C1 C2 C3 C4 0.2(9) . . . . ? C2 C3 C4 C5 -1.2(9) . . . . ? C3 C4 C5 C6 -0.1(9) . . . . ? C4 C5 C6 C1 2.5(8) . . . . ? C2 C1 C6 C5 -3.4(7) . . . . ? P1 C1 C6 C5 -175.0(4) . . . . ? N1 P1 C7 C12 98.7(4) . . . . ? C1 P1 C7 C12 -148.1(4) . . . . ? Cu1 P1 C7 C12 -3.1(5) . . . . ? N1 P1 C7 C8 -77.5(4) . . . . ? C1 P1 C7 C8 35.8(4) . . . . ? Cu1 P1 C7 C8 -179.2(3) . . . . ? C12 C7 C8 C9 -0.6(7) . . . . ? P1 C7 C8 C9 175.6(4) . . . . ? C7 C8 C9 C10 1.6(9) . . . . ? C8 C9 C10 C11 -1.3(10) . . . . ? C9 C10 C11 C12 -0.1(10) . . . . ? C8 C7 C12 C11 -0.9(8) . . . . ? P1 C7 C12 C11 -177.1(4) . . . . ? C10 C11 C12 C7 1.2(9) . . . . ? N1 P2 C13 C14 30.5(5) . . . . ? C19 P2 C13 C14 144.9(5) . . . . ? Cu1 P2 C13 C14 -70.2(5) . . . . ? N1 P2 C13 C18 -157.9(4) . . . . ? C19 P2 C13 C18 -43.5(5) . . . . ? Cu1 P2 C13 C18 101.4(4) . . . . ? C18 C13 C14 C15 1.5(9) . . . . ? P2 C13 C14 C15 173.4(5) . . . . ? C13 C14 C15 C16 -2.6(12) . . . . ? C14 C15 C16 C17 1.8(14) . . . . ? C15 C16 C17 C18 -0.1(14) . . . . ? C14 C13 C18 C17 0.2(9) . . . . ? P2 C13 C18 C17 -171.9(5) . . . . ? C16 C17 C18 C13 -0.9(12) . . . . ? N1 P2 C19 C24 -113.1(4) . . . . ? C13 P2 C19 C24 134.1(4) . . . . ? Cu1 P2 C19 C24 -9.7(5) . . . . ? N1 P2 C19 C20 67.8(5) . . . . ? C13 P2 C19 C20 -45.1(5) . . . . ? Cu1 P2 C19 C20 171.1(4) . . . . ? C24 C19 C20 C21 2.2(8) . . . . ? P2 C19 C20 C21 -178.6(5) . . . . ? C19 C20 C21 C22 -2.4(11) . . . . ? C20 C21 C22 C23 1.2(13) . . . . ? C21 C22 C23 C24 0.2(14) . . . . ? C20 C19 C24 C23 -0.9(9) . . . . ? P2 C19 C24 C23 179.9(5) . . . . ? C22 C23 C24 C19 -0.3(12) . . . . ? P2 N1 C25 C30 -104.7(4) . . . . ? P1 N1 C25 C30 94.9(4) . . . . ? P2 N1 C25 C26 76.5(5) . . . . ? P1 N1 C25 C26 -84.0(4) . . . . ? C30 C25 C26 O26 -178.3(4) . . . . ? N1 C25 C26 O26 0.5(6) . . . . ? C30 C25 C26 C27 2.1(7) . . . . ? N1 C25 C26 C27 -179.0(4) . . . . ? O26 C26 C27 C28 177.9(5) . . . . ? C25 C26 C27 C28 -2.6(7) . . . . ? C26 C27 C28 C29 1.0(8) . . . . ? C27 C28 C29 C30 1.1(8) . . . . ? C28 C29 C30 C25 -1.5(7) . . . . ? C26 C25 C30 C29 -0.1(7) . . . . ? N1 C25 C30 C29 -179.0(4) . . . . ? C27 C26 O26 C261 0.3(7) . . . . ? C25 C26 O26 C261 -179.2(5) . . . . ? P1 Cu1 P3 N3 -133.53(13) . . . . ? P2 Cu1 P3 N3 121.94(13) . . . . ? P4 Cu1 P3 N3 -1.41(12) . . . . ? P1 Cu1 P3 C37 -21.8(2) . . . . ? P2 Cu1 P3 C37 -126.3(2) . . . . ? P4 Cu1 P3 C37 110.4(2) . . . . ? P1 Cu1 P3 C31 118.2(2) . . . . ? P2 Cu1 P3 C31 13.6(2) . . . . ? P4 Cu1 P3 C31 -109.7(2) . . . . ? C37 P3 N3 C55 49.9(4) . . . . ? C31 P3 N3 C55 -62.5(4) . . . . ? Cu1 P3 N3 C55 178.5(4) . . . . ? C37 P3 N3 P4 -126.7(2) . . . . ? C31 P3 N3 P4 120.9(2) . . . . ? Cu1 P3 N3 P4 1.9(2) . . . . ? C55 N3 P4 C43 -54.5(4) . . . . ? P3 N3 P4 C43 121.9(2) . . . . ? C55 N3 P4 C49 57.5(4) . . . . ? P3 N3 P4 C49 -126.1(2) . . . . ? C55 N3 P4 Cu1 -178.3(4) . . . . ? P3 N3 P4 Cu1 -1.9(2) . . . . ? P3 Cu1 P4 N3 1.39(12) . . . . ? P1 Cu1 P4 N3 133.47(13) . . . . ? P2 Cu1 P4 N3 -126.25(13) . . . . ? P3 Cu1 P4 C43 -110.6(2) . . . . ? P1 Cu1 P4 C43 21.5(2) . . . . ? P2 Cu1 P4 C43 121.8(2) . . . . ? P3 Cu1 P4 C49 110.2(2) . . . . ? P1 Cu1 P4 C49 -117.8(2) . . . . ? P2 Cu1 P4 C49 -17.5(2) . . . . ? N3 P3 C31 C36 140.9(4) . . . . ? C37 P3 C31 C36 27.7(5) . . . . ? Cu1 P3 C31 C36 -119.7(4) . . . . ? N3 P3 C31 C32 -48.6(5) . . . . ? C37 P3 C31 C32 -161.9(4) . . . . ? Cu1 P3 C31 C32 50.7(5) . . . . ? C36 C31 C32 C33 -0.9(9) . . . . ? P3 C31 C32 C33 -171.6(5) . . . . ? C31 C32 C33 C34 1.5(13) . . . . ? C32 C33 C34 C35 -1.1(19) . . . . ? C33 C34 C35 C36 0.0(21) . . . . ? C32 C31 C36 C35 0.0(9) . . . . ? P3 C31 C36 C35 170.3(6) . . . . ? C34 C35 C36 C31 0.5(15) . . . . ? N3 P3 C37 C38 105.8(4) . . . . ? C31 P3 C37 C38 -141.8(4) . . . . ? Cu1 P3 C37 C38 1.8(5) . . . . ? N3 P3 C37 C42 -72.4(4) . . . . ? C31 P3 C37 C42 40.1(5) . . . . ? Cu1 P3 C37 C42 -176.3(3) . . . . ? C42 C37 C38 C39 -3.7(8) . . . . ? P3 C37 C38 C39 178.1(4) . . . . ? C37 C38 C39 C40 2.9(10) . . . . ? C38 C39 C40 C41 -0.7(14) . . . . ? C39 C40 C41 C42 -0.7(17) . . . . ? C40 C41 C42 C37 -0.1(13) . . . . ? C38 C37 C42 C41 2.3(9) . . . . ? P3 C37 C42 C41 -179.6(6) . . . . ? N3 P4 C43 C48 -127.7(3) . . . . ? C49 P4 C43 C48 119.1(4) . . . . ? Cu1 P4 C43 C48 -26.5(4) . . . . ? N3 P4 C43 C44 53.0(5) . . . . ? C49 P4 C43 C44 -60.2(5) . . . . ? Cu1 P4 C43 C44 154.2(4) . . . . ? C48 C43 C44 C45 2.1(8) . . . . ? P4 C43 C44 C45 -178.7(4) . . . . ? C43 C44 C45 C46 -1.4(9) . . . . ? C44 C45 C46 C47 -0.7(10) . . . . ? C45 C46 C47 C48 2.0(9) . . . . ? C46 C47 C48 C43 -1.3(8) . . . . ? C44 C43 C48 C47 -0.8(7) . . . . ? P4 C43 C48 C47 179.9(4) . . . . ? N3 P4 C49 C50 -61.3(5) . . . . ? C43 P4 C49 C50 53.8(5) . . . . ? Cu1 P4 C49 C50 -161.0(4) . . . . ? N3 P4 C49 C54 124.5(4) . . . . ? C43 P4 C49 C54 -120.4(4) . . . . ? Cu1 P4 C49 C54 24.8(5) . . . . ? C54 C49 C50 C51 -7.4(9) . . . . ? P4 C49 C50 C51 178.4(5) . . . . ? C49 C50 C51 C52 5.5(11) . . . . ? C50 C51 C52 C53 0.4(12) . . . . ? C51 C52 C53 C54 -3.7(12) . . . . ? C50 C49 C54 C53 4.0(9) . . . . ? P4 C49 C54 C53 178.9(5) . . . . ? C52 C53 C54 C49 1.4(11) . . . . ? P3 N3 C55 C56 -88.3(5) . . . . ? P4 N3 C55 C56 87.5(5) . . . . ? P3 N3 C55 C60 89.9(5) . . . . ? P4 N3 C55 C60 -94.3(5) . . . . ? C60 C55 C56 O56 -177.2(4) . . . . ? N3 C55 C56 O56 1.0(7) . . . . ? C60 C55 C56 C57 2.2(7) . . . . ? N3 C55 C56 C57 -179.6(5) . . . . ? O56 C56 C57 C58 176.9(6) . . . . ? C55 C56 C57 C58 -2.5(9) . . . . ? C56 C57 C58 C59 1.0(12) . . . . ? C57 C58 C59 C60 0.8(12) . . . . ? C56 C55 C60 C59 -0.5(8) . . . . ? N3 C55 C60 C59 -178.7(5) . . . . ? C58 C59 C60 C55 -1.0(10) . . . . ? C55 C56 O56 C561 179.6(6) . . . . ? C57 C56 O56 C561 0.3(9) . . . . ? _refine_diff_density_max 0.373 _refine_diff_density_min -0.296 _refine_diff_density_rms 0.060 #---end data_13 #----------------------------------------------------------------------- _publ_section_references ; Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Altomare, A., Cascarano, M., Giacovazzo, C., Guagliardi, A. (1993). J. Appl. Cryst., 26, 343. ; #----------------------------------------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1993) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #----------------------------------------------------------------------- _cell_length_a 12.587(6) _cell_length_b 14.127(5) _cell_length_c 11.423(6) _cell_angle_alpha 92.14(4) _cell_angle_beta 112.82(4) _cell_angle_gamma 111.20(3) _cell_volume 1708(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 10.4 _cell_measurement_theta_max 12.0 #----------------------------------------------------------------------- _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #----------------------------------------------------------------------- _exptl_crystal_description 'plate' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_diffrn 1.438 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1478.68 _chemical_formula_analytical 'C65 H58 Cl10 N2 O2 P4 Ru ' _chemical_formula_sum 'C65 H58 Cl10 N2 O2 P4 Ru ' _chemical_formula_moiety 'C62 H54 Cl2 N2 O2 P4 Ru.(C H Cl3)2.(CH2 Cl2)' _chemical_formula_structural 'C65 H58 Cl10 N2 O2 P4 Ru ' _chemical_compound_source - _exptl_crystal_F_000 752.00 _exptl_absorpt_coefficient_mu 0.757 _exptl_absorpt_correction_type ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 0.998 _exptl_absorpt_correction_T_min 0.914 _exptl_special_details ; The scan width was (0.84+0.35tan\q)\% with an \w scan speed of 0\% per minute (up to 5 scans to achieve I/\s(I) > 12). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #----------------------------------------------------------------------- _diffrn_special_details ; - ; _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -3.66 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 -3 3 2 -5 1 2 -5 -1 _diffrn_reflns_number 6314 _reflns_number_total 6016 _reflns_number_gt 4071 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.02034 _diffrn_reflns_av_sigmaI/netI 0.070 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.03852 _diffrn_orient_matrix_UB_12 -0.04959 _diffrn_orient_matrix_UB_13 -0.00632 _diffrn_orient_matrix_UB_21 0.08615 _diffrn_orient_matrix_UB_22 0.05750 _diffrn_orient_matrix_UB_23 0.04544 _diffrn_orient_matrix_UB_31 0.00325 _diffrn_orient_matrix_UB_32 -0.01600 _diffrn_orient_matrix_UB_33 0.08555 #----------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 65 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 58 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 2 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 2 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 4 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 10 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ru 0 1 -1.420 0.836 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #----------------------------------------------------------------------- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Ru(1) 0.0000 0.0000 0.0000 0.0279(3) 0.500 S Uani d ? Cl(1) 0.0586(2) -0.1402(2) -0.0337(2) 0.0410(6) 1.000 . Uani d ? Cl(2) 0.6114(5) 0.2561(5) -0.0839(6) 0.171(2) 1.000 . Uani d ? Cl(3) 0.8447(5) 0.3295(5) 0.1392(5) 0.156(2) 1.000 . Uani d ? Cl(4) 0.8427(6) 0.3790(5) -0.0981(7) 0.181(2) 1.000 . Uani d ? Cl(5) 0.9797 0.4726 0.4238 0.296 0.500 . Uani d ? Cl(6) 0.9008 0.4601 0.6169 0.136 0.500 . Uani d ? P(1) 0.1771(2) 0.1135(2) -0.0231(2) 0.0325(6) 1.000 . Uani d ? P(2) 0.1765(2) 0.0629(2) 0.2004(2) 0.0335(6) 1.000 . Uani d ? O(26) 0.2611(7) 0.3114(5) 0.2113(8) 0.057(2) 1.000 . Uani d ? N(1) 0.2780(7) 0.1396(6) 0.1381(7) 0.033(2) 1.000 . Uani d ? C(1) 0.2417(9) 0.0573(8) -0.1128(9) 0.039(3) 1.000 . Uani d ? C(2) 0.314(1) 0.0050(9) -0.062(1) 0.046(3) 1.000 . Uani d ? C(3) 0.350(1) -0.0436(9) -0.136(1) 0.058(3) 1.000 . Uani d ? C(4) 0.311(1) -0.035(1) -0.268(1) 0.077(4) 1.000 . Uani d ? C(5) 0.236(1) 0.0134(9) -0.323(1) 0.057(3) 1.000 . Uani d ? C(6) 0.203(1) 0.0612(9) -0.245(1) 0.054(3) 1.000 . Uani d ? C(7) 0.2100(9) 0.2400(8) -0.0698(9) 0.039(3) 1.000 . Uani d ? C(8) 0.327(1) 0.2954(9) -0.069(1) 0.047(3) 1.000 . Uani d ? C(9) 0.356(1) 0.391(1) -0.099(1) 0.064(4) 1.000 . Uani d ? C(10) 0.271(1) 0.4363(9) -0.128(1) 0.077(4) 1.000 . Uani d ? C(11) 0.151(1) 0.381(1) -0.132(1) 0.073(4) 1.000 . Uani d ? C(12) 0.120(1) 0.2819(8) -0.102(1) 0.051(3) 1.000 . Uani d ? C(13) 0.196(1) 0.1431(8) 0.3444(9) 0.039(3) 1.000 . Uani d ? C(14) 0.312(1) 0.1915(9) 0.449(1) 0.054(3) 1.000 . Uani d ? C(15) 0.325(1) 0.248(1) 0.558(1) 0.075(4) 1.000 . Uani d ? C(16) 0.221(2) 0.255(1) 0.565(1) 0.088(5) 1.000 . Uani d ? C(17) 0.107(1) 0.207(1) 0.460(1) 0.091(5) 1.000 . Uani d ? C(18) 0.094(1) 0.1490(9) 0.351(1) 0.057(3) 1.000 . Uani d ? C(19) 0.2443(9) -0.0246(7) 0.2812(9) 0.036(2) 1.000 . Uani d ? C(20) 0.174(1) -0.0947(9) 0.333(1) 0.053(3) 1.000 . Uani d ? C(21) 0.214(1) -0.1648(9) 0.393(1) 0.066(4) 1.000 . Uani d ? C(22) 0.327(1) -0.167(1) 0.404(1) 0.072(4) 1.000 . Uani d ? C(23) 0.400(1) -0.097(1) 0.355(1) 0.068(4) 1.000 . Uani d ? C(24) 0.357(1) -0.0262(8) 0.294(1) 0.051(3) 1.000 . Uani d ? C(25) 0.3895(9) 0.2299(8) 0.2063(9) 0.040(3) 1.000 . Uani d ? C(26) 0.381(1) 0.3210(8) 0.246(1) 0.044(3) 1.000 . Uani d ? C(27) 0.492(1) 0.4121(9) 0.317(1) 0.064(4) 1.000 . Uani d ? C(28) 0.605(1) 0.412(1) 0.344(1) 0.079(4) 1.000 . Uani d ? C(29) 0.617(1) 0.325(1) 0.307(1) 0.073(4) 1.000 . Uani d ? C(30) 0.507(1) 0.2327(9) 0.235(1) 0.054(3) 1.000 . Uani d ? C(31) 0.236(1) 0.401(1) 0.247(2) 0.125(6) 1.000 . Uani d ? C(40) 0.767(2) 0.285(1) -0.031(2) 0.116(6) 1.000 . Uani d ? C(50) 1.0130 0.4512 0.5488 0.096 0.500 . Uani d ? H(2) 0.3423 0.0030 0.0277 0.054 1.000 . Uiso c ? H(3) 0.3990 -0.0822 -0.0997 0.069 1.000 . Uiso c ? H(4) 0.3395 -0.0659 -0.3191 0.091 1.000 . Uiso c ? H(5) 0.2078 0.0146 -0.4123 0.067 1.000 . Uiso c ? H(6) 0.1526 0.0982 -0.2820 0.064 1.000 . Uiso c ? H(8) 0.3872 0.2663 -0.0473 0.055 1.000 . Uiso c ? H(9) 0.4351 0.4270 -0.1009 0.077 1.000 . Uiso c ? H(10) 0.2936 0.5042 -0.1449 0.091 1.000 . Uiso c ? H(11) 0.0913 0.4111 -0.1539 0.086 1.000 . Uiso c ? H(12) 0.0397 0.2441 -0.1049 0.061 1.000 . Uiso c ? H(14) 0.3833 0.1857 0.4463 0.063 1.000 . Uiso c ? H(15) 0.4062 0.2827 0.6288 0.089 1.000 . Uiso c ? H(16) 0.2289 0.2917 0.6412 0.105 1.000 . Uiso c ? H(17) 0.0362 0.2137 0.4620 0.110 1.000 . Uiso c ? H(18) 0.0122 0.1134 0.2808 0.068 1.000 . Uiso c ? H(20) 0.0974 -0.0933 0.3262 0.063 1.000 . Uiso c ? H(21) 0.1649 -0.2123 0.4281 0.077 1.000 . Uiso c ? H(22) 0.3541 -0.2167 0.4443 0.085 1.000 . Uiso c ? H(23) 0.4776 -0.0974 0.3627 0.081 1.000 . Uiso c ? H(24) 0.4068 0.0221 0.2601 0.058 1.000 . Uiso c ? H(27) 0.4861 0.4731 0.3458 0.076 1.000 . Uiso c ? H(28) 0.6787 0.4747 0.3898 0.092 1.000 . Uiso c ? H(29) 0.6984 0.3258 0.3302 0.089 1.000 . Uiso c ? H(30) 0.5153 0.1726 0.2070 0.063 1.000 . Uiso c ? H(31B) 0.2707 0.4568 0.2095 0.146 1.000 . Uiso c ? H(31A) 0.2744 0.4228 0.3381 0.146 1.000 . Uiso c ? H(31C) 0.1477 0.3812 0.2138 0.146 1.000 . Uiso c ? H(40) 0.7764 0.2239 -0.0502 0.136 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru(1) 0.0326(5) 0.0273(5) 0.0278(5) 0.0144(4) 0.0149(4) 0.0072(4) Cl(1) 0.048(1) 0.037(1) 0.048(1) 0.024(1) 0.025(1) 0.010(1) Cl(2) 0.100(3) 0.254(6) 0.165(5) 0.097(3) 0.045(3) 0.007(5) Cl(3) 0.181(4) 0.186(5) 0.116(4) 0.116(3) 0.044(3) -0.001(3) Cl(4) 0.263(5) 0.126(4) 0.236(5) 0.094(4) 0.172(4) 0.080(4) Cl(5) 0.2359 0.3061 0.2605 0.0476 0.0867 0.0012 Cl(6) 0.1146 0.1494 0.1068 0.0618 0.0062 -0.0068 P(1) 0.036(1) 0.033(1) 0.032(1) 0.015(1) 0.0169(9) 0.010(1) P(2) 0.037(1) 0.035(1) 0.030(1) 0.016(1) 0.015(1) 0.009(1) O(26) 0.070(4) 0.043(4) 0.064(5) 0.031(3) 0.029(4) 0.012(4) N(1) 0.027(4) 0.039(4) 0.023(4) 0.007(3) 0.007(3) 0.005(3) C(1) 0.033(5) 0.042(6) 0.039(5) 0.007(4) 0.020(4) 0.005(5) C(2) 0.045(5) 0.054(6) 0.046(6) 0.024(5) 0.022(4) 0.010(5) C(3) 0.065(6) 0.063(7) 0.055(7) 0.038(5) 0.025(5) 0.006(6) C(4) 0.068(7) 0.08(1) 0.085(8) 0.017(6) 0.054(5) -0.010(7) C(5) 0.080(7) 0.053(7) 0.057(6) 0.029(5) 0.048(5) 0.015(5) C(6) 0.077(7) 0.052(6) 0.053(6) 0.034(5) 0.041(5) 0.024(5) C(7) 0.051(6) 0.034(5) 0.031(5) 0.016(4) 0.018(4) 0.009(4) C(8) 0.047(6) 0.046(6) 0.037(6) 0.011(5) 0.016(4) 0.008(5) C(9) 0.059(7) 0.057(8) 0.049(7) -0.001(6) 0.019(6) 0.003(6) C(10) 0.12(1) 0.038(7) 0.060(7) 0.014(7) 0.045(7) 0.014(6) C(11) 0.115(9) 0.066(7) 0.076(8) 0.055(6) 0.058(6) 0.042(6) C(12) 0.070(7) 0.042(6) 0.052(6) 0.025(5) 0.035(5) 0.018(5) C(13) 0.057(6) 0.037(5) 0.030(5) 0.021(4) 0.023(4) 0.008(4) C(14) 0.069(7) 0.043(6) 0.036(6) 0.017(5) 0.017(5) 0.003(5) C(15) 0.11(1) 0.052(7) 0.035(7) 0.030(7) 0.013(7) 0.008(6) C(16) 0.13(1) 0.082(9) 0.049(7) 0.053(8) 0.033(7) -0.003(7) C(17) 0.120(9) 0.12(1) 0.073(8) 0.066(8) 0.059(6) 0.012(8) C(18) 0.072(7) 0.067(7) 0.040(6) 0.033(6) 0.027(5) 0.004(5) C(19) 0.047(5) 0.033(5) 0.025(5) 0.019(4) 0.012(4) 0.006(4) C(20) 0.063(6) 0.056(7) 0.052(6) 0.031(5) 0.029(5) 0.021(5) C(21) 0.082(8) 0.048(6) 0.069(7) 0.028(6) 0.031(6) 0.040(5) C(22) 0.10(1) 0.052(7) 0.057(7) 0.033(6) 0.025(7) 0.027(6) C(23) 0.074(7) 0.077(8) 0.061(8) 0.046(6) 0.024(6) 0.019(6) C(24) 0.051(6) 0.049(6) 0.064(7) 0.028(5) 0.026(5) 0.030(5) C(25) 0.037(5) 0.043(6) 0.035(5) 0.008(4) 0.018(4) 0.015(4) C(26) 0.047(6) 0.032(5) 0.046(6) 0.012(5) 0.015(5) 0.008(5) C(27) 0.077(8) 0.045(7) 0.059(7) 0.013(6) 0.030(6) 0.010(6) C(28) 0.053(8) 0.060(9) 0.078(9) -0.014(7) 0.020(7) 0.002(8) C(29) 0.034(6) 0.09(1) 0.070(8) 0.005(7) 0.017(6) 0.011(8) C(30) 0.049(6) 0.061(7) 0.055(6) 0.021(5) 0.028(5) 0.021(5) C(31) 0.10(1) 0.08(1) 0.18(2) 0.053(7) 0.04(1) -0.03(1) C(40) 0.11(1) 0.09(1) 0.15(2) 0.066(7) 0.04(1) 0.00(1) C(50) 0.0836 0.0925 0.0694 -0.0109 0.0334 0.0395 #----------------------------------------------------------------------- _refine_special_details ; - ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00000|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef - _refine_ls_abs_structure_details - _refine_ls_abs_structure_Flack - _refine_ls_number_reflns 4071 _refine_ls_number_parameters 368 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0874 _refine_ls_R_factor_gt 0.0874 _refine_ls_wR_factor_all 0.1186 _refine_ls_wR_factor_ref 0.1186 _refine_ls_goodness_of_fit_all 6.086 _refine_ls_goodness_of_fit_ref 6.086 _refine_ls_shift/esd_max 4.4590 _refine_ls_shift/esd_mean 0.0790 _refine_diff_density_min -1.22 _refine_diff_density_max 5.26 #----------------------------------------------------------------------- _geom_special_details ; - ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru(1) Cl(1) 2.416(3) . . yes Ru(1) Cl(1) 2.416(3) . 2 yes Ru(1) P(1) 2.348(3) . . yes Ru(1) P(1) 2.348(3) . 2 yes Ru(1) P(2) 2.332(2) . . yes Ru(1) P(2) 2.332(2) . 2 yes Cl(2) C(40) 1.69(2) . . yes Cl(3) C(40) 1.76(2) . . yes Cl(4) C(40) 1.73(2) . . yes Cl(5) Cl(5) 1.6775(1) . 2_766 yes Cl(5) Cl(6) 1.7090(6) . 2_766 yes Cl(5) C(50) 1.402 . . yes Cl(5) C(50) 1.0704(1) . 2_766 yes Cl(6) C(50) 1.8937(6) . . yes P(1) N(1) 1.714(7) . . yes P(1) C(1) 1.84(1) . . yes P(1) C(7) 1.83(1) . . yes P(2) N(1) 1.754(8) . . yes P(2) C(13) 1.84(1) . . yes P(2) C(19) 1.83(1) . . yes O(26) C(26) 1.35(1) . . yes O(26) C(31) 1.49(2) . . yes N(1) C(25) 1.41(1) . . yes C(1) C(2) 1.35(1) . . yes C(1) C(6) 1.41(1) . . yes C(2) C(3) 1.36(2) . . yes C(2) H(2) 0.95 . . no C(3) C(4) 1.42(2) . . yes C(3) H(3) 0.95 . . no C(4) C(5) 1.34(2) . . yes C(4) H(4) 0.95 . . no C(5) C(6) 1.36(2) . . yes C(5) H(5) 0.95 . . no C(6) H(6) 0.95 . . no C(7) C(8) 1.39(1) . . yes C(7) C(12) 1.39(2) . . yes C(8) C(9) 1.36(2) . . yes C(8) H(8) 0.95 . . no C(9) C(10) 1.37(2) . . yes C(9) H(9) 0.95 . . no C(10) C(11) 1.41(2) . . yes C(10) H(10) 0.95 . . no C(11) C(12) 1.40(2) . . yes C(11) H(11) 0.95 . . no C(12) H(12) 0.95 . . no C(13) C(14) 1.38(1) . . yes C(13) C(18) 1.35(2) . . yes C(14) C(15) 1.37(2) . . yes C(14) H(14) 0.95 . . no C(15) C(16) 1.38(2) . . yes C(15) H(15) 0.95 . . no C(16) C(17) 1.36(2) . . yes C(16) H(16) 0.95 . . no C(17) C(18) 1.38(2) . . yes C(17) H(17) 0.94 . . no C(18) H(18) 0.95 . . no C(19) C(20) 1.39(1) . . yes C(19) C(24) 1.38(1) . . yes C(20) C(21) 1.36(2) . . yes C(20) H(20) 0.95 . . no C(21) C(22) 1.39(2) . . yes C(21) H(21) 0.95 . . no C(22) C(23) 1.38(2) . . yes C(22) H(22) 0.95 . . no C(23) C(24) 1.39(2) . . yes C(23) H(23) 0.95 . . no C(24) H(24) 0.95 . . no C(25) C(26) 1.40(2) . . yes C(25) C(30) 1.37(1) . . yes C(26) C(27) 1.42(1) . . yes C(27) C(28) 1.33(2) . . yes C(27) H(27) 0.95 . . no C(28) C(29) 1.37(2) . . yes C(28) H(28) 0.95 . . no C(29) C(30) 1.42(2) . . yes C(29) H(29) 0.95 . . no C(30) H(30) 0.95 . . no C(31) H(31B) 0.95 . . no C(31) H(31A) 0.94 . . no C(31) H(31C) 0.95 . . no C(40) H(40) 0.95 . . no C(50) C(50) 1.8465(1) . 2_766 yes #----------------------------------------------------------------------- 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(1) Ru(1) Cl(1) 180.00 . . 2 yes Cl(1) Ru(1) P(1) 88.49(9) . . . yes Cl(1) Ru(1) P(1) 91.51(9) . . 2 yes Cl(1) Ru(1) P(2) 87.89(9) . . . yes Cl(1) Ru(1) P(2) 92.11(9) . . 2 yes Cl(1) Ru(1) P(1) 91.51(9) 2 . . yes Cl(1) Ru(1) P(1) 88.49(9) 2 . 2 yes Cl(1) Ru(1) P(2) 92.11(9) 2 . . yes Cl(1) Ru(1) P(2) 87.89(9) 2 . 2 yes P(1) Ru(1) P(1) 180.00 . . 2 yes P(1) Ru(1) P(2) 69.84(9) . . . yes P(1) Ru(1) P(2) 110.16(9) . . 2 yes P(1) Ru(1) P(2) 110.16(9) 2 . . yes P(1) Ru(1) P(2) 69.84(9) 2 . 2 yes P(2) Ru(1) P(2) 180.00 . . 2 yes Cl(5) Cl(5) Cl(6) 107.746(6) 2_766 . 2_766 yes Cl(5) Cl(5) C(50) 39.418(2) 2_766 . . yes Cl(5) Cl(5) C(50) 56.276(3) 2_766 . 2_766 yes Cl(6) Cl(5) C(50) 117.70(2) 2_766 . . yes Cl(6) Cl(5) C(50) 82.45(1) 2_766 . 2_766 yes C(50) Cl(5) C(50) 95.693(4) . . 2_766 yes Cl(5) Cl(6) C(50) 34.08(1) 2_766 . . yes Ru(1) P(1) N(1) 94.8(3) . . . yes Ru(1) P(1) C(1) 117.6(3) . . . yes Ru(1) P(1) C(7) 130.7(4) . . . yes N(1) P(1) C(1) 106.5(4) . . . yes N(1) P(1) C(7) 105.2(4) . . . yes C(1) P(1) C(7) 99.5(5) . . . yes Ru(1) P(2) N(1) 94.2(2) . . . yes Ru(1) P(2) C(13) 126.2(4) . . . yes Ru(1) P(2) C(19) 120.3(3) . . . yes N(1) P(2) C(13) 108.7(4) . . . yes N(1) P(2) C(19) 107.4(4) . . . yes C(13) P(2) C(19) 98.7(5) . . . yes C(26) O(26) C(31) 120.5(9) . . . yes P(1) N(1) P(2) 101.2(4) . . . yes P(1) N(1) C(25) 126.3(7) . . . yes P(2) N(1) C(25) 126.9(7) . . . yes P(1) C(1) C(2) 123.9(8) . . . yes P(1) C(1) C(6) 117.6(9) . . . yes C(2) C(1) C(6) 118(1) . . . yes C(1) C(2) C(3) 122(1) . . . yes C(1) C(2) H(2) 118.9 . . . no C(3) C(2) H(2) 119.2 . . . no C(2) C(3) C(4) 118(1) . . . yes C(2) C(3) H(3) 121.2 . . . no C(4) C(3) H(3) 121.2 . . . no C(3) C(4) C(5) 122(1) . . . yes C(3) C(4) H(4) 118.5 . . . no C(5) C(4) H(4) 119.3 . . . no C(4) C(5) C(6) 118(1) . . . yes C(4) C(5) H(5) 120.8 . . . no C(6) C(5) H(5) 121.2 . . . no C(1) C(6) C(5) 122(1) . . . yes C(1) C(6) H(6) 119.2 . . . no C(5) C(6) H(6) 118.9 . . . no P(1) C(7) C(8) 119.6(9) . . . yes P(1) C(7) C(12) 120.5(8) . . . yes C(8) C(7) C(12) 120(1) . . . yes C(7) C(8) C(9) 121(1) . . . yes C(7) C(8) H(8) 119.5 . . . no C(9) C(8) H(8) 119.3 . . . no C(8) C(9) C(10) 121(1) . . . yes C(8) C(9) H(9) 119.9 . . . no C(10) C(9) H(9) 119.5 . . . no C(9) C(10) C(11) 120(1) . . . yes C(9) C(10) H(10) 120.0 . . . no C(11) C(10) H(10) 120.4 . . . no C(10) C(11) C(12) 120(1) . . . yes C(10) C(11) H(11) 120.0 . . . no C(12) C(11) H(11) 120.2 . . . no C(7) C(12) C(11) 119(1) . . . yes C(7) C(12) H(12) 120.7 . . . no C(11) C(12) H(12) 120.4 . . . no P(2) C(13) C(14) 120.9(9) . . . yes P(2) C(13) C(18) 119.6(8) . . . yes C(14) C(13) C(18) 119(1) . . . yes C(13) C(14) C(15) 121(1) . . . yes C(13) C(14) H(14) 119.6 . . . no C(15) C(14) H(14) 119.6 . . . no C(14) C(15) C(16) 120(1) . . . yes C(14) C(15) H(15) 119.8 . . . no C(16) C(15) H(15) 120.1 . . . no C(15) C(16) C(17) 118(1) . . . yes C(15) C(16) H(16) 120.4 . . . no C(17) C(16) H(16) 121.6 . . . no C(16) C(17) C(18) 122(1) . . . yes C(16) C(17) H(17) 118.6 . . . no C(18) C(17) H(17) 119.5 . . . no C(13) C(18) C(17) 120(1) . . . yes C(13) C(18) H(18) 120.4 . . . no C(17) C(18) H(18) 119.9 . . . no P(2) C(19) C(20) 115.9(8) . . . yes P(2) C(19) C(24) 125.6(8) . . . yes C(20) C(19) C(24) 119(1) . . . yes C(19) C(20) C(21) 121(1) . . . yes C(19) C(20) H(20) 119.3 . . . no C(21) C(20) H(20) 119.4 . . . no C(20) C(21) C(22) 120(1) . . . yes C(20) C(21) H(21) 120.3 . . . no C(22) C(21) H(21) 120.1 . . . no C(21) C(22) C(23) 120(1) . . . yes C(21) C(22) H(22) 120.1 . . . no C(23) C(22) H(22) 119.5 . . . no C(22) C(23) C(24) 119(1) . . . yes C(22) C(23) H(23) 121.0 . . . no C(24) C(23) H(23) 120.3 . . . no C(19) C(24) C(23) 121(1) . . . yes C(19) C(24) H(24) 119.4 . . . no C(23) C(24) H(24) 119.3 . . . no N(1) C(25) C(26) 119(1) . . . yes N(1) C(25) C(30) 123(1) . . . yes C(26) C(25) C(30) 118.3(9) . . . yes O(26) C(26) C(25) 114.2(8) . . . yes O(26) C(26) C(27) 126(1) . . . yes C(25) C(26) C(27) 120(1) . . . yes C(26) C(27) C(28) 120(1) . . . yes C(26) C(27) H(27) 119.7 . . . no C(28) C(27) H(27) 120.0 . . . no C(27) C(28) C(29) 121(1) . . . yes C(27) C(28) H(28) 118.8 . . . no C(29) C(28) H(28) 119.9 . . . no C(28) C(29) C(30) 120(1) . . . yes C(28) C(29) H(29) 119.8 . . . no C(30) C(29) H(29) 120.6 . . . no C(25) C(30) C(29) 121(1) . . . yes C(25) C(30) H(30) 119.8 . . . no C(29) C(30) H(30) 119.6 . . . no O(26) C(31) H(31B) 108.9 . . . no O(26) C(31) H(31A) 109.5 . . . no O(26) C(31) H(31C) 109.2 . . . no H(31B) C(31) H(31A) 109.8 . . . no H(31B) C(31) H(31C) 109.2 . . . no H(31A) C(31) H(31C) 110.2 . . . no Cl(2) C(40) Cl(3) 110(1) . . . yes Cl(2) C(40) Cl(4) 114(1) . . . yes Cl(2) C(40) H(40) 108.2 . . . no Cl(3) C(40) Cl(4) 107.6(9) . . . yes Cl(3) C(40) H(40) 107.9 . . . no Cl(4) C(40) H(40) 108.6 . . . no Cl(5) C(50) Cl(5) 84.307(4) . . 2_766 yes Cl(5) C(50) Cl(6) 111.31(2) . . . yes Cl(5) C(50) C(50) 35.229(2) . . 2_766 yes Cl(5) C(50) Cl(6) 63.465(3) 2_766 . . yes Cl(5) C(50) C(50) 49.077(3) 2_766 . 2_766 yes Cl(6) C(50) C(50) 90.976(9) . . 2_766 yes #----------------------------------------------------------------------- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(1) C(40) 3.42(2) . 2_655 no Cl(3) Cl(5) 3.207(5) . . no Cl(3) Cl(6) 3.526(5) . 2_766 no C(3) C(3) 3.55(2) . 2_655 no C(5) C(15) 3.60(2) . 1_554 no C(6) C(16) 3.56(2) . 1_554 no C(9) C(9) 3.58(2) . 2_665 no C(23) C(23) 3.56(2) . 2_656 no #---end