Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email A.D.BURROWS@BATH.AC.UK _publ_contact_author_name 'Dr Andrew David Burrows' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_year ? _journal_page_first ? _publ_contact_author_address ; Department of Chemistry University of Bath Claverton Down Bath BA2 7AY UNITED KINGDOM ; _publ_section_title ; The synthesis and late transition metal chemistry of 7-aza-N-indolyl phosphines and the activity of their palladium complexes in CO-ethene co-polymerisation ; loop_ _publ_author_name 'Andrew David Burrows' 'M. Mahon' 'Maurizio Varrone' data_compound1a_99ab5 _database_code_CSD 217632 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C19 H15 Cl2 N2 P Pd' _chemical_formula_weight 479.60 _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' Cl Cl 0.1484 0.1585 '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' 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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.849(2) _cell_length_b 15.522(2) _cell_length_c 12.376(2) _cell_angle_alpha 90.00 _cell_angle_beta 111.190(10) _cell_angle_gamma 90.00 _cell_volume 1764.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.806 _exptl_crystal_density_method ? _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 1.450 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 170(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3359 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0178 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 24.98 _reflns_number_total 3104 _reflns_number_observed 2930 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 4 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^)+(0.0391P)^2^+1.3626P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0160(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3100 _refine_ls_number_parameters 227 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0262 _refine_ls_R_factor_obs 0.0236 _refine_ls_wR_factor_all 0.0654 _refine_ls_wR_factor_obs 0.0626 _refine_ls_goodness_of_fit_all 1.109 _refine_ls_goodness_of_fit_obs 1.127 _refine_ls_restrained_S_all 1.141 _refine_ls_restrained_S_obs 1.127 _refine_ls_shift/esd_max 0.000 _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 Pd1 Pd 0.18290(2) 0.095102(11) 0.078958(14) 0.01269(10) Uani 1 d . . P1 P 0.19602(6) 0.18767(4) -0.05307(5) 0.01283(14) Uani 1 d . . Cl1 Cl 0.15857(7) -0.00220(4) 0.21572(5) 0.02235(15) Uani 1 d . . Cl2 Cl 0.42004(6) 0.05800(4) 0.11498(5) 0.01985(15) Uani 1 d . . N1 N 0.0345(2) 0.24131(13) -0.0806(2) 0.0162(4) Uani 1 d . . N2 N -0.0273(2) 0.13649(12) 0.0345(2) 0.0151(4) Uani 1 d . . C1 C 0.3382(2) 0.26744(14) -0.0191(2) 0.0155(5) Uani 1 d . . C2 C 0.3465(3) 0.3218(2) -0.1066(2) 0.0185(5) Uani 1 d . . H2 H 0.2788(3) 0.3156(2) -0.1836(2) 0.022 Uiso 1 calc R . C3 C 0.4529(3) 0.3847(2) -0.0813(2) 0.0211(5) Uani 1 d . . H3 H 0.4571(3) 0.4225(2) -0.1403(2) 0.025 Uiso 1 calc R . C4 C 0.5538(3) 0.3922(2) 0.0311(2) 0.0220(5) Uani 1 d . . H4 H 0.6286(3) 0.4344(2) 0.0480(2) 0.026 Uiso 1 calc R . C5 C 0.5463(3) 0.3389(2) 0.1184(2) 0.0220(5) Uani 1 d . . H5 H 0.6149(3) 0.3451(2) 0.1950(2) 0.026 Uiso 1 calc R . C6 C 0.4384(3) 0.2764(2) 0.0940(2) 0.0188(5) Uani 1 d . . H6 H 0.4326(3) 0.2400(2) 0.1539(2) 0.023 Uiso 1 calc R . C7 C 0.1820(2) 0.14167(14) -0.1905(2) 0.0147(5) Uani 1 d . . C8 C 0.3016(3) 0.09743(14) -0.1982(2) 0.0186(5) Uani 1 d . . H8 H 0.3894(3) 0.09381(14) -0.1327(2) 0.022 Uiso 1 calc R . C9 C 0.2920(3) 0.0588(2) -0.3018(2) 0.0219(5) Uani 1 d . . H9 H 0.3735(3) 0.0291(2) -0.3075(2) 0.026 Uiso 1 calc R . C10 C 0.1632(3) 0.0635(2) -0.3970(2) 0.0233(5) Uani 1 d . . H10 H 0.1570(3) 0.0376(2) -0.4681(2) 0.028 Uiso 1 calc R . C11 C 0.0443(3) 0.1056(2) -0.3889(2) 0.0216(5) Uani 1 d . . H11 H -0.0438(3) 0.1079(2) -0.4543(2) 0.026 Uiso 1 calc R . C12 C 0.0518(3) 0.1445(2) -0.2861(2) 0.0188(5) Uani 1 d . . H12 H -0.0310(3) 0.1729(2) -0.2807(2) 0.023 Uiso 1 calc R . C13 C -0.0418(3) 0.3068(2) -0.1572(2) 0.0203(5) Uani 1 d . . H13 H -0.0012(3) 0.3442(2) -0.1983(2) 0.024 Uiso 1 calc R . C14 C -0.1823(3) 0.3083(2) -0.1634(2) 0.0236(5) Uani 1 d . . H14 H -0.2559(3) 0.3465(2) -0.2092(2) 0.028 Uiso 1 calc R . C15 C -0.2001(3) 0.2419(2) -0.0886(2) 0.0204(5) Uani 1 d . . C16 C -0.3105(3) 0.2072(2) -0.0558(2) 0.0242(6) Uani 1 d . . H16 H -0.4063(3) 0.2301(2) -0.0852(2) 0.029 Uiso 1 calc R . C17 C -0.2763(3) 0.1389(2) 0.0201(2) 0.0241(6) Uani 1 d . . H17 H -0.3499(3) 0.1147(2) 0.0436(2) 0.029 Uiso 1 calc R . C18 C -0.1366(3) 0.1043(2) 0.0635(2) 0.0201(5) Uani 1 d . . H18 H -0.1178(3) 0.0566(2) 0.1149(2) 0.024 Uiso 1 calc R . C19 C -0.0630(2) 0.20265(15) -0.0396(2) 0.0161(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 Pd1 0.01363(13) 0.01222(13) 0.01111(13) 0.00090(6) 0.00316(8) -0.00048(6) P1 0.0127(3) 0.0132(3) 0.0118(3) 0.0013(2) 0.0034(2) 0.0009(2) Cl1 0.0258(3) 0.0211(3) 0.0184(3) 0.0060(2) 0.0059(2) -0.0051(2) Cl2 0.0171(3) 0.0192(3) 0.0224(3) 0.0041(2) 0.0061(2) 0.0045(2) N1 0.0155(10) 0.0177(10) 0.0146(9) 0.0013(8) 0.0045(8) 0.0038(8) N2 0.0153(9) 0.0169(10) 0.0127(9) -0.0040(8) 0.0048(8) -0.0025(8) C1 0.0153(11) 0.0133(11) 0.0172(11) -0.0006(9) 0.0049(9) 0.0015(9) C2 0.0185(12) 0.0166(12) 0.0174(12) 0.0006(9) 0.0030(10) 0.0011(9) C3 0.0243(13) 0.0169(11) 0.0208(13) 0.0045(10) 0.0068(10) -0.0004(10) C4 0.0201(12) 0.0158(12) 0.0274(14) -0.0029(10) 0.0054(11) -0.0033(10) C5 0.0225(13) 0.0198(12) 0.0186(12) -0.0042(10) 0.0015(10) -0.0016(10) C6 0.0223(12) 0.0164(11) 0.0161(11) 0.0008(9) 0.0051(10) 0.0003(9) C7 0.0178(11) 0.0129(11) 0.0131(11) 0.0003(9) 0.0052(9) -0.0033(9) C8 0.0191(12) 0.0182(12) 0.0166(12) 0.0010(9) 0.0040(10) 0.0018(9) C9 0.0284(13) 0.0165(12) 0.0223(13) 0.0005(10) 0.0112(11) 0.0038(10) C10 0.0375(15) 0.0167(12) 0.0166(12) -0.0024(10) 0.0108(11) -0.0035(11) C11 0.0267(13) 0.0172(12) 0.0141(12) 0.0008(9) -0.0008(10) -0.0050(10) C12 0.0174(12) 0.0179(12) 0.0193(12) 0.0011(10) 0.0044(10) -0.0024(9) C13 0.0246(12) 0.0198(12) 0.0142(11) 0.0037(9) 0.0040(10) 0.0060(10) C14 0.0208(12) 0.0245(13) 0.0195(12) -0.0039(10) 0.0001(10) 0.0091(10) C15 0.0157(12) 0.0237(13) 0.0174(12) -0.0076(10) 0.0008(9) 0.0031(9) C16 0.0143(12) 0.0294(14) 0.0262(13) -0.0119(11) 0.0041(10) 0.0007(10) C17 0.0179(12) 0.0307(14) 0.0255(13) -0.0117(11) 0.0099(10) -0.0083(10) C18 0.0220(13) 0.0206(12) 0.0184(12) -0.0085(9) 0.0082(10) -0.0067(10) C19 0.0145(11) 0.0182(11) 0.0141(11) -0.0060(9) 0.0034(9) -0.0012(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N2 2.044(2) . ? Pd1 P1 2.2144(6) . ? Pd1 Cl2 2.2875(7) . ? Pd1 Cl1 2.3444(6) . ? P1 N1 1.717(2) . ? P1 C1 1.802(2) . ? P1 C7 1.803(2) . ? N1 C19 1.376(3) . ? N1 C13 1.407(3) . ? N2 C19 1.337(3) . ? N2 C18 1.348(3) . ? C1 C2 1.398(3) . ? C1 C6 1.398(3) . ? C2 C3 1.382(3) . ? C3 C4 1.391(4) . ? C4 C5 1.384(4) . ? C5 C6 1.389(4) . ? C7 C8 1.396(3) . ? C7 C12 1.397(3) . ? C8 C9 1.388(3) . ? C9 C10 1.386(4) . ? C10 C11 1.376(4) . ? C11 C12 1.386(4) . ? C13 C14 1.358(4) . ? C14 C15 1.437(4) . ? C15 C16 1.398(4) . ? C15 C19 1.404(3) . ? C16 C17 1.375(4) . ? C17 C18 1.391(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 N2 Pd1 P1 85.47(6) . . ? N2 Pd1 Cl2 174.29(6) . . ? P1 Pd1 Cl2 88.82(2) . . ? N2 Pd1 Cl1 92.22(6) . . ? P1 Pd1 Cl1 177.64(2) . . ? Cl2 Pd1 Cl1 93.48(2) . . ? N1 P1 C1 107.44(10) . . ? N1 P1 C7 104.79(10) . . ? C1 P1 C7 106.26(10) . . ? N1 P1 Pd1 99.44(7) . . ? C1 P1 Pd1 121.45(8) . . ? C7 P1 Pd1 115.72(8) . . ? C19 N1 C13 106.8(2) . . ? C19 N1 P1 115.8(2) . . ? C13 N1 P1 135.6(2) . . ? C19 N2 C18 115.5(2) . . ? C19 N2 Pd1 114.6(2) . . ? C18 N2 Pd1 129.8(2) . . ? C2 C1 C6 119.9(2) . . ? C2 C1 P1 119.5(2) . . ? C6 C1 P1 120.6(2) . . ? C3 C2 C1 120.1(2) . . ? C2 C3 C4 119.7(2) . . ? C5 C4 C3 120.6(2) . . ? C4 C5 C6 120.1(2) . . ? C5 C6 C1 119.6(2) . . ? C8 C7 C12 119.7(2) . . ? C8 C7 P1 118.7(2) . . ? C12 C7 P1 121.4(2) . . ? C9 C8 C7 119.9(2) . . ? C10 C9 C8 119.9(2) . . ? C11 C10 C9 120.3(2) . . ? C10 C11 C12 120.6(2) . . ? C11 C12 C7 119.5(2) . . ? C14 C13 N1 109.6(2) . . ? C13 C14 C15 108.1(2) . . ? C16 C15 C19 115.7(2) . . ? C16 C15 C14 138.8(2) . . ? C19 C15 C14 105.5(2) . . ? C17 C16 C15 118.2(2) . . ? C16 C17 C18 121.6(2) . . ? N2 C18 C17 121.8(2) . . ? N2 C19 N1 122.9(2) . . ? N2 C19 C15 127.1(2) . . ? N1 C19 C15 110.0(2) . . ? _refine_diff_density_max 0.491 _refine_diff_density_min -0.627 _refine_diff_density_rms 0.126 #===END data_compound1b_k00adb9 _database_code_CSD 217633 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H13 Cl2 N4 P Pd' _chemical_formula_weight 457.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.74000(10) _cell_length_b 10.87000(10) _cell_length_c 17.4600(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.0630(4) _cell_angle_gamma 90.00 _cell_volume 1638.06(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 18 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.855 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 1.559 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33639 _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_av_sigmaI/netI 0.0216 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.59 _diffrn_reflns_theta_max 30.03 _reflns_number_total 4771 _reflns_number_gt 4577 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'Denzo and Scalepack (otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0191P)^2^+1.5635P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0096(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4771 _refine_ls_number_parameters 209 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0233 _refine_ls_R_factor_gt 0.0222 _refine_ls_wR_factor_ref 0.0537 _refine_ls_wR_factor_gt 0.0531 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.115 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.323150(12) 0.291049(10) 0.227905(6) 0.01179(5) Uani 1 1 d . . . Cl1 Cl 0.18913(4) 0.33999(4) 0.10458(2) 0.01793(8) Uani 1 1 d . . . Cl2 Cl 0.44505(5) 0.12433(4) 0.18463(2) 0.02109(9) Uani 1 1 d . . . P P 0.43116(4) 0.24004(4) 0.34517(2) 0.01241(8) Uani 1 1 d . . . N1 N 0.22728(15) 0.43453(12) 0.28047(7) 0.0141(2) Uani 1 1 d . . . N2 N 0.35220(16) 0.34503(13) 0.39845(8) 0.0158(2) Uani 1 1 d . . . C1 C 0.1345(2) 0.52672(16) 0.24937(10) 0.0202(3) Uani 1 1 d . . . H1 H 0.1109 0.5339 0.1946 0.024 Uiso 1 1 calc R . . C2 C 0.0723(2) 0.61175(17) 0.29581(11) 0.0255(4) Uani 1 1 d . . . H2 H 0.0068 0.6751 0.2718 0.031 Uiso 1 1 calc R . . C3 C 0.1035(2) 0.60619(16) 0.37621(11) 0.0232(3) Uani 1 1 d . . . H3 H 0.0587 0.6633 0.4074 0.028 Uiso 1 1 calc R . . C4 C 0.20315(19) 0.51369(15) 0.40958(9) 0.0169(3) Uani 1 1 d . . . C5 C 0.2660(2) 0.46995(17) 0.48634(10) 0.0213(3) Uani 1 1 d . . . H5 H 0.2487 0.5053 0.5340 0.026 Uiso 1 1 calc R . . C6 C 0.3542(2) 0.36941(16) 0.47826(9) 0.0197(3) Uani 1 1 d . . . H6 H 0.4088 0.3226 0.5198 0.024 Uiso 1 1 calc R . . C7 C 0.25966(17) 0.43343(14) 0.35792(9) 0.0136(3) Uani 1 1 d . . . N3 N 0.62381(15) 0.24239(13) 0.36789(8) 0.0160(2) Uani 1 1 d . . . C8 C 0.7161(2) 0.19427(17) 0.43397(10) 0.0211(3) Uani 1 1 d . . . H8 H 0.6815 0.1437 0.4722 0.025 Uiso 1 1 calc R . . C9 C 0.8638(2) 0.23285(18) 0.43364(10) 0.0238(3) Uani 1 1 d . . . H9 H 0.9512 0.2132 0.4713 0.029 Uiso 1 1 calc R . . C10 C 0.8646(2) 0.30781(18) 0.36690(11) 0.0236(3) Uani 1 1 d . . . H10 H 0.9528 0.3473 0.3524 0.028 Uiso 1 1 calc R . . C11 C 0.71812(19) 0.31334(16) 0.32752(10) 0.0192(3) Uani 1 1 d . . . H11 H 0.6854 0.3575 0.2809 0.023 Uiso 1 1 calc R . . N4 N 0.38413(15) 0.10682(13) 0.38353(8) 0.0156(2) Uani 1 1 d . . . C12 C 0.4531(2) -0.00667(16) 0.37216(10) 0.0206(3) Uani 1 1 d . . . H12 H 0.5555 -0.0183 0.3616 0.025 Uiso 1 1 calc R . . C13 C 0.3490(2) -0.09712(17) 0.37876(10) 0.0239(3) Uani 1 1 d . . . H13 H 0.3664 -0.1830 0.3748 0.029 Uiso 1 1 calc R . . C14 C 0.2085(2) -0.04033(18) 0.39264(11) 0.0263(4) Uani 1 1 d . . . H14 H 0.1156 -0.0817 0.3992 0.032 Uiso 1 1 calc R . . C15 C 0.23132(19) 0.08309(17) 0.39478(11) 0.0222(3) Uani 1 1 d . . . H15 H 0.1566 0.1433 0.4026 0.027 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.01106(7) 0.01330(7) 0.01083(7) 0.00000(4) 0.00116(4) 0.00020(4) Cl1 0.01645(17) 0.02244(19) 0.01373(16) 0.00079(13) -0.00128(12) -0.00022(13) Cl2 0.02569(19) 0.01983(18) 0.01809(18) -0.00279(14) 0.00445(14) 0.00636(14) P 0.01114(16) 0.01413(18) 0.01194(17) 0.00072(13) 0.00172(13) 0.00171(13) N1 0.0132(6) 0.0145(6) 0.0144(6) 0.0000(5) 0.0017(4) 0.0008(5) N2 0.0184(6) 0.0163(6) 0.0124(6) 0.0003(5) 0.0020(5) 0.0038(5) C1 0.0218(8) 0.0185(8) 0.0197(7) 0.0023(6) 0.0008(6) 0.0053(6) C2 0.0276(9) 0.0208(8) 0.0270(9) 0.0011(7) 0.0004(7) 0.0105(7) C3 0.0263(8) 0.0186(8) 0.0251(8) -0.0033(6) 0.0054(7) 0.0070(6) C4 0.0183(7) 0.0150(7) 0.0179(7) -0.0026(6) 0.0044(6) 0.0003(6) C5 0.0244(8) 0.0234(8) 0.0165(7) -0.0037(6) 0.0047(6) 0.0015(6) C6 0.0242(8) 0.0227(8) 0.0120(7) -0.0012(6) 0.0023(6) 0.0026(6) C7 0.0122(6) 0.0126(7) 0.0159(7) 0.0002(5) 0.0021(5) 0.0000(5) N3 0.0121(6) 0.0204(6) 0.0153(6) 0.0027(5) 0.0014(5) 0.0006(5) C8 0.0175(7) 0.0304(9) 0.0146(7) 0.0030(6) 0.0001(6) 0.0044(6) C9 0.0153(7) 0.0336(9) 0.0208(8) -0.0075(7) -0.0021(6) 0.0045(7) C10 0.0153(7) 0.0273(9) 0.0285(9) -0.0060(7) 0.0048(6) -0.0037(6) C11 0.0170(7) 0.0212(7) 0.0202(7) 0.0011(6) 0.0051(6) -0.0026(6) N4 0.0130(6) 0.0160(6) 0.0186(6) 0.0031(5) 0.0049(5) 0.0021(5) C12 0.0242(8) 0.0173(7) 0.0217(8) 0.0022(6) 0.0083(6) 0.0057(6) C13 0.0339(9) 0.0172(8) 0.0210(8) 0.0021(6) 0.0052(7) -0.0006(7) C14 0.0203(8) 0.0288(9) 0.0288(9) 0.0091(7) 0.0012(7) -0.0052(7) C15 0.0141(7) 0.0251(8) 0.0287(9) 0.0086(7) 0.0076(6) 0.0030(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 Pd N1 2.0541(13) . ? Pd P 2.1867(4) . ? Pd Cl2 2.2899(4) . ? Pd Cl1 2.3446(4) . ? P N3 1.6681(14) . ? P N4 1.6737(14) . ? P N2 1.6871(14) . ? N1 C7 1.3373(19) . ? N1 C1 1.348(2) . ? N2 C7 1.3777(19) . ? N2 C6 1.416(2) . ? C1 C2 1.395(2) . ? C2 C3 1.389(3) . ? C3 C4 1.396(2) . ? C4 C7 1.400(2) . ? C4 C5 1.447(2) . ? C5 C6 1.357(2) . ? N3 C11 1.398(2) . ? N3 C8 1.401(2) . ? C8 C9 1.359(2) . ? C9 C10 1.423(3) . ? C10 C11 1.356(2) . ? N4 C12 1.401(2) . ? N4 C15 1.404(2) . ? C12 C13 1.357(3) . ? C13 C14 1.429(3) . ? C14 C15 1.356(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 Pd P 85.44(4) . . ? N1 Pd Cl2 172.78(4) . . ? P Pd Cl2 87.341(15) . . ? N1 Pd Cl1 93.33(4) . . ? P Pd Cl1 175.551(14) . . ? Cl2 Pd Cl1 93.878(14) . . ? N3 P N4 102.73(7) . . ? N3 P N2 110.11(7) . . ? N4 P N2 102.53(7) . . ? N3 P Pd 119.30(5) . . ? N4 P Pd 119.80(5) . . ? N2 P Pd 101.01(5) . . ? C7 N1 C1 115.59(14) . . ? C7 N1 Pd 114.13(10) . . ? C1 N1 Pd 130.25(11) . . ? C7 N2 C6 106.87(13) . . ? C7 N2 P 116.53(11) . . ? C6 N2 P 136.61(12) . . ? N1 C1 C2 121.54(15) . . ? C3 C2 C1 121.74(16) . . ? C2 C3 C4 117.62(15) . . ? C3 C4 C7 116.13(15) . . ? C3 C4 C5 138.10(16) . . ? C7 C4 C5 105.73(14) . . ? C6 C5 C4 107.90(14) . . ? C5 C6 N2 109.50(14) . . ? N1 C7 N2 122.63(14) . . ? N1 C7 C4 127.31(14) . . ? N2 C7 C4 110.00(13) . . ? C11 N3 C8 108.21(13) . . ? C11 N3 P 122.81(11) . . ? C8 N3 P 128.22(12) . . ? C9 C8 N3 107.79(15) . . ? C8 C9 C10 107.91(15) . . ? C11 C10 C9 108.33(16) . . ? C10 C11 N3 107.74(15) . . ? C12 N4 C15 107.35(14) . . ? C12 N4 P 124.53(11) . . ? C15 N4 P 120.92(11) . . ? C13 C12 N4 108.46(15) . . ? C12 C13 C14 107.90(16) . . ? C15 C14 C13 107.76(16) . . ? C14 C15 N4 108.49(15) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.601 _refine_diff_density_min -0.947 _refine_diff_density_rms 0.108 #===END data_compound3a_k01adb6 _database_code_CSD 217634 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H15 Cl N2 O P Rh' _chemical_formula_weight 468.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' Rh Rh -1.1178 0.9187 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0020(2) _cell_length_b 13.8360(4) _cell_length_c 15.0090(4) _cell_angle_alpha 85.7660(11) _cell_angle_beta 82.9660(11) _cell_angle_gamma 87.5270(14) _cell_volume 1849.16(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 18 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.683 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 1.166 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_max 1.038 _exptl_absorpt_correction_T_min 0.971 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21848 _diffrn_reflns_av_R_equivalents 0.0682 _diffrn_reflns_av_sigmaI/netI 0.0731 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.67 _diffrn_reflns_theta_max 27.57 _reflns_number_total 8370 _reflns_number_gt 6875 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'Denzo and Scalepack (otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0458P)^2^+0.3188P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0100(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8370 _refine_ls_number_parameters 465 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0526 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.1033 _refine_ls_wR_factor_gt 0.0959 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.64964(2) 1.288740(17) 0.185276(16) 0.01949(9) Uani 1 1 d . . . Rh2 Rh 0.07538(2) 0.836548(17) 0.321037(16) 0.01890(9) Uani 1 1 d . . . P1 P 0.80037(8) 1.26265(6) 0.06213(5) 0.01887(17) Uani 1 1 d . . . P2 P 0.19534(8) 0.76583(6) 0.42969(5) 0.01774(17) Uani 1 1 d . . . Cl1 Cl 0.47739(9) 1.30807(6) 0.31636(6) 0.02779(18) Uani 1 1 d . . . Cl2 Cl -0.07149(9) 0.92142(7) 0.21879(6) 0.0319(2) Uani 1 1 d . . . N1 N 0.5926(3) 1.14183(19) 0.17998(18) 0.0219(6) Uani 1 1 d . . . N2 N 0.7710(3) 1.14335(19) 0.04910(18) 0.0216(5) Uani 1 1 d . . . N3 N 0.1177(3) 0.96643(18) 0.37730(18) 0.0204(5) Uani 1 1 d . . . N4 N 0.2294(3) 0.86415(18) 0.48726(18) 0.0205(5) Uani 1 1 d . . . O1 O 0.7356(3) 1.49440(18) 0.16980(19) 0.0376(6) Uani 1 1 d . . . O2 O 0.0201(3) 0.65065(18) 0.24571(17) 0.0310(5) Uani 1 1 d . . . C1 C 0.7024(4) 1.4150(3) 0.1768(2) 0.0265(7) Uani 1 1 d . . . C2 C 0.4903(4) 1.0873(3) 0.2324(2) 0.0287(7) Uani 1 1 d . . . H2 H 0.4354 1.1138 0.2819 0.034 Uiso 1 1 calc R . . C3 C 0.4646(4) 0.9920(3) 0.2142(3) 0.0330(8) Uani 1 1 d . . . H3 H 0.3914 0.9575 0.2509 0.040 Uiso 1 1 calc R . . C4 C 0.5444(4) 0.9486(3) 0.1438(3) 0.0330(8) Uani 1 1 d . . . H4 H 0.5292 0.8844 0.1339 0.040 Uiso 1 1 calc R . . C5 C 0.6490(4) 1.0024(2) 0.0871(2) 0.0267(7) Uani 1 1 d . . . C6 C 0.6648(3) 1.0984(2) 0.1107(2) 0.0207(6) Uani 1 1 d . . . C7 C 0.7535(4) 0.9908(2) 0.0078(2) 0.0295(7) Uani 1 1 d . . . H7 H 0.7694 0.9351 -0.0237 0.035 Uiso 1 1 calc R . . C8 C 0.8250(4) 1.0755(2) -0.0131(2) 0.0266(7) Uani 1 1 d . . . H8 H 0.8987 1.0868 -0.0614 0.032 Uiso 1 1 calc R . . C9 C 1.0015(3) 1.2689(2) 0.0572(2) 0.0217(6) Uani 1 1 d . . . C10 C 1.0651(4) 1.2529(2) 0.1376(2) 0.0258(7) Uani 1 1 d . . . H10 H 1.0039 1.2420 0.1917 0.031 Uiso 1 1 calc R . . C11 C 1.2200(4) 1.2531(3) 0.1370(3) 0.0325(8) Uani 1 1 d . . . H11 H 1.2624 1.2415 0.1904 0.039 Uiso 1 1 calc R . . C12 C 1.3108(4) 1.2707(3) 0.0560(3) 0.0303(8) Uani 1 1 d . . . H12 H 1.4142 1.2710 0.0554 0.036 Uiso 1 1 calc R . . C13 C 1.2485(4) 1.2876(3) -0.0234(3) 0.0340(8) Uani 1 1 d . . . H13 H 1.3097 1.3000 -0.0773 0.041 Uiso 1 1 calc R . . C14 C 1.0939(4) 1.2861(3) -0.0228(2) 0.0292(7) Uani 1 1 d . . . H14 H 1.0522 1.2968 -0.0766 0.035 Uiso 1 1 calc R . . C15 C 0.7505(3) 1.3279(2) -0.0395(2) 0.0212(6) Uani 1 1 d . . . C16 C 0.7800(5) 1.4267(3) -0.0534(2) 0.0343(8) Uani 1 1 d . . . H16 H 0.8368 1.4552 -0.0154 0.041 Uiso 1 1 calc R . . C17 C 0.7249(5) 1.4823(3) -0.1236(3) 0.0421(10) Uani 1 1 d . . . H17 H 0.7462 1.5477 -0.1332 0.050 Uiso 1 1 calc R . . C18 C 0.6379(4) 1.4403(3) -0.1797(3) 0.0372(9) Uani 1 1 d . . . H18 H 0.5975 1.4781 -0.2253 0.045 Uiso 1 1 calc R . . C19 C 0.6119(4) 1.3434(3) -0.1678(2) 0.0329(8) Uani 1 1 d . . . H19 H 0.5567 1.3149 -0.2066 0.040 Uiso 1 1 calc R . . C20 C 0.6679(3) 1.2872(3) -0.0976(2) 0.0268(7) Uani 1 1 d . . . H20 H 0.6492 1.2213 -0.0899 0.032 Uiso 1 1 calc R . . C28 C 0.3051(4) 0.8797(2) 0.5610(2) 0.0246(7) Uani 1 1 d . . . H28 H 0.3453 0.8311 0.5980 0.030 Uiso 1 1 calc R . . C27 C 0.3109(4) 0.9761(2) 0.5701(2) 0.0291(7) Uani 1 1 d . . . H27 H 0.3537 1.0046 0.6147 0.035 Uiso 1 1 calc R . . C25 C 0.2395(3) 1.0267(2) 0.4990(2) 0.0231(7) Uani 1 1 d . . . C26 C 0.1896(3) 0.9538(2) 0.4503(2) 0.0190(6) Uani 1 1 d . . . C34 C 0.1455(4) 0.6457(2) 0.5900(2) 0.0249(7) Uani 1 1 d . . . H34 H 0.2411 0.6600 0.6014 0.030 Uiso 1 1 calc R . . C29 C 0.0926(3) 0.6822(2) 0.5107(2) 0.0211(6) Uani 1 1 d . . . C30 C -0.0504(3) 0.6592(2) 0.4940(2) 0.0219(6) Uani 1 1 d . . . H30 H -0.0856 0.6824 0.4404 0.026 Uiso 1 1 calc R . . C31 C -0.1405(4) 0.6020(2) 0.5564(2) 0.0252(7) Uani 1 1 d . . . H31 H -0.2360 0.5874 0.5451 0.030 Uiso 1 1 calc R . . C32 C -0.0876(4) 0.5666(3) 0.6355(2) 0.0301(8) Uani 1 1 d . . . H32 H -0.1481 0.5286 0.6777 0.036 Uiso 1 1 calc R . . C33 C 0.0553(4) 0.5874(3) 0.6525(2) 0.0308(8) Uani 1 1 d . . . H33 H 0.0909 0.5627 0.7055 0.037 Uiso 1 1 calc R . . C35 C 0.3815(3) 0.7106(2) 0.4076(2) 0.0196(6) Uani 1 1 d . . . C40 C 0.5004(3) 0.7706(2) 0.3754(2) 0.0252(7) Uani 1 1 d . . . H40 H 0.4857 0.8377 0.3730 0.030 Uiso 1 1 calc R . . C39 C 0.6401(3) 0.7297(3) 0.3472(2) 0.0285(7) Uani 1 1 d . . . H39 H 0.7192 0.7696 0.3262 0.034 Uiso 1 1 calc R . . C38 C 0.6627(4) 0.6294(3) 0.3501(2) 0.0297(7) Uani 1 1 d . . . H38 H 0.7560 0.6023 0.3300 0.036 Uiso 1 1 calc R . . C37 C 0.5447(4) 0.5700(2) 0.3832(2) 0.0275(7) Uani 1 1 d . . . H37 H 0.5599 0.5029 0.3866 0.033 Uiso 1 1 calc R . . C36 C 0.4044(4) 0.6105(2) 0.4113(2) 0.0244(7) Uani 1 1 d . . . H36 H 0.3255 0.5705 0.4326 0.029 Uiso 1 1 calc R . . C21 C 0.0454(3) 0.7221(2) 0.2744(2) 0.0238(7) Uani 1 1 d . . . C22 C 0.0916(4) 1.0603(2) 0.3485(2) 0.0262(7) Uani 1 1 d . . . H22 H 0.0404 1.0733 0.2986 0.031 Uiso 1 1 calc R . . C23 C 0.1382(4) 1.1375(2) 0.3908(2) 0.0292(7) Uani 1 1 d . . . H23 H 0.1187 1.2006 0.3682 0.035 Uiso 1 1 calc R . . C24 C 0.2136(4) 1.1221(3) 0.4661(2) 0.0288(7) Uiso 1 1 d . . . H24 H 0.2459 1.1739 0.4940 0.035 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01640(13) 0.02379(14) 0.01823(14) -0.00083(10) -0.00223(9) -0.00071(9) Rh2 0.01554(13) 0.02261(14) 0.01830(14) 0.00085(9) -0.00245(9) -0.00049(9) P1 0.0163(4) 0.0217(4) 0.0186(4) -0.0002(3) -0.0023(3) -0.0023(3) P2 0.0145(3) 0.0184(4) 0.0204(4) 0.0002(3) -0.0031(3) -0.0017(3) Cl1 0.0237(4) 0.0344(4) 0.0240(4) -0.0030(3) 0.0017(3) 0.0026(3) Cl2 0.0300(4) 0.0414(5) 0.0242(4) 0.0039(4) -0.0092(3) 0.0065(4) N1 0.0171(12) 0.0275(14) 0.0204(14) 0.0036(11) -0.0025(10) -0.0002(11) N2 0.0190(12) 0.0214(13) 0.0239(14) -0.0021(11) -0.0001(10) -0.0016(10) N3 0.0185(12) 0.0197(12) 0.0214(14) 0.0030(10) 0.0004(10) 0.0005(10) N4 0.0226(13) 0.0182(12) 0.0213(14) 0.0004(10) -0.0055(11) -0.0011(10) O1 0.0491(16) 0.0243(13) 0.0401(16) -0.0044(11) -0.0061(13) -0.0048(12) O2 0.0283(12) 0.0340(13) 0.0314(14) -0.0104(11) -0.0002(10) -0.0047(10) C1 0.0238(16) 0.0375(19) 0.0185(16) -0.0048(14) -0.0035(13) 0.0024(14) C2 0.0213(15) 0.0351(18) 0.0281(18) 0.0067(14) -0.0014(13) -0.0013(14) C3 0.0259(17) 0.0340(19) 0.038(2) 0.0101(16) -0.0047(15) -0.0079(15) C4 0.0285(17) 0.0232(16) 0.048(2) 0.0025(15) -0.0109(16) -0.0058(14) C5 0.0228(15) 0.0222(16) 0.036(2) -0.0004(14) -0.0092(14) -0.0033(13) C6 0.0164(14) 0.0254(15) 0.0213(16) 0.0014(12) -0.0072(12) -0.0017(12) C7 0.0323(18) 0.0254(17) 0.0316(19) -0.0052(14) -0.0058(15) -0.0008(14) C8 0.0250(16) 0.0285(17) 0.0256(18) -0.0016(14) -0.0009(13) 0.0004(13) C9 0.0164(14) 0.0229(15) 0.0262(17) -0.0015(12) -0.0045(12) -0.0019(12) C10 0.0202(15) 0.0323(17) 0.0245(17) 0.0017(14) -0.0033(13) 0.0005(13) C11 0.0260(17) 0.0344(19) 0.040(2) -0.0018(16) -0.0147(15) -0.0010(14) C12 0.0160(15) 0.0298(17) 0.046(2) -0.0039(15) -0.0064(14) -0.0006(13) C13 0.0210(16) 0.041(2) 0.038(2) 0.0027(16) 0.0028(15) -0.0062(15) C14 0.0218(16) 0.041(2) 0.0243(18) 0.0002(15) -0.0010(13) -0.0013(14) C15 0.0190(14) 0.0245(16) 0.0190(16) 0.0006(12) 0.0005(12) 0.0001(12) C16 0.053(2) 0.0241(17) 0.0265(19) -0.0032(14) -0.0069(17) -0.0024(16) C17 0.068(3) 0.0266(18) 0.029(2) -0.0003(15) -0.0010(19) 0.0098(18) C18 0.0310(18) 0.053(2) 0.0239(19) 0.0073(17) 0.0013(15) 0.0158(17) C19 0.0217(16) 0.052(2) 0.0249(18) 0.0013(16) -0.0038(14) -0.0047(15) C20 0.0199(15) 0.0363(18) 0.0241(17) 0.0012(14) -0.0021(13) -0.0076(14) C28 0.0271(16) 0.0242(16) 0.0252(17) -0.0013(13) -0.0132(14) -0.0023(13) C27 0.0313(18) 0.0276(17) 0.0306(19) -0.0040(14) -0.0115(15) -0.0011(14) C25 0.0196(15) 0.0216(15) 0.0272(18) -0.0046(13) 0.0009(13) 0.0017(12) C26 0.0132(13) 0.0182(14) 0.0246(16) 0.0002(12) 0.0010(11) -0.0006(11) C34 0.0214(15) 0.0276(16) 0.0260(18) 0.0002(13) -0.0051(13) -0.0010(13) C29 0.0173(14) 0.0197(14) 0.0263(17) -0.0008(12) -0.0019(12) -0.0027(12) C30 0.0188(14) 0.0209(15) 0.0265(17) -0.0012(12) -0.0050(12) -0.0027(12) C31 0.0216(15) 0.0234(16) 0.0304(18) -0.0025(13) -0.0003(13) -0.0049(13) C32 0.0329(18) 0.0267(17) 0.0280(19) 0.0052(14) 0.0048(15) -0.0071(14) C33 0.0358(19) 0.0321(18) 0.0242(18) 0.0054(14) -0.0064(15) -0.0018(15) C35 0.0159(14) 0.0215(15) 0.0212(16) -0.0013(12) -0.0017(12) -0.0013(12) C40 0.0189(15) 0.0211(15) 0.0360(19) 0.0005(13) -0.0062(13) -0.0036(12) C39 0.0154(15) 0.0336(18) 0.037(2) -0.0039(15) -0.0027(14) -0.0044(13) C38 0.0193(15) 0.0364(19) 0.035(2) -0.0090(15) -0.0057(14) 0.0007(14) C37 0.0257(16) 0.0206(16) 0.037(2) -0.0027(14) -0.0070(14) 0.0034(13) C36 0.0218(15) 0.0234(16) 0.0282(18) -0.0014(13) -0.0037(13) -0.0047(13) C21 0.0151(14) 0.0348(18) 0.0205(16) 0.0012(14) 0.0002(12) -0.0023(13) C22 0.0267(16) 0.0254(16) 0.0246(18) 0.0033(13) 0.0006(13) 0.0034(13) C23 0.0338(18) 0.0170(15) 0.034(2) 0.0043(13) 0.0032(15) 0.0031(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C1 1.821(4) . ? Rh1 N1 2.127(3) . ? Rh1 P1 2.1977(9) . ? Rh1 Cl1 2.3752(8) . ? Rh2 C21 1.821(3) . ? Rh2 N3 2.109(3) . ? Rh2 P2 2.2108(8) . ? Rh2 Cl2 2.3620(8) . ? P1 N2 1.712(3) . ? P1 C9 1.808(3) . ? P1 C15 1.809(3) . ? P2 N4 1.722(3) . ? P2 C29 1.812(3) . ? P2 C35 1.815(3) . ? N1 C6 1.326(4) . ? N1 C2 1.354(4) . ? N2 C6 1.380(4) . ? N2 C8 1.403(4) . ? N3 C26 1.336(4) . ? N3 C22 1.358(4) . ? N4 C26 1.372(4) . ? N4 C28 1.403(4) . ? O1 C1 1.146(4) . ? O2 C21 1.149(4) . ? C2 C3 1.400(5) . ? C3 C4 1.366(6) . ? C4 C5 1.392(5) . ? C5 C6 1.416(4) . ? C5 C7 1.439(5) . ? C7 C8 1.359(5) . ? C9 C14 1.386(5) . ? C9 C10 1.398(4) . ? C10 C11 1.393(4) . ? C11 C12 1.392(5) . ? C12 C13 1.379(5) . ? C13 C14 1.391(5) . ? C15 C20 1.378(4) . ? C15 C16 1.400(5) . ? C16 C17 1.386(5) . ? C17 C18 1.390(6) . ? C18 C19 1.366(6) . ? C19 C20 1.394(5) . ? C28 C27 1.355(5) . ? C27 C25 1.436(5) . ? C25 C24 1.395(5) . ? C25 C26 1.408(4) . ? C34 C29 1.388(4) . ? C34 C33 1.396(5) . ? C29 C30 1.396(4) . ? C30 C31 1.386(4) . ? C31 C32 1.382(5) . ? C32 C33 1.388(5) . ? C35 C36 1.389(4) . ? C35 C40 1.400(4) . ? C40 C39 1.387(5) . ? C39 C38 1.393(5) . ? C38 C37 1.392(5) . ? C37 C36 1.390(5) . ? C22 C23 1.387(5) . ? C23 C24 1.388(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Rh1 N1 173.92(13) . . ? C1 Rh1 P1 90.30(11) . . ? N1 Rh1 P1 84.41(8) . . ? C1 Rh1 Cl1 93.18(11) . . ? N1 Rh1 Cl1 92.04(8) . . ? P1 Rh1 Cl1 176.18(3) . . ? C21 Rh2 N3 177.67(12) . . ? C21 Rh2 P2 93.30(10) . . ? N3 Rh2 P2 84.57(7) . . ? C21 Rh2 Cl2 90.93(10) . . ? N3 Rh2 Cl2 91.28(7) . . ? P2 Rh2 Cl2 173.06(3) . . ? N2 P1 C9 104.38(14) . . ? N2 P1 C15 105.33(14) . . ? C9 P1 C15 105.99(14) . . ? N2 P1 Rh1 101.72(10) . . ? C9 P1 Rh1 122.04(11) . . ? C15 P1 Rh1 115.46(11) . . ? N4 P2 C29 106.39(14) . . ? N4 P2 C35 101.86(13) . . ? C29 P2 C35 105.43(14) . . ? N4 P2 Rh2 101.16(9) . . ? C29 P2 Rh2 117.52(10) . . ? C35 P2 Rh2 122.11(11) . . ? C6 N1 C2 115.0(3) . . ? C6 N1 Rh1 113.9(2) . . ? C2 N1 Rh1 131.0(2) . . ? C6 N2 C8 107.2(3) . . ? C6 N2 P1 116.7(2) . . ? C8 N2 P1 136.0(2) . . ? C26 N3 C22 115.1(3) . . ? C26 N3 Rh2 114.2(2) . . ? C22 N3 Rh2 130.6(2) . . ? C26 N4 C28 106.9(2) . . ? C26 N4 P2 116.6(2) . . ? C28 N4 P2 136.1(2) . . ? O1 C1 Rh1 178.7(3) . . ? N1 C2 C3 121.8(3) . . ? C4 C3 C2 121.6(3) . . ? C3 C4 C5 118.6(3) . . ? C4 C5 C6 115.3(3) . . ? C4 C5 C7 139.0(3) . . ? C6 C5 C7 105.6(3) . . ? N1 C6 N2 123.1(3) . . ? N1 C6 C5 127.6(3) . . ? N2 C6 C5 109.3(3) . . ? C8 C7 C5 107.9(3) . . ? C7 C8 N2 109.9(3) . . ? C14 C9 C10 119.3(3) . . ? C14 C9 P1 122.7(2) . . ? C10 C9 P1 117.9(2) . . ? C11 C10 C9 120.2(3) . . ? C12 C11 C10 119.6(3) . . ? C13 C12 C11 120.5(3) . . ? C12 C13 C14 119.9(3) . . ? C9 C14 C13 120.6(3) . . ? C20 C15 C16 118.6(3) . . ? C20 C15 P1 122.2(2) . . ? C16 C15 P1 118.6(2) . . ? C17 C16 C15 120.3(3) . . ? C16 C17 C18 120.0(4) . . ? C19 C18 C17 119.8(3) . . ? C18 C19 C20 120.2(3) . . ? C15 C20 C19 120.9(3) . . ? C27 C28 N4 109.8(3) . . ? C28 C27 C25 108.0(3) . . ? C24 C25 C26 116.2(3) . . ? C24 C25 C27 138.3(3) . . ? C26 C25 C27 105.4(3) . . ? N3 C26 N4 123.2(3) . . ? N3 C26 C25 126.9(3) . . ? N4 C26 C25 109.8(3) . . ? C29 C34 C33 120.1(3) . . ? C34 C29 C30 119.4(3) . . ? C34 C29 P2 123.2(2) . . ? C30 C29 P2 117.3(2) . . ? C31 C30 C29 120.6(3) . . ? C32 C31 C30 119.7(3) . . ? C31 C32 C33 120.4(3) . . ? C32 C33 C34 119.9(3) . . ? C36 C35 C40 119.8(3) . . ? C36 C35 P2 121.4(2) . . ? C40 C35 P2 118.4(2) . . ? C39 C40 C35 119.7(3) . . ? C40 C39 C38 120.5(3) . . ? C37 C38 C39 119.6(3) . . ? C36 C37 C38 120.2(3) . . ? C37 C36 C35 120.2(3) . . ? O2 C21 Rh2 177.1(3) . . ? N3 C22 C23 122.6(3) . . ? C22 C23 C24 121.0(3) . . ? C23 C24 C25 118.1(3) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.708 _refine_diff_density_min -1.122 _refine_diff_density_rms 0.135 #===END data_compound3b_h01adb4 _database_code_CSD 217635 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H13 Cl N4 O P Rh' _chemical_formula_weight 446.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.71300(10) _cell_length_b 11.0150(2) _cell_length_c 17.8380(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.2540(10) _cell_angle_gamma 90.00 _cell_volume 1689.70(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 18 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.756 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 1.274 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.70 _exptl_absorpt_correction_T_max 0.80 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29040 _diffrn_reflns_av_R_equivalents 0.0323 _diffrn_reflns_av_sigmaI/netI 0.0213 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3794 _reflns_number_gt 3675 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'Denzo and Scalepack (otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+1.5445*P+(0.0351P)^2^+0.0000sin\q/\l] where P = 0.00000Fo^2^ + 1.00000Fc^2^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0113(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3794 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0225 _refine_ls_R_factor_gt 0.0217 _refine_ls_wR_factor_ref 0.0615 _refine_ls_wR_factor_gt 0.0608 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.184388(14) 0.215684(11) 0.273641(7) 0.01613(8) Uani 1 1 d . . . P1 P 0.08027(5) 0.26265(4) 0.15886(2) 0.01670(10) Uani 1 1 d . . . Cl2 Cl 0.31314(5) 0.15820(4) 0.39520(2) 0.02309(11) Uani 1 1 d . . . C3 C 0.4334(2) -0.10875(19) 0.20516(12) 0.0327(4) Uani 1 1 d . . . H3 H 0.4993 -0.1730 0.2279 0.039 Uiso 1 1 d R . . N3 N 0.12093(17) 0.39359(14) 0.11655(9) 0.0203(3) Uani 1 1 d . . . N4 N -0.11426(17) 0.25920(15) 0.13310(9) 0.0208(3) Uani 1 1 d . . . O1 O 0.03852(19) 0.42672(15) 0.33848(9) 0.0382(4) Uani 1 1 d . . . N2 N 0.15848(18) 0.15870(14) 0.10545(8) 0.0212(3) Uani 1 1 d . . . C4 C 0.4006(2) -0.10314(18) 0.12673(12) 0.0297(4) Uani 1 1 d . . . H4 H 0.4419 -0.1617 0.0954 0.036 Uiso 1 1 d R . . C16 C -0.2112(2) 0.19497(18) 0.17420(11) 0.0249(4) Uani 1 1 d . . . H16 H -0.1916 0.1545 0.2225 0.030 Uiso 1 1 d R . . N1 N 0.28207(17) 0.06867(14) 0.22094(8) 0.0195(3) Uani 1 1 d . . . C6 C 0.2390(2) 0.03284(19) 0.01945(11) 0.0290(4) Uani 1 1 d . . . H6 H 0.2467 0.0035 -0.0305 0.035 Uiso 1 1 d R . . C12 C 0.0509(2) 0.50442(17) 0.12873(11) 0.0267(4) Uani 1 1 d . . . H12 H -0.0490 0.5233 0.1419 0.032 Uiso 1 1 d R . . C1 C 0.0950(2) 0.34640(18) 0.31305(10) 0.0238(4) Uani 1 1 d . . . C8 C 0.25043(19) 0.07057(15) 0.14505(10) 0.0185(3) Uani 1 1 d . . . C13 C -0.2045(2) 0.29988(19) 0.06590(11) 0.0263(4) Uani 1 1 d . . . H13 H -0.1784 0.3450 0.0237 0.032 Uiso 1 1 d R . . C15 C -0.3573(2) 0.1969(2) 0.13386(13) 0.0307(4) Uani 1 1 d . . . H15 H -0.4535 0.1619 0.1430 0.037 Uiso 1 1 d R . . C2 C 0.3739(2) -0.02300(18) 0.25077(11) 0.0271(4) Uani 1 1 d . . . H2 H 0.4001 -0.0312 0.3049 0.033 Uiso 1 1 d R . . C5 C 0.3035(2) -0.01026(17) 0.09411(11) 0.0228(4) Uani 1 1 d . . . C14 C -0.3532(2) 0.2636(2) 0.06579(12) 0.0299(4) Uani 1 1 d . . . H14 H -0.4467 0.2765 0.0302 0.036 Uiso 1 1 d R . . C7 C 0.1537(2) 0.13333(19) 0.02775(10) 0.0280(4) Uani 1 1 d . . . H7 H 0.1011 0.1753 -0.0162 0.034 Uiso 1 1 d R . . C9 C 0.2706(2) 0.41922(19) 0.10214(12) 0.0284(4) Uani 1 1 d . . . H9 H 0.3537 0.3672 0.0925 0.034 Uiso 1 1 d R . . C11 C 0.1513(3) 0.59483(18) 0.11998(11) 0.0309(4) Uani 1 1 d . . . H11 H 0.1432 0.6816 0.1230 0.037 Uiso 1 1 d R . . C10 C 0.2904(2) 0.5410(2) 0.10309(12) 0.0325(4) Uani 1 1 d . . . H10 H 0.3762 0.5913 0.0949 0.039 Uiso 1 1 d 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 Rh1 0.01472(10) 0.01708(10) 0.01626(10) 0.00042(4) 0.00153(5) 0.00067(4) P1 0.0150(2) 0.0183(2) 0.0167(2) 0.00144(15) 0.00225(15) 0.00200(15) Cl2 0.0218(2) 0.0273(2) 0.0187(2) 0.00148(15) -0.00112(15) 0.00025(16) C3 0.0339(10) 0.0270(10) 0.0355(11) 0.0007(8) 0.0002(8) 0.0136(8) N3 0.0175(7) 0.0200(7) 0.0241(7) 0.0039(6) 0.0059(5) 0.0032(5) N4 0.0165(7) 0.0258(7) 0.0199(7) 0.0031(6) 0.0020(5) 0.0013(6) O1 0.0443(9) 0.0368(8) 0.0334(8) -0.0083(6) 0.0063(7) 0.0167(7) N2 0.0237(7) 0.0206(7) 0.0188(7) 0.0006(6) 0.0024(5) 0.0039(6) C4 0.0322(10) 0.0234(9) 0.0338(10) -0.0044(8) 0.0064(8) 0.0069(8) C16 0.0224(9) 0.0266(9) 0.0269(9) 0.0002(7) 0.0077(7) -0.0037(7) N1 0.0193(6) 0.0180(7) 0.0206(7) -0.0002(5) 0.0014(5) 0.0013(6) C6 0.0353(10) 0.0297(10) 0.0226(9) -0.0029(7) 0.0060(7) 0.0047(8) C12 0.0313(10) 0.0230(9) 0.0279(9) 0.0033(7) 0.0110(7) 0.0082(7) C1 0.0226(8) 0.0286(9) 0.0197(8) 0.0023(7) 0.0016(6) 0.0021(7) C8 0.0163(7) 0.0170(7) 0.0223(8) -0.0001(6) 0.0034(6) -0.0007(6) C13 0.0217(9) 0.0372(10) 0.0185(9) 0.0032(7) -0.0014(7) 0.0051(8) C15 0.0196(9) 0.0355(10) 0.0376(11) -0.0067(8) 0.0061(8) -0.0045(8) C2 0.0287(9) 0.0244(9) 0.0266(9) 0.0009(7) -0.0010(7) 0.0073(7) C5 0.0228(8) 0.0210(8) 0.0253(9) -0.0027(7) 0.0054(7) -0.0005(7) C14 0.0200(9) 0.0396(11) 0.0280(10) -0.0086(8) -0.0029(7) 0.0046(8) C7 0.0356(10) 0.0313(10) 0.0169(8) 0.0000(7) 0.0036(7) 0.0064(8) C9 0.0192(8) 0.0326(10) 0.0349(10) 0.0114(8) 0.0093(7) 0.0032(7) C11 0.0447(12) 0.0213(9) 0.0272(10) 0.0032(7) 0.0070(8) 0.0008(8) C10 0.0254(9) 0.0344(11) 0.0363(11) 0.0127(9) 0.0007(8) -0.0063(8) _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 Rh1 C1 1.8305(19) . ? Rh1 N1 2.1184(15) . ? Rh1 P1 2.1646(4) . ? Rh1 Cl2 2.3620(4) . ? P1 N4 1.6837(16) . ? P1 N3 1.6915(15) . ? P1 N2 1.7006(15) . ? C3 C4 1.384(3) . ? C3 C2 1.399(3) . ? N3 C12 1.397(2) . ? N3 C9 1.398(2) . ? N4 C16 1.397(2) . ? N4 C13 1.397(2) . ? O1 C1 1.141(2) . ? N2 C8 1.379(2) . ? N2 C7 1.408(2) . ? C4 C5 1.394(3) . ? C16 C15 1.358(3) . ? N1 C8 1.338(2) . ? N1 C2 1.344(2) . ? C6 C7 1.355(3) . ? C6 C5 1.440(3) . ? C12 C11 1.351(3) . ? C8 C5 1.403(2) . ? C13 C14 1.355(3) . ? C15 C14 1.425(3) . ? C9 C10 1.353(3) . ? C11 C10 1.425(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 C1 Rh1 N1 176.30(7) . . ? C1 Rh1 P1 92.05(6) . . ? N1 Rh1 P1 84.27(4) . . ? C1 Rh1 Cl2 91.54(6) . . ? N1 Rh1 Cl2 92.12(4) . . ? P1 Rh1 Cl2 175.852(16) . . ? N4 P1 N3 99.87(8) . . ? N4 P1 N2 107.97(8) . . ? N3 P1 N2 101.11(8) . . ? N4 P1 Rh1 120.21(6) . . ? N3 P1 Rh1 122.67(6) . . ? N2 P1 Rh1 102.96(5) . . ? C4 C3 C2 121.49(18) . . ? C12 N3 C9 107.19(16) . . ? C12 N3 P1 123.21(12) . . ? C9 N3 P1 121.52(13) . . ? C16 N4 C13 107.96(15) . . ? C16 N4 P1 122.38(13) . . ? C13 N4 P1 129.03(13) . . ? C8 N2 C7 106.70(15) . . ? C8 N2 P1 116.05(12) . . ? C7 N2 P1 137.23(13) . . ? C3 C4 C5 117.88(18) . . ? C15 C16 N4 107.97(18) . . ? C8 N1 C2 115.16(15) . . ? C8 N1 Rh1 113.89(11) . . ? C2 N1 Rh1 130.91(13) . . ? C7 C6 C5 107.92(17) . . ? C11 C12 N3 108.64(17) . . ? O1 C1 Rh1 178.92(18) . . ? N1 C8 N2 122.53(15) . . ? N1 C8 C5 127.59(16) . . ? N2 C8 C5 109.87(15) . . ? C14 C13 N4 108.21(18) . . ? C16 C15 C14 108.04(18) . . ? N1 C2 C3 121.98(18) . . ? C4 C5 C8 115.89(17) . . ? C4 C5 C6 138.46(18) . . ? C8 C5 C6 105.63(16) . . ? C13 C14 C15 107.82(17) . . ? C6 C7 N2 109.87(17) . . ? C10 C9 N3 108.61(18) . . ? C12 C11 C10 107.84(18) . . ? C9 C10 C11 107.69(18) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.625 _refine_diff_density_min -0.586 _refine_diff_density_rms 0.064 #===END data_compound7a_k01adb3 _database_code_CSD 217636 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H18 F3 N2 O4 P Pd S' _chemical_formula_weight 600.81 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' F F 0.0171 0.0103 '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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.22800(10) _cell_length_b 9.3830(2) _cell_length_c 14.8820(2) _cell_angle_alpha 77.7580(8) _cell_angle_beta 77.8980(8) _cell_angle_gamma 75.6470(9) _cell_volume 1203.06(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 18 _exptl_crystal_description Tabloid _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.659 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 600 _exptl_absorpt_coefficient_mu 0.979 _exptl_absorpt_correction_type multiscan _exptl_absorpt_process_details 'Sortav Blessing (1995) ' _exptl_absorpt_correction_T_min 0.8282 _exptl_absorpt_correction_T_max 0.9258 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22342 _diffrn_reflns_av_R_equivalents 0.0511 _diffrn_reflns_av_sigmaI/netI 0.0432 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.33 _diffrn_reflns_theta_max 27.54 _reflns_number_total 5517 _reflns_number_gt 4881 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'Denzo and Scalepack (otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+0.5637P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0060(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5517 _refine_ls_number_parameters 309 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0379 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0808 _refine_ls_wR_factor_gt 0.0767 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.735607(17) -0.120492(19) 0.252665(11) 0.01915(8) Uani 1 1 d . . . S1 S 0.97567(6) -0.45107(7) 0.27645(4) 0.02597(14) Uani 1 1 d . . . P1 P 0.55837(6) 0.07921(7) 0.21727(4) 0.01833(13) Uani 1 1 d . . . F1 F 0.8993(5) -0.5437(3) 0.45368(15) 0.1209(13) Uani 1 1 d . . . F2 F 0.9139(4) -0.7035(2) 0.36745(18) 0.1045(11) Uani 1 1 d . . . F3 F 0.7261(3) -0.5128(3) 0.3742(2) 0.1128(12) Uani 1 1 d . . . O1 O 0.91447(19) -0.29910(19) 0.29554(13) 0.0302(4) Uani 1 1 d . . . O2 O 1.1304(2) -0.5015(3) 0.28617(19) 0.0561(6) Uani 1 1 d . . . O3 O 0.9350(3) -0.4804(2) 0.19631(15) 0.0483(5) Uani 1 1 d . . . O4 O 0.6535(2) -0.2344(3) 0.11284(15) 0.0437(5) Uani 1 1 d . . . N1 N 0.5330(2) 0.1588(2) 0.31484(13) 0.0217(4) Uani 1 1 d . . . N2 N 0.7210(2) -0.0356(2) 0.38145(13) 0.0226(4) Uani 1 1 d . . . C1 C 0.6091(2) 0.2214(3) 0.12153(15) 0.0198(5) Uani 1 1 d . . . C2 C 0.6990(3) 0.3146(3) 0.13222(17) 0.0257(5) Uani 1 1 d . . . H2 H 0.7222 0.3120 0.1919 0.031 Uiso 1 1 calc R . . C3 C 0.7540(3) 0.4107(3) 0.05593(18) 0.0319(6) Uani 1 1 d . . . H3 H 0.8143 0.4748 0.0632 0.038 Uiso 1 1 calc R . . C4 C 0.7211(3) 0.4135(3) -0.03120(18) 0.0324(6) Uani 1 1 d . . . H4 H 0.7609 0.4781 -0.0838 0.039 Uiso 1 1 calc R . . C5 C 0.6309(3) 0.3231(3) -0.04202(17) 0.0305(6) Uani 1 1 d . . . H5 H 0.6072 0.3272 -0.1018 0.037 Uiso 1 1 calc R . . C6 C 0.5747(3) 0.2262(3) 0.03382(16) 0.0264(5) Uani 1 1 d . . . H6 H 0.5132 0.1635 0.0261 0.032 Uiso 1 1 calc R . . C7 C 0.3735(2) 0.0557(3) 0.20909(15) 0.0210(5) Uani 1 1 d . . . C8 C 0.3442(3) -0.0872(3) 0.23108(16) 0.0248(5) Uani 1 1 d . . . H8 H 0.4234 -0.1714 0.2438 0.030 Uiso 1 1 calc R . . C9 C 0.1978(3) -0.1063(3) 0.23431(18) 0.0323(6) Uani 1 1 d . . . H9 H 0.1764 -0.2033 0.2501 0.039 Uiso 1 1 calc R . . C10 C 0.0850(3) 0.0166(3) 0.21446(19) 0.0337(6) Uani 1 1 d . . . H10 H -0.0146 0.0033 0.2170 0.040 Uiso 1 1 calc R . . C11 C 0.1132(3) 0.1592(3) 0.19088(18) 0.0318(6) Uani 1 1 d . . . H11 H 0.0340 0.2426 0.1767 0.038 Uiso 1 1 calc R . . C12 C 0.2585(3) 0.1791(3) 0.18810(17) 0.0265(5) Uani 1 1 d . . . H12 H 0.2793 0.2764 0.1720 0.032 Uiso 1 1 calc R . . C13 C 0.4378(3) 0.2892(3) 0.34284(17) 0.0263(5) Uani 1 1 d . . . H13 H 0.3667 0.3573 0.3080 0.032 Uiso 1 1 calc R . . C14 C 0.4622(3) 0.3037(3) 0.42681(18) 0.0302(6) Uani 1 1 d . . . H14 H 0.4118 0.3823 0.4606 0.036 Uiso 1 1 calc R . . C15 C 0.5779(3) 0.1790(3) 0.45520(16) 0.0263(5) Uani 1 1 d . . . C16 C 0.6578(3) 0.1263(3) 0.53020(17) 0.0330(6) Uani 1 1 d . . . H16 H 0.6382 0.1796 0.5806 0.040 Uiso 1 1 calc R . . C17 C 0.7656(3) -0.0047(3) 0.52889(17) 0.0354(6) Uani 1 1 d . . . H17 H 0.8206 -0.0424 0.5792 0.042 Uiso 1 1 calc R . . C18 C 0.7952(3) -0.0832(3) 0.45470(17) 0.0298(6) Uani 1 1 d . . . H18 H 0.8703 -0.1732 0.4560 0.036 Uiso 1 1 calc R . . C19 C 0.6180(2) 0.0921(3) 0.38453(15) 0.0211(5) Uani 1 1 d . . . C20 C 0.8738(5) -0.5589(4) 0.3739(3) 0.0641(11) Uani 1 1 d . . . C21 C 0.7449(3) -0.1786(3) 0.12991(18) 0.0281(5) Uani 1 1 d . . . C22 C 0.8835(3) -0.1464(4) 0.06087(19) 0.0435(7) Uani 1 1 d . . . H22A H 0.9732 -0.1811 0.0915 0.052 Uiso 1 1 calc R . . H22B H 0.8696 -0.0388 0.0382 0.052 Uiso 1 1 calc R . . H22C H 0.8973 -0.1986 0.0082 0.052 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01735(11) 0.01948(12) 0.02102(11) -0.00300(7) -0.00534(7) -0.00321(7) S1 0.0221(3) 0.0213(3) 0.0320(3) -0.0030(2) -0.0043(2) -0.0015(2) P1 0.0167(3) 0.0194(3) 0.0198(3) -0.0028(2) -0.0053(2) -0.0039(2) F1 0.225(4) 0.0811(19) 0.0310(12) -0.0008(12) 0.0127(16) -0.021(2) F2 0.158(3) 0.0321(12) 0.0924(18) -0.0094(11) 0.0612(18) -0.0336(14) F3 0.0686(16) 0.092(2) 0.168(3) -0.047(2) 0.0637(18) -0.0488(15) O1 0.0252(9) 0.0227(9) 0.0442(10) -0.0061(8) -0.0166(8) 0.0015(7) O2 0.0267(10) 0.0406(13) 0.0977(19) -0.0146(12) -0.0170(11) 0.0068(9) O3 0.0674(15) 0.0349(12) 0.0434(12) -0.0144(9) -0.0197(11) 0.0031(10) O4 0.0354(10) 0.0545(14) 0.0512(12) -0.0301(11) -0.0140(9) -0.0045(9) N1 0.0183(9) 0.0247(11) 0.0225(10) -0.0060(8) -0.0044(8) -0.0024(8) N2 0.0219(9) 0.0259(11) 0.0210(10) -0.0012(8) -0.0057(8) -0.0072(8) C1 0.0174(10) 0.0195(11) 0.0218(11) -0.0043(9) -0.0031(8) -0.0017(9) C2 0.0244(12) 0.0281(13) 0.0269(12) -0.0048(10) -0.0064(10) -0.0078(10) C3 0.0305(13) 0.0272(14) 0.0387(14) -0.0034(11) -0.0025(11) -0.0120(11) C4 0.0316(13) 0.0281(14) 0.0288(13) 0.0031(11) 0.0038(11) -0.0044(11) C5 0.0351(13) 0.0328(14) 0.0209(12) -0.0045(10) -0.0041(10) -0.0032(11) C6 0.0271(12) 0.0286(13) 0.0253(12) -0.0058(10) -0.0067(10) -0.0064(10) C7 0.0194(10) 0.0267(13) 0.0193(11) -0.0060(9) -0.0029(9) -0.0079(9) C8 0.0249(12) 0.0265(13) 0.0244(12) -0.0056(10) -0.0037(9) -0.0073(10) C9 0.0320(13) 0.0371(15) 0.0333(13) -0.0103(11) 0.0009(11) -0.0193(11) C10 0.0192(11) 0.0489(17) 0.0394(15) -0.0177(13) 0.0004(10) -0.0150(11) C11 0.0201(11) 0.0418(16) 0.0353(14) -0.0125(12) -0.0071(10) -0.0028(11) C12 0.0244(12) 0.0285(13) 0.0281(12) -0.0047(10) -0.0066(10) -0.0066(10) C13 0.0215(11) 0.0250(13) 0.0314(13) -0.0084(10) -0.0024(10) -0.0015(10) C14 0.0290(13) 0.0312(14) 0.0315(13) -0.0136(11) 0.0008(10) -0.0062(11) C15 0.0273(12) 0.0320(14) 0.0222(12) -0.0069(10) 0.0005(9) -0.0134(10) C16 0.0416(15) 0.0409(16) 0.0211(12) -0.0069(11) -0.0055(11) -0.0158(13) C17 0.0423(15) 0.0453(17) 0.0227(12) 0.0018(11) -0.0137(11) -0.0162(13) C18 0.0302(13) 0.0321(14) 0.0275(13) 0.0000(11) -0.0117(10) -0.0062(11) C19 0.0202(11) 0.0251(12) 0.0197(11) -0.0014(9) -0.0019(9) -0.0110(9) C20 0.087(3) 0.0364(19) 0.056(2) -0.0089(16) 0.030(2) -0.0228(18) C21 0.0268(12) 0.0261(13) 0.0298(13) -0.0082(10) -0.0102(10) 0.0050(10) C22 0.0430(16) 0.054(2) 0.0278(14) -0.0118(13) 0.0036(12) -0.0044(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C21 1.994(3) . ? Pd1 O1 2.1346(16) . ? Pd1 N2 2.193(2) . ? Pd1 P1 2.2106(6) . ? S1 O2 1.416(2) . ? S1 O3 1.420(2) . ? S1 O1 1.4624(19) . ? S1 C20 1.813(3) . ? P1 N1 1.718(2) . ? P1 C1 1.803(2) . ? P1 C7 1.805(2) . ? F1 C20 1.300(5) . ? F2 C20 1.334(4) . ? F3 C20 1.323(5) . ? O4 C21 1.190(3) . ? N1 C19 1.380(3) . ? N1 C13 1.404(3) . ? N2 C19 1.335(3) . ? N2 C18 1.346(3) . ? C1 C6 1.396(3) . ? C1 C2 1.398(3) . ? C2 C3 1.383(3) . ? C3 C4 1.386(4) . ? C4 C5 1.380(4) . ? C5 C6 1.387(3) . ? C7 C8 1.391(3) . ? C7 C12 1.393(3) . ? C8 C9 1.396(3) . ? C9 C10 1.375(4) . ? C10 C11 1.384(4) . ? C11 C12 1.390(3) . ? C13 C14 1.355(4) . ? C14 C15 1.431(4) . ? C15 C19 1.400(3) . ? C15 C16 1.402(3) . ? C16 C17 1.377(4) . ? C17 C18 1.398(4) . ? C21 C22 1.513(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 C21 Pd1 O1 95.59(8) . . ? C21 Pd1 N2 174.85(9) . . ? O1 Pd1 N2 88.53(7) . . ? C21 Pd1 P1 89.83(7) . . ? O1 Pd1 P1 173.67(5) . . ? N2 Pd1 P1 85.89(5) . . ? O2 S1 O3 116.23(15) . . ? O2 S1 O1 112.30(12) . . ? O3 S1 O1 114.80(11) . . ? O2 S1 C20 105.18(19) . . ? O3 S1 C20 104.58(18) . . ? O1 S1 C20 101.77(14) . . ? N1 P1 C1 104.49(10) . . ? N1 P1 C7 105.83(10) . . ? C1 P1 C7 107.50(10) . . ? N1 P1 Pd1 99.50(7) . . ? C1 P1 Pd1 118.18(7) . . ? C7 P1 Pd1 119.16(8) . . ? S1 O1 Pd1 135.02(11) . . ? C19 N1 C13 106.71(19) . . ? C19 N1 P1 120.29(16) . . ? C13 N1 P1 133.00(17) . . ? C19 N2 C18 115.2(2) . . ? C19 N2 Pd1 111.09(15) . . ? C18 N2 Pd1 133.69(18) . . ? C6 C1 C2 119.8(2) . . ? C6 C1 P1 119.91(18) . . ? C2 C1 P1 119.82(17) . . ? C3 C2 C1 119.9(2) . . ? C2 C3 C4 120.0(2) . . ? C5 C4 C3 120.4(2) . . ? C4 C5 C6 120.4(2) . . ? C5 C6 C1 119.5(2) . . ? C8 C7 C12 120.3(2) . . ? C8 C7 P1 118.77(18) . . ? C12 C7 P1 120.75(18) . . ? C7 C8 C9 119.7(2) . . ? C10 C9 C8 119.4(2) . . ? C9 C10 C11 121.5(2) . . ? C10 C11 C12 119.4(2) . . ? C11 C12 C7 119.7(2) . . ? C14 C13 N1 110.1(2) . . ? C13 C14 C15 107.4(2) . . ? C19 C15 C16 115.7(2) . . ? C19 C15 C14 106.5(2) . . ? C16 C15 C14 137.8(2) . . ? C17 C16 C15 118.2(2) . . ? C16 C17 C18 121.1(2) . . ? N2 C18 C17 122.3(2) . . ? N2 C19 N1 123.2(2) . . ? N2 C19 C15 127.5(2) . . ? N1 C19 C15 109.3(2) . . ? F1 C20 F3 107.1(3) . . ? F1 C20 F2 108.3(4) . . ? F3 C20 F2 109.0(4) . . ? F1 C20 S1 112.2(3) . . ? F3 C20 S1 109.7(3) . . ? F2 C20 S1 110.4(2) . . ? O4 C21 C22 123.5(2) . . ? O4 C21 Pd1 124.1(2) . . ? C22 C21 Pd1 112.41(19) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.486 _refine_diff_density_min -0.552 _refine_diff_density_rms 0.084 #===END data_compound7b_k01adb5 _database_code_CSD 217637 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H16 F3 N4 O4 P Pd S' _chemical_formula_weight 578.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.41300(10) _cell_length_b 13.4650(2) _cell_length_c 21.9600(3) _cell_angle_alpha 88.8130(5) _cell_angle_beta 77.8690(5) _cell_angle_gamma 81.8480(6) _cell_volume 3265.89(7) _cell_formula_units_Z 6 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 18 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.766 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 1.081 _exptl_absorpt_correction_type multiscan _exptl_absorpt_process_details 'Sortav Blessing (1995) ' _exptl_absorpt_correction_T_min 0.7739 _exptl_absorpt_correction_T_max 0.8129 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29069 _diffrn_reflns_av_R_equivalents 0.0684 _diffrn_reflns_av_sigmaI/netI 0.0548 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.51 _diffrn_reflns_theta_max 23.00 _reflns_number_total 9023 _reflns_number_gt 8036 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'Denzo and Scalepack (otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0737P)^2^+10.7337P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0026(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9023 _refine_ls_number_parameters 869 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.1102 _refine_ls_wR_factor_gt 0.1024 _refine_ls_goodness_of_fit_ref 0.880 _refine_ls_restrained_S_all 0.880 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd -0.45620(3) -0.48466(3) -0.330579(16) 0.02877(13) Uani 1 1 d . . . Pd2 Pd 0.16096(3) 0.11380(2) -0.672022(15) 0.02270(13) Uani 1 1 d . . . Pd3 Pd 0.05310(3) 0.19207(2) -0.086023(14) 0.01918(13) Uani 1 1 d . . . S1 S -0.73033(11) -0.42064(11) -0.26908(6) 0.0380(3) Uani 1 1 d . . . S2 S 0.18006(14) 0.15213(10) -0.52311(6) 0.0416(3) Uani 1 1 d . . . S3 S -0.17035(11) 0.35805(8) -0.08332(5) 0.0278(3) Uani 1 1 d . . . P1 P -0.28187(10) -0.55925(9) -0.38113(5) 0.0238(3) Uani 1 1 d . . . P2 P 0.14472(10) 0.11040(8) -0.76932(5) 0.0199(3) Uani 1 1 d . . . P3 P 0.24478(10) 0.13277(8) -0.11362(5) 0.0207(3) Uani 1 1 d . . . F1 F -0.6840(3) -0.4863(2) -0.16260(14) 0.0503(8) Uani 1 1 d . . . F2 F -0.7819(4) -0.3394(3) -0.15806(16) 0.0742(12) Uani 1 1 d . . . F3 F -0.8707(3) -0.4645(3) -0.16682(19) 0.0742(12) Uani 1 1 d . . . F4 F 0.3598(5) 0.1387(4) -0.46479(19) 0.0956(17) Uani 1 1 d . . . F5 F 0.3724(4) 0.0171(4) -0.5265(2) 0.0817(12) Uani 1 1 d . . . F6 F 0.4101(5) 0.1634(5) -0.5620(2) 0.111(2) Uani 1 1 d . . . F7 F -0.3469(3) 0.3775(2) 0.01559(16) 0.0557(9) Uani 1 1 d . . . F8 F -0.3069(4) 0.5149(2) -0.02862(17) 0.0692(11) Uani 1 1 d . . . F9 F -0.1894(4) 0.4376(3) 0.02600(16) 0.0688(11) Uani 1 1 d . . . O1 O -0.4592(4) -0.6341(3) -0.23856(19) 0.0549(11) Uani 1 1 d . . . O2 O -0.6117(3) -0.3871(3) -0.28154(17) 0.0397(8) Uani 1 1 d . . . O3 O -0.8241(3) -0.3473(3) -0.28410(15) 0.0348(8) Uani 1 1 d . . . O4 O -0.7245(4) -0.5231(3) -0.2903(2) 0.0555(11) Uani 1 1 d . . . O5 O 0.4135(3) 0.0574(3) -0.69955(19) 0.0435(9) Uani 1 1 d . . . O6 O 0.1743(4) 0.0940(3) -0.57764(16) 0.0459(9) Uani 1 1 d . . . O7 O 0.1145(4) 0.1099(4) -0.46794(19) 0.0688(13) Uani 1 1 d . . . O8 O 0.1665(9) 0.2553(4) -0.5311(3) 0.133(3) Uani 1 1 d . . . O9 O 0.0480(3) 0.1420(3) 0.03889(15) 0.0390(9) Uani 1 1 d . . . O10 O -0.2560(4) 0.3543(3) -0.12143(18) 0.0538(11) Uani 1 1 d . . . O11 O -0.1314(3) 0.2603(2) -0.05742(14) 0.0253(7) Uani 1 1 d . . . O12 O -0.0726(3) 0.4134(3) -0.1050(2) 0.0513(10) Uani 1 1 d . . . N1 N -0.4749(3) -0.4173(3) -0.42027(17) 0.0256(8) Uani 1 1 d . . . N2 N -0.2784(3) -0.5127(3) -0.45363(17) 0.0252(8) Uani 1 1 d . . . N3 N -0.1486(3) -0.5340(3) -0.36851(18) 0.0271(9) Uani 1 1 d . . . N4 N -0.2548(3) -0.6852(3) -0.38558(18) 0.0279(9) Uani 1 1 d . . . N5 N -0.0346(3) 0.1071(3) -0.65135(17) 0.0250(8) Uani 1 1 d . . . N6 N -0.0053(3) 0.1116(3) -0.76226(16) 0.0238(8) Uani 1 1 d . . . N7 N 0.1704(3) 0.2054(3) -0.81905(16) 0.0218(8) Uani 1 1 d . . . N8 N 0.2184(3) 0.0121(3) -0.81326(16) 0.0228(8) Uani 1 1 d . . . N9 N 0.0541(3) 0.1758(3) -0.18584(16) 0.0227(8) Uani 1 1 d . . . N10 N 0.2686(3) 0.1436(3) -0.19224(17) 0.0244(8) Uani 1 1 d . . . N11 N 0.3575(3) 0.1888(3) -0.09723(17) 0.0226(8) Uani 1 1 d . . . N12 N 0.2900(3) 0.0130(3) -0.09734(18) 0.0268(9) Uani 1 1 d . . . C1 C -0.5622(4) -0.3542(3) -0.4396(2) 0.0289(11) Uani 1 1 d . . . H1 H -0.6341 -0.3306 -0.4102 0.035 Uiso 1 1 calc R . . C2 C -0.5511(5) -0.3224(4) -0.5007(2) 0.0329(11) Uani 1 1 d . . . H2 H -0.6151 -0.2778 -0.5121 0.039 Uiso 1 1 calc R . . C3 C -0.4487(5) -0.3545(4) -0.5454(2) 0.0325(11) Uani 1 1 d . . . H3 H -0.4414 -0.3325 -0.5873 0.039 Uiso 1 1 calc R . . C4 C -0.3567(4) -0.4197(3) -0.5275(2) 0.0296(11) Uani 1 1 d . . . C5 C -0.3772(4) -0.4468(3) -0.4646(2) 0.0240(10) Uani 1 1 d . . . C6 C -0.2388(5) -0.4712(4) -0.5554(2) 0.0357(12) Uani 1 1 d . . . H6 H -0.1990 -0.4674 -0.5978 0.043 Uiso 1 1 calc R . . C7 C -0.1948(4) -0.5255(4) -0.5112(2) 0.0313(11) Uani 1 1 d . . . H7 H -0.1184 -0.5667 -0.5178 0.038 Uiso 1 1 calc R . . C8 C -0.1086(4) -0.4398(4) -0.3810(2) 0.0312(11) Uani 1 1 d . . . H8 H -0.1321 -0.3928 -0.4105 0.037 Uiso 1 1 calc R . . C9 C -0.0314(5) -0.4281(4) -0.3439(3) 0.0405(13) Uani 1 1 d . . . H9 H 0.0105 -0.3721 -0.3434 0.049 Uiso 1 1 calc R . . C10 C -0.0237(5) -0.5138(4) -0.3056(3) 0.0420(13) Uani 1 1 d . . . H10 H 0.0243 -0.5252 -0.2750 0.050 Uiso 1 1 calc R . . C11 C -0.0963(4) -0.5762(4) -0.3202(2) 0.0343(12) Uani 1 1 d . . . H11 H -0.1096 -0.6386 -0.3009 0.041 Uiso 1 1 calc R . . C12 C -0.3420(5) -0.7475(4) -0.3625(2) 0.0330(11) Uani 1 1 d . . . H12 H -0.4205 -0.7264 -0.3381 0.040 Uiso 1 1 calc R . . C13 C -0.2949(5) -0.8433(4) -0.3808(2) 0.0400(13) Uani 1 1 d . . . H13 H -0.3343 -0.9011 -0.3715 0.048 Uiso 1 1 calc R . . C14 C -0.1759(5) -0.8411(4) -0.4166(2) 0.0388(13) Uani 1 1 d . . . H14 H -0.1218 -0.8976 -0.4354 0.047 Uiso 1 1 calc R . . C15 C -0.1528(5) -0.7464(4) -0.4194(2) 0.0334(11) Uani 1 1 d . . . H15 H -0.0798 -0.7242 -0.4407 0.040 Uiso 1 1 calc R . . C16 C -0.4319(5) -0.5494(4) -0.2511(2) 0.0405(13) Uani 1 1 d . . . C17 C -0.3928(6) -0.4846(5) -0.2098(3) 0.0533(15) Uani 1 1 d . . . H17A H -0.3896 -0.5189 -0.1702 0.080 Uiso 1 1 calc R . . H17B H -0.4501 -0.4225 -0.2020 0.080 Uiso 1 1 calc R . . H17C H -0.3122 -0.4687 -0.2290 0.080 Uiso 1 1 calc R . . C18 C -0.7685(5) -0.4278(4) -0.1843(2) 0.0359(12) Uani 1 1 d . . . C19 C -0.1193(4) 0.1068(4) -0.5978(2) 0.0328(11) Uani 1 1 d . . . H19 H -0.0940 0.1053 -0.5593 0.039 Uiso 1 1 calc R . . C20 C -0.2408(5) 0.1087(4) -0.5971(2) 0.0357(12) Uani 1 1 d . . . H20 H -0.2966 0.1091 -0.5584 0.043 Uiso 1 1 calc R . . C21 C -0.2829(4) 0.1099(4) -0.6521(2) 0.0328(11) Uani 1 1 d . . . H21 H -0.3665 0.1108 -0.6516 0.039 Uiso 1 1 calc R . . C22 C -0.1989(4) 0.1099(3) -0.7078(2) 0.0266(10) Uani 1 1 d . . . C23 C -0.0784(4) 0.1091(3) -0.7024(2) 0.0233(10) Uani 1 1 d . . . C24 C -0.1985(4) 0.1119(3) -0.7732(2) 0.0296(11) Uani 1 1 d . . . H24 H -0.2673 0.1121 -0.7912 0.036 Uiso 1 1 calc R . . C25 C -0.0831(4) 0.1136(3) -0.8050(2) 0.0283(10) Uani 1 1 d . . . H25 H -0.0583 0.1157 -0.8490 0.034 Uiso 1 1 calc R . . C26 C 0.1074(4) 0.3020(3) -0.8066(2) 0.0260(10) Uani 1 1 d . . . H26 H 0.0295 0.3187 -0.7807 0.031 Uiso 1 1 calc R . . C27 C 0.1767(4) 0.3679(4) -0.8380(2) 0.0317(11) Uani 1 1 d . . . H27 H 0.1556 0.4387 -0.8383 0.038 Uiso 1 1 calc R . . C28 C 0.2872(4) 0.3123(4) -0.8706(2) 0.0330(11) Uani 1 1 d . . . H28 H 0.3522 0.3395 -0.8968 0.040 Uiso 1 1 calc R . . C29 C 0.2827(4) 0.2144(4) -0.8578(2) 0.0279(10) Uani 1 1 d . . . H29 H 0.3451 0.1606 -0.8724 0.033 Uiso 1 1 calc R . . C30 C 0.2909(4) -0.0683(3) -0.7916(2) 0.0252(10) Uani 1 1 d . . . H30 H 0.3078 -0.0742 -0.7510 0.030 Uiso 1 1 calc R . . C31 C 0.3325(4) -0.1362(4) -0.8388(2) 0.0307(11) Uani 1 1 d . . . H31 H 0.3839 -0.1977 -0.8371 0.037 Uiso 1 1 calc R . . C32 C 0.2854(4) -0.0987(4) -0.8912(2) 0.0299(11) Uani 1 1 d . . . H32 H 0.3004 -0.1310 -0.9307 0.036 Uiso 1 1 calc R . . C33 C 0.2158(4) -0.0096(4) -0.8754(2) 0.0291(11) Uani 1 1 d . . . H33 H 0.1728 0.0313 -0.9015 0.035 Uiso 1 1 calc R . . C34 C 0.3357(4) 0.1290(4) -0.6965(2) 0.0274(10) Uani 1 1 d . . . C35 C 0.3603(5) 0.2355(4) -0.7033(3) 0.0409(13) Uani 1 1 d . . . H35A H 0.3189 0.2735 -0.6654 0.061 Uiso 1 1 calc R . . H35B H 0.3303 0.2656 -0.7391 0.061 Uiso 1 1 calc R . . H35C H 0.4476 0.2370 -0.7098 0.061 Uiso 1 1 calc R . . C36 C 0.3406(6) 0.1138(6) -0.5181(3) 0.0594(19) Uani 1 1 d . . . C37 C -0.0328(4) 0.1803(3) -0.2190(2) 0.0286(11) Uani 1 1 d . . . H37 H -0.1150 0.1940 -0.1979 0.034 Uiso 1 1 calc R . . C38 C -0.0065(5) 0.1657(3) -0.2834(2) 0.0303(11) Uani 1 1 d . . . H38 H -0.0711 0.1674 -0.3047 0.036 Uiso 1 1 calc R . . C39 C 0.1123(5) 0.1488(4) -0.3172(2) 0.0338(12) Uani 1 1 d . . . H39 H 0.1303 0.1411 -0.3612 0.041 Uiso 1 1 calc R . . C40 C 0.2041(4) 0.1437(3) -0.2835(2) 0.0287(11) Uani 1 1 d . . . C41 C 0.1677(4) 0.1562(3) -0.2192(2) 0.0237(10) Uani 1 1 d . . . C42 C 0.3341(5) 0.1228(4) -0.2961(2) 0.0347(12) Uani 1 1 d . . . H42 H 0.3857 0.1114 -0.3361 0.042 Uiso 1 1 calc R . . C43 C 0.3701(4) 0.1224(4) -0.2413(2) 0.0321(11) Uani 1 1 d . . . H43 H 0.4517 0.1097 -0.2366 0.039 Uiso 1 1 calc R . . C44 C 0.3777(4) 0.2856(3) -0.1169(2) 0.0292(11) Uani 1 1 d . . . H44 H 0.3528 0.3194 -0.1514 0.035 Uiso 1 1 calc R . . C45 C 0.4384(5) 0.3225(4) -0.0783(3) 0.0393(13) Uani 1 1 d . . . H45 H 0.4657 0.3863 -0.0815 0.047 Uiso 1 1 calc R . . C46 C 0.4547(4) 0.2501(4) -0.0321(2) 0.0377(13) Uani 1 1 d . . . H46 H 0.4947 0.2572 0.0011 0.045 Uiso 1 1 calc R . . C47 C 0.4042(4) 0.1698(4) -0.0430(2) 0.0317(11) Uani 1 1 d . . . H47 H 0.4006 0.1108 -0.0185 0.038 Uiso 1 1 calc R . . C48 C 0.4007(4) -0.0455(4) -0.1195(2) 0.0324(11) Uani 1 1 d . . . H48 H 0.4719 -0.0215 -0.1417 0.039 Uiso 1 1 calc R . . C49 C 0.3903(4) -0.1422(4) -0.1043(2) 0.0334(11) Uani 1 1 d . . . H49 H 0.4525 -0.1979 -0.1137 0.040 Uiso 1 1 calc R . . C50 C 0.2686(4) -0.1453(4) -0.0715(2) 0.0312(11) Uani 1 1 d . . . H50 H 0.2354 -0.2035 -0.0551 0.037 Uiso 1 1 calc R . . C51 C 0.2092(4) -0.0509(3) -0.0679(2) 0.0257(10) Uani 1 1 d . . . H51 H 0.1267 -0.0311 -0.0486 0.031 Uiso 1 1 calc R . . C52 C 0.0661(4) 0.2074(4) 0.0022(2) 0.0264(10) Uani 1 1 d . . . C53 C 0.0932(5) 0.3102(4) 0.0165(3) 0.0409(13) Uani 1 1 d . . . H53A H 0.0634 0.3253 0.0610 0.061 Uiso 1 1 calc R . . H53B H 0.0530 0.3607 -0.0079 0.061 Uiso 1 1 calc R . . H53C H 0.1809 0.3112 0.0057 0.061 Uiso 1 1 calc R . . C54 C -0.2580(5) 0.4256(4) -0.0135(2) 0.0370(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0233(2) 0.0352(2) 0.0229(2) 0.00539(16) -0.00112(15) 0.00597(16) Pd2 0.0253(2) 0.0269(2) 0.0155(2) -0.00198(14) -0.00564(14) 0.00046(15) Pd3 0.0175(2) 0.0245(2) 0.0155(2) 0.00199(14) -0.00484(14) -0.00106(14) S1 0.0273(7) 0.0520(8) 0.0304(7) 0.0028(6) -0.0015(5) 0.0016(6) S2 0.0746(10) 0.0304(7) 0.0212(6) 0.0001(5) -0.0179(6) -0.0005(6) S3 0.0306(6) 0.0257(6) 0.0250(6) 0.0016(5) -0.0066(5) 0.0041(5) P1 0.0214(6) 0.0243(6) 0.0241(6) 0.0028(5) -0.0036(5) 0.0000(5) P2 0.0204(6) 0.0224(6) 0.0159(6) -0.0015(5) -0.0032(4) 0.0001(5) P3 0.0186(6) 0.0240(6) 0.0192(6) 0.0019(5) -0.0044(5) -0.0019(5) F1 0.0459(19) 0.057(2) 0.0406(18) 0.0159(15) -0.0062(15) 0.0118(16) F2 0.135(4) 0.042(2) 0.0383(19) -0.0084(16) -0.021(2) 0.021(2) F3 0.047(2) 0.104(3) 0.068(3) 0.038(2) -0.0007(18) -0.020(2) F4 0.115(4) 0.149(4) 0.053(2) 0.024(3) -0.048(3) -0.075(3) F5 0.050(2) 0.087(3) 0.107(4) 0.007(3) -0.019(2) -0.001(2) F6 0.111(4) 0.188(5) 0.066(3) 0.048(3) -0.033(3) -0.116(4) F7 0.0433(19) 0.0474(19) 0.062(2) 0.0021(16) 0.0167(16) -0.0018(15) F8 0.099(3) 0.0261(17) 0.062(2) 0.0013(16) 0.009(2) 0.0215(18) F9 0.080(3) 0.081(3) 0.046(2) -0.0288(19) -0.0179(19) -0.006(2) O1 0.062(3) 0.056(3) 0.041(2) 0.009(2) -0.004(2) -0.002(2) O2 0.0308(19) 0.046(2) 0.041(2) 0.0029(17) -0.0054(16) -0.0050(16) O3 0.0223(17) 0.046(2) 0.0349(19) 0.0056(16) -0.0091(14) 0.0023(15) O4 0.061(3) 0.038(2) 0.069(3) -0.018(2) -0.014(2) -0.0084(19) O5 0.031(2) 0.038(2) 0.061(3) -0.0041(18) -0.0151(18) 0.0028(17) O6 0.058(2) 0.054(2) 0.0284(19) -0.0011(17) -0.0135(17) -0.0084(19) O7 0.065(3) 0.093(4) 0.037(2) 0.012(2) -0.002(2) 0.013(3) O8 0.273(10) 0.036(3) 0.102(5) -0.004(3) -0.086(6) 0.012(4) O9 0.035(2) 0.060(2) 0.0220(18) 0.0155(18) -0.0059(15) -0.0071(17) O10 0.064(3) 0.054(2) 0.045(2) -0.0098(19) -0.033(2) 0.020(2) O11 0.0211(16) 0.0222(16) 0.0315(17) 0.0032(13) -0.0054(13) 0.0001(13) O12 0.043(2) 0.036(2) 0.065(3) 0.0199(19) 0.0060(19) -0.0020(17) N1 0.028(2) 0.0212(19) 0.028(2) -0.0009(16) -0.0057(17) -0.0016(16) N2 0.022(2) 0.028(2) 0.024(2) 0.0042(16) -0.0033(16) -0.0008(16) N3 0.023(2) 0.027(2) 0.029(2) 0.0028(17) -0.0036(17) -0.0019(16) N4 0.030(2) 0.021(2) 0.033(2) 0.0032(17) -0.0102(18) 0.0012(17) N5 0.029(2) 0.0238(19) 0.020(2) -0.0009(16) -0.0017(17) 0.0010(16) N6 0.025(2) 0.029(2) 0.0172(19) 0.0013(16) -0.0042(16) -0.0037(16) N7 0.0227(19) 0.024(2) 0.0167(18) 0.0021(15) -0.0031(15) 0.0022(16) N8 0.027(2) 0.0217(19) 0.0180(19) -0.0026(15) -0.0060(16) 0.0036(16) N9 0.021(2) 0.027(2) 0.0187(19) 0.0019(16) -0.0026(16) -0.0024(16) N10 0.026(2) 0.027(2) 0.020(2) 0.0008(16) -0.0066(16) 0.0008(16) N11 0.0172(19) 0.026(2) 0.023(2) 0.0007(16) -0.0030(15) -0.0021(15) N12 0.021(2) 0.026(2) 0.034(2) 0.0040(17) -0.0085(17) -0.0032(16) C1 0.030(3) 0.024(2) 0.032(3) -0.001(2) -0.009(2) 0.001(2) C2 0.040(3) 0.026(2) 0.038(3) 0.001(2) -0.022(2) -0.002(2) C3 0.044(3) 0.028(3) 0.029(3) 0.004(2) -0.014(2) -0.006(2) C4 0.035(3) 0.029(2) 0.027(3) 0.000(2) -0.008(2) -0.009(2) C5 0.028(3) 0.023(2) 0.022(2) 0.0033(19) -0.007(2) -0.005(2) C6 0.037(3) 0.042(3) 0.025(3) 0.001(2) 0.001(2) -0.008(2) C7 0.027(3) 0.039(3) 0.024(3) 0.000(2) 0.001(2) -0.001(2) C8 0.030(3) 0.030(3) 0.032(3) 0.000(2) 0.001(2) -0.005(2) C9 0.029(3) 0.049(3) 0.042(3) -0.016(3) 0.000(2) -0.010(2) C10 0.034(3) 0.059(4) 0.035(3) -0.006(3) -0.016(2) -0.001(3) C11 0.033(3) 0.039(3) 0.032(3) 0.001(2) -0.014(2) 0.004(2) C12 0.035(3) 0.034(3) 0.036(3) 0.012(2) -0.018(2) -0.010(2) C13 0.065(4) 0.025(3) 0.039(3) 0.005(2) -0.029(3) -0.011(3) C14 0.056(4) 0.030(3) 0.032(3) -0.001(2) -0.020(3) 0.007(2) C15 0.034(3) 0.033(3) 0.032(3) 0.000(2) -0.008(2) 0.002(2) C16 0.031(3) 0.047(3) 0.034(3) 0.012(3) 0.005(2) 0.006(2) C17 0.054(4) 0.062(4) 0.049(4) 0.010(3) -0.020(3) -0.009(3) C18 0.030(3) 0.039(3) 0.033(3) 0.007(2) 0.000(2) 0.003(2) C19 0.036(3) 0.033(3) 0.024(3) 0.002(2) 0.003(2) -0.002(2) C20 0.036(3) 0.036(3) 0.029(3) 0.005(2) 0.007(2) -0.001(2) C21 0.027(3) 0.029(3) 0.038(3) 0.001(2) 0.003(2) -0.003(2) C22 0.026(3) 0.019(2) 0.033(3) 0.0016(19) -0.003(2) -0.0028(19) C23 0.028(2) 0.017(2) 0.022(2) 0.0005(18) 0.0010(19) 0.0004(18) C24 0.024(3) 0.029(2) 0.038(3) 0.002(2) -0.010(2) -0.005(2) C25 0.030(3) 0.032(3) 0.024(2) 0.000(2) -0.012(2) -0.001(2) C26 0.025(2) 0.026(2) 0.025(2) 0.000(2) -0.005(2) 0.002(2) C27 0.034(3) 0.024(2) 0.034(3) 0.003(2) -0.005(2) 0.003(2) C28 0.031(3) 0.037(3) 0.028(3) 0.006(2) 0.001(2) -0.006(2) C29 0.024(2) 0.033(3) 0.022(2) 0.002(2) 0.0006(19) 0.002(2) C30 0.020(2) 0.026(2) 0.030(3) -0.001(2) -0.0080(19) -0.0008(19) C31 0.019(2) 0.028(2) 0.043(3) -0.012(2) -0.003(2) 0.0021(19) C32 0.027(3) 0.035(3) 0.027(3) -0.011(2) -0.004(2) -0.004(2) C33 0.032(3) 0.035(3) 0.019(2) -0.004(2) -0.006(2) -0.002(2) C34 0.031(3) 0.030(3) 0.023(2) -0.007(2) -0.012(2) -0.001(2) C35 0.042(3) 0.039(3) 0.044(3) 0.002(2) -0.013(3) -0.008(2) C36 0.066(4) 0.083(5) 0.046(4) 0.000(3) -0.021(3) -0.050(4) C37 0.033(3) 0.028(2) 0.028(3) -0.001(2) -0.011(2) -0.004(2) C38 0.040(3) 0.029(2) 0.028(3) 0.001(2) -0.020(2) -0.003(2) C39 0.049(3) 0.034(3) 0.018(2) 0.003(2) -0.008(2) -0.003(2) C40 0.040(3) 0.025(2) 0.020(2) 0.0010(19) -0.002(2) -0.005(2) C41 0.031(3) 0.021(2) 0.020(2) 0.0016(18) -0.007(2) -0.0026(19) C42 0.039(3) 0.036(3) 0.023(3) -0.003(2) 0.004(2) 0.000(2) C43 0.026(3) 0.038(3) 0.027(3) -0.001(2) 0.002(2) 0.002(2) C44 0.027(3) 0.024(2) 0.033(3) 0.001(2) 0.001(2) -0.002(2) C45 0.030(3) 0.035(3) 0.050(3) -0.019(3) 0.001(2) -0.006(2) C46 0.025(3) 0.056(3) 0.034(3) -0.017(3) -0.007(2) -0.008(2) C47 0.026(3) 0.045(3) 0.024(3) 0.000(2) -0.005(2) -0.004(2) C48 0.017(2) 0.035(3) 0.044(3) 0.007(2) -0.005(2) -0.002(2) C49 0.027(3) 0.029(3) 0.045(3) 0.005(2) -0.014(2) 0.004(2) C50 0.037(3) 0.026(3) 0.030(3) 0.008(2) -0.006(2) -0.006(2) C51 0.023(2) 0.032(3) 0.023(2) 0.007(2) -0.0041(19) -0.010(2) C52 0.012(2) 0.041(3) 0.023(2) 0.000(2) -0.0017(18) 0.000(2) C53 0.037(3) 0.054(3) 0.037(3) -0.014(3) -0.016(2) -0.006(3) C54 0.044(3) 0.030(3) 0.033(3) -0.002(2) -0.001(2) 0.000(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 Pd1 C16 1.989(5) . ? Pd1 O2 2.151(4) . ? Pd1 P1 2.1796(12) . ? Pd1 N1 2.190(4) . ? Pd2 C34 1.993(5) . ? Pd2 O6 2.119(4) . ? Pd2 P2 2.1851(11) . ? Pd2 N5 2.196(4) . ? Pd3 C52 1.990(5) . ? Pd3 O11 2.143(3) . ? Pd3 P3 2.1813(11) . ? Pd3 N9 2.205(4) . ? S1 O3 1.437(3) . ? S1 O4 1.454(4) . ? S1 O2 1.457(4) . ? S1 C18 1.825(5) . ? S2 O8 1.387(5) . ? S2 O7 1.436(5) . ? S2 O6 1.462(4) . ? S2 C36 1.858(7) . ? S3 O10 1.420(4) . ? S3 O12 1.423(4) . ? S3 O11 1.471(3) . ? S3 C54 1.826(5) . ? P1 N4 1.681(4) . ? P1 N3 1.683(4) . ? P1 N2 1.694(4) . ? P2 N8 1.670(4) . ? P2 N7 1.681(4) . ? P2 N6 1.684(4) . ? P3 N12 1.676(4) . ? P3 N11 1.683(4) . ? P3 N10 1.697(4) . ? F1 C18 1.319(6) . ? F2 C18 1.308(6) . ? F3 C18 1.312(6) . ? F4 C36 1.295(7) . ? F5 C36 1.307(8) . ? F6 C36 1.344(7) . ? F7 C54 1.325(6) . ? F8 C54 1.319(6) . ? F9 C54 1.311(6) . ? O1 C16 1.235(7) . ? O5 C34 1.207(6) . ? O9 C52 1.192(6) . ? N1 C5 1.335(6) . ? N1 C1 1.349(6) . ? N2 C5 1.392(6) . ? N2 C7 1.413(6) . ? N3 C11 1.397(6) . ? N3 C8 1.410(6) . ? N4 C12 1.399(6) . ? N4 C15 1.406(6) . ? N5 C23 1.318(6) . ? N5 C19 1.356(6) . ? N6 C23 1.405(6) . ? N6 C25 1.418(6) . ? N7 C29 1.400(6) . ? N7 C26 1.397(6) . ? N8 C30 1.404(6) . ? N8 C33 1.408(6) . ? N9 C41 1.341(6) . ? N9 C37 1.342(6) . ? N10 C41 1.390(6) . ? N10 C43 1.407(6) . ? N11 C44 1.400(6) . ? N11 C47 1.409(6) . ? N12 C48 1.389(6) . ? N12 C51 1.400(6) . ? C1 C2 1.385(7) . ? C2 C3 1.382(7) . ? C3 C4 1.388(7) . ? C4 C5 1.400(7) . ? C4 C6 1.440(7) . ? C6 C7 1.341(7) . ? C8 C9 1.346(7) . ? C9 C10 1.417(8) . ? C10 C11 1.348(8) . ? C12 C13 1.360(7) . ? C13 C14 1.423(8) . ? C14 C15 1.336(7) . ? C16 C17 1.448(8) . ? C19 C20 1.380(7) . ? C20 C21 1.390(7) . ? C21 C22 1.385(7) . ? C22 C23 1.403(6) . ? C22 C24 1.435(7) . ? C24 C25 1.358(7) . ? C26 C27 1.353(7) . ? C27 C28 1.427(7) . ? C28 C29 1.349(7) . ? C30 C31 1.357(7) . ? C31 C32 1.424(7) . ? C32 C33 1.350(7) . ? C34 C35 1.498(7) . ? C37 C38 1.395(7) . ? C38 C39 1.392(7) . ? C39 C40 1.398(7) . ? C40 C41 1.392(6) . ? C40 C42 1.439(7) . ? C42 C43 1.350(7) . ? C44 C45 1.344(7) . ? C45 C46 1.415(8) . ? C46 C47 1.344(7) . ? C48 C49 1.353(7) . ? C49 C50 1.431(7) . ? C50 C51 1.349(7) . ? C52 C53 1.515(7) . ? 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 C16 Pd1 O2 90.60(18) . . ? C16 Pd1 P1 91.96(15) . . ? O2 Pd1 P1 169.50(10) . . ? C16 Pd1 N1 177.35(18) . . ? O2 Pd1 N1 92.02(14) . . ? P1 Pd1 N1 85.39(10) . . ? C34 Pd2 O6 90.95(17) . . ? C34 Pd2 P2 91.76(13) . . ? O6 Pd2 P2 171.44(11) . . ? C34 Pd2 N5 174.90(17) . . ? O6 Pd2 N5 93.17(14) . . ? P2 Pd2 N5 84.59(10) . . ? C52 Pd3 O11 86.60(15) . . ? C52 Pd3 P3 91.71(13) . . ? O11 Pd3 P3 175.93(8) . . ? C52 Pd3 N9 175.49(15) . . ? O11 Pd3 N9 97.39(12) . . ? P3 Pd3 N9 84.17(10) . . ? O3 S1 O4 117.4(2) . . ? O3 S1 O2 113.4(2) . . ? O4 S1 O2 112.1(2) . . ? O3 S1 C18 104.1(2) . . ? O4 S1 C18 104.5(3) . . ? O2 S1 C18 103.4(2) . . ? O8 S2 O7 120.0(4) . . ? O8 S2 O6 114.9(3) . . ? O7 S2 O6 109.5(3) . . ? O8 S2 C36 106.1(5) . . ? O7 S2 C36 103.0(3) . . ? O6 S2 C36 100.5(3) . . ? O10 S3 O12 118.1(3) . . ? O10 S3 O11 113.6(2) . . ? O12 S3 O11 112.7(2) . . ? O10 S3 C54 104.0(2) . . ? O12 S3 C54 104.7(2) . . ? O11 S3 C54 101.5(2) . . ? N4 P1 N3 100.36(19) . . ? N4 P1 N2 109.00(19) . . ? N3 P1 N2 101.02(19) . . ? N4 P1 Pd1 119.99(14) . . ? N3 P1 Pd1 123.10(14) . . ? N2 P1 Pd1 101.42(13) . . ? N8 P2 N7 101.16(18) . . ? N8 P2 N6 109.03(19) . . ? N7 P2 N6 101.30(18) . . ? N8 P2 Pd2 118.04(13) . . ? N7 P2 Pd2 123.73(13) . . ? N6 P2 Pd2 101.88(13) . . ? N12 P3 N11 100.90(18) . . ? N12 P3 N10 107.84(19) . . ? N11 P3 N10 101.68(18) . . ? N12 P3 Pd3 118.65(14) . . ? N11 P3 Pd3 124.28(13) . . ? N10 P3 Pd3 101.49(13) . . ? S1 O2 Pd1 119.8(2) . . ? S2 O6 Pd2 140.5(2) . . ? S3 O11 Pd3 119.14(18) . . ? C5 N1 C1 114.7(4) . . ? C5 N1 Pd1 111.1(3) . . ? C1 N1 Pd1 134.1(3) . . ? C5 N2 C7 106.2(4) . . ? C5 N2 P1 119.0(3) . . ? C7 N2 P1 134.8(3) . . ? C11 N3 C8 106.8(4) . . ? C11 N3 P1 123.4(3) . . ? C8 N3 P1 122.9(3) . . ? C12 N4 C15 107.3(4) . . ? C12 N4 P1 123.7(3) . . ? C15 N4 P1 128.4(3) . . ? C23 N5 C19 114.1(4) . . ? C23 N5 Pd2 112.0(3) . . ? C19 N5 Pd2 133.7(3) . . ? C23 N6 C25 106.7(4) . . ? C23 N6 P2 118.8(3) . . ? C25 N6 P2 134.5(3) . . ? C29 N7 C26 107.6(4) . . ? C29 N7 P2 124.2(3) . . ? C26 N7 P2 121.8(3) . . ? C30 N8 C33 107.7(4) . . ? C30 N8 P2 124.0(3) . . ? C33 N8 P2 128.3(3) . . ? C41 N9 C37 115.0(4) . . ? C41 N9 Pd3 110.9(3) . . ? C37 N9 Pd3 134.1(3) . . ? C41 N10 C43 106.4(4) . . ? C41 N10 P3 117.6(3) . . ? C43 N10 P3 134.5(3) . . ? C44 N11 C47 107.4(4) . . ? C44 N11 P3 123.2(3) . . ? C47 N11 P3 123.6(3) . . ? C48 N12 C51 107.6(4) . . ? C48 N12 P3 128.6(3) . . ? C51 N12 P3 122.6(3) . . ? N1 C1 C2 122.5(4) . . ? C1 C2 C3 121.2(5) . . ? C4 C3 C2 118.1(4) . . ? C3 C4 C5 116.0(4) . . ? C3 C4 C6 138.2(5) . . ? C5 C4 C6 105.8(4) . . ? N1 C5 N2 123.0(4) . . ? N1 C5 C4 127.5(4) . . ? N2 C5 C4 109.5(4) . . ? C7 C6 C4 108.2(4) . . ? C6 C7 N2 110.3(4) . . ? C9 C8 N3 108.3(5) . . ? C8 C9 C10 108.1(5) . . ? C11 C10 C9 108.1(5) . . ? C10 C11 N3 108.6(5) . . ? C13 C12 N4 108.3(5) . . ? C12 C13 C14 107.4(5) . . ? C15 C14 C13 108.7(5) . . ? C14 C15 N4 108.4(5) . . ? O1 C16 C17 125.8(5) . . ? O1 C16 Pd1 120.2(4) . . ? C17 C16 Pd1 113.7(4) . . ? F2 C18 F3 107.8(5) . . ? F2 C18 F1 107.8(4) . . ? F3 C18 F1 108.2(4) . . ? F2 C18 S1 111.8(4) . . ? F3 C18 S1 109.6(4) . . ? F1 C18 S1 111.4(3) . . ? N5 C19 C20 122.7(5) . . ? C19 C20 C21 121.2(4) . . ? C22 C21 C20 117.8(5) . . ? C21 C22 C23 115.7(4) . . ? C21 C22 C24 137.7(5) . . ? C23 C22 C24 106.6(4) . . ? N5 C23 C22 128.5(4) . . ? N5 C23 N6 122.6(4) . . ? C22 C23 N6 108.9(4) . . ? C25 C24 C22 108.4(4) . . ? C24 C25 N6 109.5(4) . . ? C27 C26 N7 108.2(4) . . ? C26 C27 C28 108.1(4) . . ? C29 C28 C27 107.7(4) . . ? C28 C29 N7 108.5(4) . . ? C31 C30 N8 108.0(4) . . ? C30 C31 C32 107.9(4) . . ? C33 C32 C31 108.6(4) . . ? C32 C33 N8 107.8(4) . . ? O5 C34 C35 124.1(4) . . ? O5 C34 Pd2 121.1(4) . . ? C35 C34 Pd2 114.5(3) . . ? F4 C36 F5 109.0(6) . . ? F4 C36 F6 107.1(5) . . ? F5 C36 F6 109.9(6) . . ? F4 C36 S2 111.2(5) . . ? F5 C36 S2 111.4(4) . . ? F6 C36 S2 108.1(5) . . ? N9 C37 C38 122.4(4) . . ? C39 C38 C37 121.4(4) . . ? C38 C39 C40 117.1(4) . . ? C41 C40 C39 116.7(4) . . ? C41 C40 C42 105.9(4) . . ? C39 C40 C42 137.3(4) . . ? N9 C41 N10 122.9(4) . . ? N9 C41 C40 127.3(4) . . ? N10 C41 C40 109.7(4) . . ? C43 C42 C40 108.1(4) . . ? C42 C43 N10 109.9(4) . . ? C45 C44 N11 108.1(4) . . ? C44 C45 C46 108.3(4) . . ? C47 C46 C45 108.6(4) . . ? C46 C47 N11 107.6(5) . . ? C49 C48 N12 108.7(4) . . ? C48 C49 C50 107.5(4) . . ? C51 C50 C49 107.9(4) . . ? C50 C51 N12 108.3(4) . . ? O9 C52 C53 125.7(4) . . ? O9 C52 Pd3 121.4(4) . . ? C53 C52 Pd3 112.9(4) . . ? F9 C54 F8 108.4(4) . . ? F9 C54 F7 107.8(4) . . ? F8 C54 F7 107.7(4) . . ? F9 C54 S3 111.1(4) . . ? F8 C54 S3 110.0(4) . . ? F7 C54 S3 111.8(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 23.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.367 _refine_diff_density_min -1.163 _refine_diff_density_rms 0.108 #===END data_compound8a_k01adb2 _database_code_CSD 217638 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H22 F3 N2 O4 P Pd S' _chemical_formula_weight 628.87 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' F F 0.0171 0.0103 '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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.29100(10) _cell_length_b 11.8690(2) _cell_length_c 13.8810(3) _cell_angle_alpha 71.4250(9) _cell_angle_beta 77.4640(8) _cell_angle_gamma 89.6770(13) _cell_volume 1260.97(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 18 _exptl_crystal_description needle _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.656 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 0.938 _exptl_absorpt_correction_type multiscan _exptl_absorpt_process_details 'Sortav Blessing (1995) ' _exptl_absorpt_correction_T_min 0.8721 _exptl_absorpt_correction_T_max 0.9546 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20472 _diffrn_reflns_av_R_equivalents 0.0529 _diffrn_reflns_av_sigmaI/netI 0.0413 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 24.98 _reflns_number_total 4408 _reflns_number_gt 3794 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'Denzo and Scalepack (otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0857P)^2^+1.6646P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0028(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4408 _refine_ls_number_parameters 327 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0434 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.1052 _refine_ls_wR_factor_gt 0.0969 _refine_ls_goodness_of_fit_ref 0.801 _refine_ls_restrained_S_all 0.801 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.04611(3) 0.50151(2) 0.15028(2) 0.03339(13) Uani 1 1 d . . . S1 S 0.30719(15) 0.81816(10) 0.25740(9) 0.0566(3) Uani 1 1 d . . . P1 P 0.06811(11) 0.31209(8) 0.22506(8) 0.0388(2) Uani 1 1 d . . . F1 F 0.3813(5) 0.7703(8) 0.4364(3) 0.207(4) Uani 1 1 d . . . F2 F 0.1682(4) 0.6692(4) 0.4385(3) 0.1146(14) Uani 1 1 d . . . F3 F 0.4104(5) 0.6276(5) 0.3709(4) 0.160(2) Uani 1 1 d . . . O1 O 0.0077(3) 0.6825(2) 0.0848(2) 0.0397(6) Uani 1 1 d . . . O2 O 0.2397(4) 0.7475(4) 0.2099(3) 0.0768(10) Uani 1 1 d . . . O3 O 0.4767(5) 0.8582(4) 0.2096(3) 0.1020(16) Uani 1 1 d . . . O4 O 0.1994(7) 0.9046(4) 0.2826(4) 0.125(2) Uani 1 1 d . . . N1 N 0.2095(4) 0.2806(3) 0.1285(3) 0.0447(8) Uani 1 1 d . . . N2 N 0.2282(3) 0.4840(3) 0.0218(2) 0.0366(7) Uani 1 1 d . . . C1 C 0.2916(5) 0.1792(4) 0.1169(4) 0.0577(11) Uani 1 1 d . . . H1 H 0.2721 0.1018 0.1673 0.069 Uiso 1 1 calc R . . C2 C 0.4002(5) 0.2078(4) 0.0251(4) 0.0558(11) Uani 1 1 d . . . H2 H 0.4695 0.1547 -0.0003 0.067 Uiso 1 1 calc R . . C3 C 0.3948(4) 0.3320(4) -0.0287(3) 0.0465(10) Uani 1 1 d . . . C4 C 0.4765(4) 0.4169(4) -0.1219(3) 0.0491(10) Uani 1 1 d . . . H4 H 0.5596 0.3958 -0.1709 0.059 Uiso 1 1 calc R . . C5 C 0.4318(5) 0.5330(4) -0.1402(3) 0.0473(9) Uani 1 1 d . . . H5 H 0.4858 0.5930 -0.2027 0.057 Uiso 1 1 calc R . . C6 C 0.3097(4) 0.5634(4) -0.0689(3) 0.0420(9) Uani 1 1 d . . . H6 H 0.2823 0.6441 -0.0848 0.050 Uiso 1 1 calc R . . C7 C 0.2747(4) 0.3731(3) 0.0379(3) 0.0380(8) Uani 1 1 d . . . C8 C -0.1126(4) 0.2131(3) 0.2514(3) 0.0441(9) Uani 1 1 d . . . C9 C -0.1406(5) 0.1584(4) 0.1809(4) 0.0537(11) Uani 1 1 d . . . H9 H -0.0584 0.1654 0.1194 0.064 Uiso 1 1 calc R . . C10 C -0.2896(5) 0.0939(4) 0.2014(5) 0.0659(14) Uani 1 1 d . . . H10 H -0.3084 0.0549 0.1544 0.079 Uiso 1 1 calc R . . C11 C -0.4108(5) 0.0853(4) 0.2888(5) 0.0640(14) Uani 1 1 d . . . H11 H -0.5128 0.0412 0.3013 0.077 Uiso 1 1 calc R . . C12 C -0.3856(5) 0.1403(4) 0.3587(4) 0.0595(12) Uani 1 1 d . . . H12 H -0.4697 0.1344 0.4190 0.071 Uiso 1 1 calc R . . C13 C -0.2357(5) 0.2044(4) 0.3398(4) 0.0516(10) Uani 1 1 d . . . H13 H -0.2173 0.2425 0.3876 0.062 Uiso 1 1 calc R . . C14 C 0.1445(4) 0.2647(3) 0.3435(3) 0.0448(9) Uani 1 1 d . . . C15 C 0.2035(4) 0.3516(4) 0.3779(3) 0.0449(9) Uani 1 1 d . . . H15 H 0.2088 0.4334 0.3374 0.054 Uiso 1 1 calc R . . C16 C 0.2546(5) 0.3183(4) 0.4719(3) 0.0555(11) Uani 1 1 d . . . H16 H 0.2962 0.3769 0.4952 0.067 Uiso 1 1 calc R . . C17 C 0.2441(5) 0.1994(5) 0.5306(4) 0.0710(15) Uani 1 1 d . . . H17 H 0.2771 0.1764 0.5952 0.085 Uiso 1 1 calc R . . C18 C 0.1864(5) 0.1140(5) 0.4969(4) 0.0768(17) Uani 1 1 d . . . H18 H 0.1804 0.0324 0.5383 0.092 Uiso 1 1 calc R . . C19 C 0.1366(5) 0.1453(4) 0.4026(4) 0.0624(13) Uani 1 1 d . . . H19 H 0.0978 0.0858 0.3793 0.075 Uiso 1 1 calc R . . C20 C -0.1259(4) 0.5157(3) 0.2737(3) 0.0408(8) Uani 1 1 d . . . H20A H -0.2347 0.4795 0.2762 0.049 Uiso 1 1 calc R . . H20B H -0.0926 0.4741 0.3397 0.049 Uiso 1 1 calc R . . C21 C -0.1370(5) 0.6478(4) 0.2592(3) 0.0453(9) Uani 1 1 d . . . H21A H -0.2543 0.6634 0.2817 0.054 Uiso 1 1 calc R . . H21B H -0.0742 0.6690 0.3048 0.054 Uiso 1 1 calc R . . C22 C -0.0717(4) 0.7250(3) 0.1500(3) 0.0410(9) Uani 1 1 d . . . C23 C -0.0998(6) 0.8545(4) 0.1192(4) 0.0602(12) Uani 1 1 d . . . H23A H -0.0463 0.8930 0.0455 0.090 Uiso 1 1 calc R . . H23B H -0.0526 0.8908 0.1621 0.090 Uiso 1 1 calc R . . H23C H -0.2190 0.8648 0.1298 0.090 Uiso 1 1 calc R . . C24 C 0.3171(6) 0.7175(7) 0.3820(4) 0.092(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02731(17) 0.03209(19) 0.04331(19) -0.01344(13) -0.01146(12) 0.00170(11) S1 0.0657(7) 0.0457(6) 0.0501(6) -0.0195(5) 0.0104(5) -0.0088(5) P1 0.0292(5) 0.0336(5) 0.0533(6) -0.0114(4) -0.0129(4) 0.0030(4) F1 0.082(3) 0.485(11) 0.070(2) -0.118(5) -0.007(2) -0.060(4) F2 0.0466(16) 0.148(3) 0.081(2) 0.042(2) 0.0059(15) -0.0072(18) F3 0.076(2) 0.197(5) 0.123(3) 0.052(3) -0.012(2) 0.053(3) O1 0.0416(14) 0.0323(13) 0.0496(15) -0.0175(12) -0.0131(12) 0.0022(11) O2 0.0515(18) 0.114(3) 0.092(3) -0.064(2) -0.0277(18) 0.0187(18) O3 0.097(3) 0.112(3) 0.085(3) -0.062(3) 0.052(2) -0.065(3) O4 0.171(5) 0.054(2) 0.104(3) -0.022(2) 0.057(3) 0.014(3) N1 0.0351(16) 0.0363(18) 0.065(2) -0.0176(16) -0.0143(15) 0.0083(13) N2 0.0275(14) 0.0388(17) 0.0496(18) -0.0174(14) -0.0170(13) 0.0039(12) C1 0.046(2) 0.041(2) 0.088(3) -0.018(2) -0.023(2) 0.0151(18) C2 0.040(2) 0.055(3) 0.080(3) -0.031(2) -0.014(2) 0.0157(19) C3 0.0304(18) 0.054(3) 0.068(3) -0.032(2) -0.0196(18) 0.0086(17) C4 0.0292(19) 0.064(3) 0.063(3) -0.035(2) -0.0085(18) 0.0017(18) C5 0.0330(19) 0.060(3) 0.050(2) -0.022(2) -0.0073(17) -0.0027(17) C6 0.0335(18) 0.046(2) 0.051(2) -0.0188(18) -0.0138(17) 0.0007(16) C7 0.0280(17) 0.039(2) 0.053(2) -0.0175(17) -0.0177(16) 0.0040(15) C8 0.0340(19) 0.0277(19) 0.071(3) -0.0126(18) -0.0177(18) 0.0055(15) C9 0.041(2) 0.038(2) 0.092(3) -0.034(2) -0.018(2) 0.0122(17) C10 0.046(2) 0.045(3) 0.128(5) -0.050(3) -0.032(3) 0.0116(19) C11 0.037(2) 0.035(2) 0.128(4) -0.031(3) -0.028(3) 0.0068(17) C12 0.033(2) 0.047(3) 0.094(4) -0.018(2) -0.012(2) 0.0020(18) C13 0.035(2) 0.047(2) 0.074(3) -0.020(2) -0.0149(19) 0.0000(17) C14 0.0253(17) 0.044(2) 0.054(2) -0.0002(18) -0.0097(16) 0.0028(15) C15 0.0276(18) 0.054(2) 0.044(2) -0.0048(18) -0.0057(15) -0.0023(16) C16 0.038(2) 0.075(3) 0.045(2) -0.008(2) -0.0087(18) 0.005(2) C17 0.032(2) 0.096(4) 0.058(3) 0.011(3) -0.0097(19) 0.003(2) C18 0.034(2) 0.068(3) 0.091(4) 0.028(3) -0.017(2) 0.000(2) C19 0.035(2) 0.049(3) 0.087(3) 0.006(2) -0.023(2) -0.0004(18) C20 0.0315(18) 0.039(2) 0.052(2) -0.0149(17) -0.0090(16) 0.0015(15) C21 0.037(2) 0.046(2) 0.055(2) -0.0245(19) -0.0036(17) -0.0036(16) C22 0.0356(19) 0.033(2) 0.061(2) -0.0220(18) -0.0125(17) 0.0018(15) C23 0.069(3) 0.035(2) 0.076(3) -0.023(2) -0.009(2) 0.009(2) C24 0.036(3) 0.155(6) 0.059(3) -0.002(3) -0.007(2) -0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C20 2.029(4) . ? Pd1 O1 2.102(2) . ? Pd1 N2 2.137(3) . ? Pd1 P1 2.1808(10) . ? S1 O2 1.403(3) . ? S1 O3 1.429(4) . ? S1 O4 1.435(4) . ? S1 C24 1.780(6) . ? P1 N1 1.716(3) . ? P1 C8 1.807(4) . ? P1 C14 1.811(4) . ? F1 C24 1.313(8) . ? F2 C24 1.330(6) . ? F3 C24 1.343(9) . ? O1 C22 1.238(4) . ? N1 C7 1.383(5) . ? N1 C1 1.415(5) . ? N2 C7 1.332(5) . ? N2 C6 1.346(5) . ? C1 C2 1.335(7) . ? C2 C3 1.430(6) . ? C3 C4 1.395(6) . ? C3 C7 1.401(5) . ? C4 C5 1.383(6) . ? C5 C6 1.387(6) . ? C8 C13 1.391(6) . ? C8 C9 1.393(6) . ? C9 C10 1.383(6) . ? C10 C11 1.373(7) . ? C11 C12 1.379(7) . ? C12 C13 1.391(5) . ? C14 C19 1.387(6) . ? C14 C15 1.397(6) . ? C15 C16 1.395(6) . ? C16 C17 1.378(7) . ? C17 C18 1.371(8) . ? C18 C19 1.395(7) . ? C20 C21 1.521(5) . ? C21 C22 1.482(6) . ? C22 C23 1.490(6) . ? 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 C20 Pd1 O1 82.88(13) . . ? C20 Pd1 N2 179.11(13) . . ? O1 Pd1 N2 97.98(11) . . ? C20 Pd1 P1 93.46(11) . . ? O1 Pd1 P1 175.92(7) . . ? N2 Pd1 P1 85.69(9) . . ? O2 S1 O3 113.5(2) . . ? O2 S1 O4 113.9(3) . . ? O3 S1 O4 116.7(3) . . ? O2 S1 C24 104.2(3) . . ? O3 S1 C24 103.2(3) . . ? O4 S1 C24 103.2(3) . . ? N1 P1 C8 105.45(18) . . ? N1 P1 C14 108.34(17) . . ? C8 P1 C14 105.07(18) . . ? N1 P1 Pd1 100.71(12) . . ? C8 P1 Pd1 117.03(12) . . ? C14 P1 Pd1 119.12(14) . . ? C22 O1 Pd1 112.6(2) . . ? C7 N1 C1 105.7(3) . . ? C7 N1 P1 118.1(2) . . ? C1 N1 P1 136.0(3) . . ? C7 N2 C6 114.5(3) . . ? C7 N2 Pd1 112.8(3) . . ? C6 N2 Pd1 132.7(3) . . ? C2 C1 N1 110.3(4) . . ? C1 C2 C3 108.5(4) . . ? C4 C3 C7 116.5(4) . . ? C4 C3 C2 137.9(4) . . ? C7 C3 C2 105.5(4) . . ? C5 C4 C3 117.3(4) . . ? C4 C5 C6 121.2(4) . . ? N2 C6 C5 123.1(4) . . ? N2 C7 N1 122.6(3) . . ? N2 C7 C3 127.4(4) . . ? N1 C7 C3 110.0(3) . . ? C13 C8 C9 119.7(4) . . ? C13 C8 P1 117.4(3) . . ? C9 C8 P1 122.4(3) . . ? C10 C9 C8 119.2(4) . . ? C11 C10 C9 120.9(4) . . ? C10 C11 C12 120.5(4) . . ? C11 C12 C13 119.3(5) . . ? C8 C13 C12 120.4(4) . . ? C19 C14 C15 120.1(4) . . ? C19 C14 P1 121.2(3) . . ? C15 C14 P1 118.6(3) . . ? C14 C15 C16 120.0(4) . . ? C17 C16 C15 119.3(5) . . ? C18 C17 C16 120.8(4) . . ? C17 C18 C19 120.8(4) . . ? C14 C19 C18 119.0(5) . . ? C21 C20 Pd1 107.2(3) . . ? C22 C21 C20 113.1(3) . . ? O1 C22 C21 120.3(3) . . ? O1 C22 C23 120.1(4) . . ? C21 C22 C23 119.6(4) . . ? F1 C24 F2 107.4(5) . . ? F1 C24 F3 108.3(5) . . ? F2 C24 F3 107.0(6) . . ? F1 C24 S1 111.8(6) . . ? F2 C24 S1 111.9(4) . . ? F3 C24 S1 110.1(4) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.601 _refine_diff_density_min -0.720 _refine_diff_density_rms 0.069 #===END data_compound8b_k01adb14 _database_code_CSD 217639 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H20 F3 N4 O4 P Pd S' _chemical_formula_weight 606.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.3530(2) _cell_length_b 11.2230(4) _cell_length_c 13.7950(5) _cell_angle_alpha 107.832(2) _cell_angle_beta 103.059(2) _cell_angle_gamma 94.394(2) _cell_volume 1184.34(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 18 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.702 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 608 _exptl_absorpt_coefficient_mu 0.998 _exptl_absorpt_correction_type multiscan _exptl_absorpt_process_details 'Sortav Blessing (1995) ' _exptl_absorpt_correction_T_min 0.9518 _exptl_absorpt_correction_T_max 0.9755 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15723 _diffrn_reflns_av_R_equivalents 0.0893 _diffrn_reflns_av_sigmaI/netI 0.1040 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 25.21 _reflns_number_total 4172 _reflns_number_gt 2861 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'Denzo and Scalepack (otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+0.3781*P+(0.0376P)^2^+0.0000sin\q/\l] where P = 0.00000Fo^2^ + 1.00000Fc^2^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4172 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0934 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1038 _refine_ls_wR_factor_gt 0.0902 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.03893(5) 0.00962(4) 0.84395(3) 0.02668(16) Uani 1 1 d . . . S1 S 0.28068(18) 0.31808(14) 0.76097(13) 0.0404(4) Uani 1 1 d . . . P1 P 0.07101(17) -0.18185(13) 0.76697(11) 0.0283(4) Uani 1 1 d . . . F1 F 0.3618(7) 0.3576(6) 0.6007(4) 0.136(3) Uani 1 1 d . . . F2 F 0.1791(5) 0.1942(4) 0.5573(3) 0.0745(12) Uani 1 1 d . . . F3 F 0.4313(6) 0.1882(6) 0.6277(4) 0.120(2) Uani 1 1 d . . . N1 N 0.2197(5) -0.0011(4) 0.9780(3) 0.0256(10) Uani 1 1 d . . . N2 N 0.2117(5) -0.2113(4) 0.8628(3) 0.0257(10) Uani 1 1 d . . . N3 N -0.0845(5) -0.3055(4) 0.7305(3) 0.0324(11) Uani 1 1 d . . . N4 N 0.1387(6) -0.2155(4) 0.6584(3) 0.0351(12) Uani 1 1 d . . . O1 O -0.0172(4) 0.1899(3) 0.9155(3) 0.0313(9) Uani 1 1 d . . . O2 O 0.1460(5) 0.3882(4) 0.7477(4) 0.0697(15) Uani 1 1 d . . . O3 O 0.2381(5) 0.2014(4) 0.7782(3) 0.0489(11) Uani 1 1 d . . . O4 O 0.4382(5) 0.3918(4) 0.8261(3) 0.0521(12) Uani 1 1 d . . . C1 C -0.1305(7) 0.0156(5) 0.7154(4) 0.0349(14) Uani 1 1 d . . . H1A H -0.0882 -0.0127 0.6544 0.042 Uiso 1 1 d R . . H1B H -0.2321 -0.0386 0.7047 0.042 Uiso 1 1 d R . . C2 C -0.1594(7) 0.1537(6) 0.7381(4) 0.0385(15) Uani 1 1 d . . . H2A H -0.2763 0.1528 0.7119 0.046 Uiso 1 1 d R . . H2B H -0.0989 0.1899 0.6997 0.046 Uiso 1 1 d R . . C3 C -0.1056(7) 0.2296(5) 0.8498(5) 0.0340(14) Uani 1 1 d . . . C4 C -0.1494(8) 0.3594(5) 0.8853(6) 0.0501(17) Uani 1 1 d . . . H4A H -0.2172 0.3756 0.8260 0.060 Uiso 1 1 d R . . H4B H -0.0493 0.4204 0.9147 0.060 Uiso 1 1 d R . . H4C H -0.2097 0.3657 0.9378 0.060 Uiso 1 1 d R . . C5 C 0.2105(6) -0.1232(6) 0.6253(4) 0.0370(14) Uani 1 1 d . . . H5 H 0.2105 -0.0354 0.6619 0.044 Uiso 1 1 d R . . C6 C 0.2688(8) -0.1800(7) 0.5429(5) 0.0510(18) Uani 1 1 d . . . H6 H 0.3247 -0.1487 0.4999 0.061 Uiso 1 1 d R . . C7 C 0.2336(8) -0.3128(7) 0.5222(5) 0.0585(19) Uani 1 1 d . . . H7 H 0.2562 -0.3833 0.4696 0.070 Uiso 1 1 d R . . C8 C 0.1548(8) -0.3344(6) 0.5917(5) 0.0463(16) Uani 1 1 d . . . H8 H 0.1125 -0.4098 0.6027 0.056 Uiso 1 1 d R . . C9 C -0.2226(7) -0.3263(5) 0.6444(5) 0.0435(16) Uani 1 1 d . . . H9 H -0.2126 -0.2936 0.5891 0.052 Uiso 1 1 d R . . C10 C -0.3502(8) -0.3922(5) 0.6591(5) 0.0451(16) Uani 1 1 d . . . H10 H -0.4622 -0.4242 0.6162 0.054 Uiso 1 1 d R . . C11 C -0.2976(7) -0.4133(5) 0.7558(5) 0.0381(15) Uani 1 1 d . . . H11 H -0.3544 -0.4570 0.7913 0.046 Uiso 1 1 d R . . C12 C -0.1384(7) -0.3585(5) 0.7995(5) 0.0348(14) Uani 1 1 d . . . H12 H -0.0612 -0.3508 0.8650 0.042 Uiso 1 1 d R . . C13 C 0.2982(7) -0.3131(5) 0.8720(5) 0.0349(14) Uani 1 1 d . . . H13 H 0.2745 -0.3908 0.8135 0.042 Uiso 1 1 d R . . C14 C 0.4043(7) -0.2794(5) 0.9680(5) 0.0347(14) Uani 1 1 d . . . H14 H 0.4806 -0.3245 1.0004 0.042 Uiso 1 1 d R . . C15 C 0.3927(6) -0.1515(5) 1.0269(4) 0.0296(13) Uani 1 1 d . . . C16 C 0.2726(6) -0.1139(5) 0.9582(4) 0.0266(13) Uani 1 1 d . . . C17 C 0.4662(6) -0.0633(5) 1.1252(4) 0.0324(14) Uani 1 1 d . . . H17 H 0.5496 -0.0802 1.1778 0.039 Uiso 1 1 d R . . C18 C 0.4157(6) 0.0546(5) 1.1481(4) 0.0320(14) Uani 1 1 d . . . H18 H 0.4670 0.1176 1.2156 0.038 Uiso 1 1 d R . . C19 C 0.2938(6) 0.0823(5) 1.0737(4) 0.0303(13) Uani 1 1 d . . . H19 H 0.2616 0.1648 1.0937 0.036 Uiso 1 1 d R . . C20 C 0.3166(9) 0.2629(8) 0.6316(6) 0.064(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0245(2) 0.0276(3) 0.0291(3) 0.01161(19) 0.00613(19) 0.00483(18) S1 0.0322(8) 0.0372(9) 0.0510(10) 0.0199(8) 0.0041(8) 0.0004(7) P1 0.0301(8) 0.0269(8) 0.0289(9) 0.0113(7) 0.0075(7) 0.0028(7) F1 0.146(5) 0.176(6) 0.060(3) 0.066(4) -0.019(3) -0.096(4) F2 0.065(3) 0.079(3) 0.055(3) 0.013(2) -0.010(2) -0.016(2) F3 0.061(3) 0.212(6) 0.078(3) 0.021(4) 0.031(3) 0.049(4) N1 0.022(2) 0.024(3) 0.032(3) 0.010(2) 0.011(2) 0.002(2) N2 0.031(2) 0.024(3) 0.025(3) 0.010(2) 0.010(2) 0.007(2) N3 0.039(3) 0.029(3) 0.026(3) 0.009(2) 0.003(2) 0.000(2) N4 0.042(3) 0.030(3) 0.032(3) 0.007(2) 0.014(2) 0.004(2) O1 0.032(2) 0.026(2) 0.040(2) 0.0133(19) 0.0120(19) 0.0071(18) O2 0.047(3) 0.038(3) 0.108(4) 0.016(3) -0.002(3) 0.010(2) O3 0.041(2) 0.042(3) 0.073(3) 0.034(2) 0.014(2) 0.001(2) O4 0.039(2) 0.063(3) 0.044(3) 0.023(2) -0.007(2) -0.016(2) C1 0.031(3) 0.041(4) 0.036(4) 0.017(3) 0.008(3) 0.005(3) C2 0.027(3) 0.055(4) 0.036(4) 0.026(3) -0.001(3) 0.000(3) C3 0.027(3) 0.031(4) 0.053(4) 0.025(3) 0.013(3) 0.006(3) C4 0.048(4) 0.038(4) 0.075(5) 0.032(4) 0.018(4) 0.015(3) C5 0.032(3) 0.047(4) 0.032(4) 0.018(3) 0.005(3) 0.001(3) C6 0.045(4) 0.071(5) 0.040(4) 0.019(4) 0.017(3) 0.011(4) C7 0.061(5) 0.070(5) 0.042(4) 0.007(4) 0.020(4) 0.023(4) C8 0.059(4) 0.041(4) 0.034(4) 0.004(3) 0.014(3) 0.008(3) C9 0.050(4) 0.037(4) 0.032(4) 0.013(3) -0.007(3) -0.008(3) C10 0.039(4) 0.033(4) 0.055(5) 0.011(3) 0.002(3) -0.001(3) C11 0.034(3) 0.030(3) 0.054(4) 0.019(3) 0.013(3) 0.001(3) C12 0.039(4) 0.028(3) 0.040(4) 0.017(3) 0.009(3) 0.007(3) C13 0.036(3) 0.024(3) 0.043(4) 0.009(3) 0.010(3) 0.009(3) C14 0.032(3) 0.033(4) 0.044(4) 0.021(3) 0.008(3) 0.005(3) C15 0.025(3) 0.038(4) 0.032(3) 0.017(3) 0.010(3) 0.004(3) C16 0.027(3) 0.025(3) 0.030(3) 0.010(3) 0.012(3) 0.001(3) C17 0.026(3) 0.044(4) 0.026(3) 0.012(3) 0.004(3) 0.002(3) C18 0.028(3) 0.041(4) 0.026(3) 0.007(3) 0.011(3) 0.002(3) C19 0.035(3) 0.030(3) 0.029(3) 0.009(3) 0.016(3) 0.007(3) C20 0.045(4) 0.086(6) 0.047(5) 0.029(4) -0.012(4) -0.021(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 2.027(5) . ? Pd1 O1 2.102(3) . ? Pd1 N1 2.148(4) . ? Pd1 P1 2.1532(15) . ? S1 O2 1.431(4) . ? S1 O3 1.434(4) . ? S1 O4 1.438(4) . ? S1 C20 1.803(8) . ? P1 N4 1.666(4) . ? P1 N2 1.692(4) . ? P1 N3 1.694(4) . ? F1 C20 1.321(8) . ? F2 C20 1.346(7) . ? F3 C20 1.320(9) . ? N1 C19 1.337(7) . ? N1 C16 1.343(6) . ? N2 C16 1.384(6) . ? N2 C13 1.420(6) . ? N3 C12 1.400(7) . ? N3 C9 1.401(7) . ? N4 C5 1.399(7) . ? N4 C8 1.406(7) . ? O1 C3 1.250(6) . ? C1 C2 1.533(8) . ? C2 C3 1.459(8) . ? C3 C4 1.490(8) . ? C5 C6 1.338(8) . ? C6 C7 1.423(9) . ? C7 C8 1.347(8) . ? C9 C10 1.339(8) . ? C10 C11 1.406(8) . ? C11 C12 1.340(7) . ? C13 C14 1.340(8) . ? C14 C15 1.440(7) . ? C15 C17 1.380(7) . ? C15 C16 1.401(7) . ? C17 C18 1.385(7) . ? C18 C19 1.399(7) . ? 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 C1 Pd1 O1 83.57(19) . . ? C1 Pd1 N1 178.6(2) . . ? O1 Pd1 N1 97.80(16) . . ? C1 Pd1 P1 93.33(16) . . ? O1 Pd1 P1 174.43(10) . . ? N1 Pd1 P1 85.31(12) . . ? O2 S1 O3 114.5(3) . . ? O2 S1 O4 115.6(3) . . ? O3 S1 O4 115.3(3) . . ? O2 S1 C20 103.8(4) . . ? O3 S1 C20 102.0(3) . . ? O4 S1 C20 103.1(3) . . ? N4 P1 N2 108.9(2) . . ? N4 P1 N3 100.3(2) . . ? N2 P1 N3 102.3(2) . . ? N4 P1 Pd1 119.59(17) . . ? N2 P1 Pd1 102.45(15) . . ? N3 P1 Pd1 121.77(16) . . ? C19 N1 C16 114.6(5) . . ? C19 N1 Pd1 133.3(4) . . ? C16 N1 Pd1 112.0(4) . . ? C16 N2 C13 106.0(4) . . ? C16 N2 P1 117.5(3) . . ? C13 N2 P1 136.4(4) . . ? C12 N3 C9 106.4(4) . . ? C12 N3 P1 125.1(4) . . ? C9 N3 P1 121.9(4) . . ? C5 N4 C8 107.4(5) . . ? C5 N4 P1 123.5(4) . . ? C8 N4 P1 128.7(4) . . ? C3 O1 Pd1 111.9(3) . . ? C2 C1 Pd1 106.8(4) . . ? C3 C2 C1 113.6(5) . . ? O1 C3 C2 121.1(5) . . ? O1 C3 C4 119.4(6) . . ? C2 C3 C4 119.4(5) . . ? C6 C5 N4 109.2(6) . . ? C5 C6 C7 106.9(6) . . ? C8 C7 C6 109.4(6) . . ? C7 C8 N4 107.0(6) . . ? C10 C9 N3 108.3(5) . . ? C9 C10 C11 108.6(6) . . ? C12 C11 C10 107.8(5) . . ? C11 C12 N3 108.8(5) . . ? C14 C13 N2 109.7(5) . . ? C13 C14 C15 109.0(5) . . ? C17 C15 C16 117.0(5) . . ? C17 C15 C14 138.0(5) . . ? C16 C15 C14 105.0(5) . . ? N1 C16 N2 122.7(5) . . ? N1 C16 C15 126.9(5) . . ? N2 C16 C15 110.4(4) . . ? C15 C17 C18 117.7(5) . . ? C17 C18 C19 120.8(5) . . ? N1 C19 C18 123.1(5) . . ? F1 C20 F3 108.6(7) . . ? F1 C20 F2 106.0(6) . . ? F3 C20 F2 105.8(7) . . ? F1 C20 S1 112.0(6) . . ? F3 C20 S1 112.0(5) . . ? F2 C20 S1 112.2(5) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.21 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.567 _refine_diff_density_min -0.711 _refine_diff_density_rms 0.112 #===END data_compound10_k01adb8 _database_code_CSD 217640 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H33 F6 N4 O7.50 P2 Pd S2' _chemical_formula_weight 1036.16 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' F F 0.0171 0.0103 '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' 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 P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.4210(2) _cell_length_b 20.4340(3) _cell_length_c 15.6820(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.3160(10) _cell_angle_gamma 90.00 _cell_volume 4300.64(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 18 _exptl_crystal_description Block _exptl_crystal_colour Pale_straw _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.600 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2092 _exptl_absorpt_coefficient_mu 0.684 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 1.09 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41124 _diffrn_reflns_av_R_equivalents 0.0510 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.59 _diffrn_reflns_theta_max 25.03 _reflns_number_total 7567 _reflns_number_gt 6867 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'Denzo and Scalepack (otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+15.2535*P+(0.0216P)^2^+0.0000sin\q/\l] where P = 0.00000Fo^2^ + 1.00000Fc^2^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0021(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7567 _refine_ls_number_parameters 659 _refine_ls_number_restraints 183 _refine_ls_R_factor_all 0.0520 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1190 _refine_ls_wR_factor_gt 0.1159 _refine_ls_goodness_of_fit_ref 1.225 _refine_ls_restrained_S_all 1.217 _refine_ls_shift/su_max 0.329 _refine_ls_shift/su_mean 0.011 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.46932(2) 0.159712(15) 0.19942(2) 0.02399(12) Uani 1 1 d . B . S1 S 0.65736(8) 0.02207(5) 0.30159(7) 0.0256(2) Uani 1 1 d . . . S2 S 0.3444(5) -0.3001(3) 0.2930(3) 0.0475(11) Uani 0.60 1 d P A 1 S2A S 0.3323(9) -0.3069(6) 0.3249(5) 0.063(2) Uani 0.40 1 d P A 2 P1 P 0.49710(8) 0.21323(6) 0.07568(7) 0.0273(3) Uani 1 1 d . . . P2 P 0.54053(8) 0.23715(5) 0.28133(7) 0.0250(2) Uani 1 1 d . . . F1 F 0.8003(2) -0.03402(17) 0.2163(2) 0.0634(9) Uani 1 1 d . . . F2 F 0.8473(2) 0.04967(16) 0.2891(3) 0.0713(11) Uani 1 1 d . . . F3 F 0.8161(3) -0.04141(16) 0.3520(2) 0.0653(10) Uani 1 1 d . . . F4 F 0.3237(6) -0.3410(4) 0.4426(6) 0.089(2) Uani 0.60 1 d P A 1 F4A F 0.4819(9) -0.3845(7) 0.3172(11) 0.119(4) Uani 0.40 1 d PU A 2 F5 F 0.4738(6) -0.3479(5) 0.3998(7) 0.113(3) Uani 0.60 1 d PU A 1 F5A F 0.383(4) -0.3647(7) 0.1820(12) 0.39(3) Uani 0.40 1 d P A 2 F6 F 0.3619(8) -0.4169(4) 0.3564(8) 0.132(3) Uani 0.60 1 d PU A 1 F6A F 0.3409(10) -0.4278(4) 0.2726(10) 0.106(4) Uani 0.40 1 d PU A 2 O1 O 0.6578(2) 0.05669(15) 0.38162(19) 0.0352(7) Uani 1 1 d . . . O2 O 0.6382(3) 0.06165(17) 0.2276(2) 0.0409(8) Uani 1 1 d . . . O3 O 0.6054(2) -0.04012(15) 0.3025(2) 0.0353(7) Uani 1 1 d . . . O4 O 0.3699(9) -0.2391(6) 0.3292(6) 0.071(3) Uani 0.60 1 d PU A 1 O4A O 0.3784(15) -0.2485(9) 0.2813(12) 0.084(4) Uani 0.40 1 d PU A 2 O5 O 0.2393(4) -0.3114(3) 0.2825(4) 0.102(2) Uani 1 1 d . . . O5A O 0.321(5) -0.3137(19) 0.392(2) 0.33(3) Uani 0.40 1 d P A 2 O6 O 0.4140(7) -0.3235(8) 0.2187(6) 0.127(5) Uani 0.60 1 d P A 1 O7 O 0.4103(4) -0.1021(3) 0.2715(5) 0.115(2) Uani 1 1 d D . . N1 N 0.4264(3) 0.16471(19) 0.0108(2) 0.0392(10) Uani 1 1 d . . . N2 N 0.4217(3) 0.08252(18) 0.1179(2) 0.0321(8) Uani 1 1 d . . . N3 N 0.5312(3) 0.19947(19) 0.3779(2) 0.0318(8) Uani 1 1 d . B . N4 N 0.4324(3) 0.11529(18) 0.3169(2) 0.0284(8) Uani 1 1 d . . . C1 C 0.6716(3) 0.2504(2) 0.2667(3) 0.0258(9) Uani 1 1 d . B . C2 C 0.7040(3) 0.3027(2) 0.2174(3) 0.0290(9) Uani 1 1 d . . . H2 H 0.6580 0.3353 0.1992 0.035 Uiso 1 1 calc R B . C3 C 0.8042(3) 0.3074(2) 0.1947(3) 0.0347(10) Uani 1 1 d . B . H3 H 0.8264 0.3428 0.1605 0.042 Uiso 1 1 calc R . . C4 C 0.8710(3) 0.2603(2) 0.2224(3) 0.0361(11) Uani 1 1 d . . . H4 H 0.9391 0.2630 0.2066 0.043 Uiso 1 1 calc R B . C5 C 0.8387(3) 0.2087(2) 0.2736(3) 0.0354(11) Uani 1 1 d . B . H5 H 0.8852 0.1770 0.2934 0.042 Uiso 1 1 calc R . . C6 C 0.7391(3) 0.2033(2) 0.2957(3) 0.0285(9) Uani 1 1 d . . . H6 H 0.7171 0.1680 0.3302 0.034 Uiso 1 1 calc R B . C13 C 0.6222(3) 0.2103(2) 0.0369(3) 0.0324(10) Uani 1 1 d . . . C14 C 0.6519(5) 0.2440(3) -0.0370(3) 0.0547(15) Uani 1 1 d . . . H14 H 0.6052 0.2705 -0.0669 0.066 Uiso 1 1 calc R . . C15 C 0.7479(5) 0.2388(4) -0.0662(4) 0.071(2) Uani 1 1 d . . . H15 H 0.7678 0.2618 -0.1159 0.085 Uiso 1 1 calc R . . C16 C 0.8152(5) 0.2000(3) -0.0229(4) 0.0601(17) Uani 1 1 d . . . H16 H 0.8816 0.1967 -0.0430 0.072 Uiso 1 1 calc R . . C17 C 0.7874(4) 0.1658(3) 0.0493(3) 0.0398(11) Uani 1 1 d . . . H17 H 0.8345 0.1388 0.0780 0.048 Uiso 1 1 calc R . . C18 C 0.6912(3) 0.1709(2) 0.0797(3) 0.0301(10) Uani 1 1 d . . . H18 H 0.6721 0.1476 0.1294 0.036 Uiso 1 1 calc R . . C19 C 0.4486(3) 0.2937(2) 0.0551(3) 0.0324(10) Uani 1 1 d . . . C20 C 0.5107(4) 0.3485(2) 0.0578(3) 0.0427(12) Uani 1 1 d . . . H20 H 0.5800 0.3433 0.0687 0.051 Uiso 1 1 calc R . . C21 C 0.4715(4) 0.4101(3) 0.0447(4) 0.0577(16) Uani 1 1 d . . . H21 H 0.5134 0.4475 0.0482 0.069 Uiso 1 1 calc R . . C22 C 0.3707(5) 0.4176(3) 0.0264(4) 0.0603(17) Uani 1 1 d . . . H22 H 0.3445 0.4599 0.0152 0.072 Uiso 1 1 calc R . . C23 C 0.3087(4) 0.3641(3) 0.0245(4) 0.0542(15) Uani 1 1 d . . . H23 H 0.2396 0.3697 0.0128 0.065 Uiso 1 1 calc R . . C24 C 0.3467(4) 0.3020(2) 0.0396(3) 0.0421(12) Uani 1 1 d . . . H24 H 0.3036 0.2651 0.0393 0.051 Uiso 1 1 calc R . . C25 C 0.4097(5) 0.1661(3) -0.0783(3) 0.0546(15) Uani 1 1 d . . . H25 H 0.4198 0.2030 -0.1140 0.065 Uiso 1 1 calc R . . C26 C 0.3775(5) 0.1075(3) -0.1046(4) 0.0576(16) Uani 1 1 d . B . H26 H 0.3594 0.0963 -0.1615 0.069 Uiso 1 1 calc R . . C27 C 0.3750(4) 0.0643(3) -0.0324(3) 0.0467(13) Uani 1 1 d . . . C28 C 0.3573(4) -0.0014(3) -0.0167(4) 0.0538(15) Uani 1 1 d . B . H28 H 0.3343 -0.0298 -0.0606 0.065 Uiso 1 1 calc R . . C29 C 0.3745(4) -0.0242(3) 0.0657(4) 0.0522(14) Uani 1 1 d . . . H29 H 0.3634 -0.0691 0.0783 0.063 Uiso 1 1 calc R B . C30 C 0.4077(4) 0.0176(2) 0.1301(4) 0.0433(12) Uani 1 1 d . B . H30 H 0.4211 -0.0002 0.1850 0.052 Uiso 1 1 calc R . . C31 C 0.4072(4) 0.1021(2) 0.0374(3) 0.0358(11) Uani 1 1 d . B . C32 C 0.5626(4) 0.2158(3) 0.4613(3) 0.0478(13) Uani 1 1 d . . . H32 H 0.6033 0.2521 0.4761 0.057 Uiso 1 1 calc R B . C33 C 0.5256(4) 0.1718(3) 0.5166(3) 0.0537(15) Uani 1 1 d . B . H33 H 0.5361 0.1719 0.5765 0.064 Uiso 1 1 calc R . . C34 C 0.4677(4) 0.1246(3) 0.4701(3) 0.0432(13) Uani 1 1 d . . . C35 C 0.4126(5) 0.0690(3) 0.4862(4) 0.0569(16) Uani 1 1 d . B . H35 H 0.4068 0.0520 0.5423 0.068 Uiso 1 1 calc R . . C36 C 0.3664(5) 0.0391(3) 0.4182(4) 0.0610(17) Uani 1 1 d . . . H36 H 0.3268 0.0013 0.4280 0.073 Uiso 1 1 calc R B . C37 C 0.3759(4) 0.0627(3) 0.3354(4) 0.0475(13) Uani 1 1 d . B . H37 H 0.3415 0.0410 0.2905 0.057 Uiso 1 1 calc R . . C38 C 0.4737(3) 0.1440(2) 0.3844(3) 0.0306(10) Uani 1 1 d . B . C39 C 0.7868(4) -0.0018(2) 0.2886(4) 0.0418(12) Uani 1 1 d . . . C40A C 0.3807(13) -0.3548(7) 0.3770(11) 0.084(4) Uani 0.60 1 d P A 1 C40B C 0.3879(15) -0.3707(10) 0.264(2) 0.106(9) Uani 0.40 1 d P A 2 C71 C 0.4749(7) 0.3143(3) 0.2877(7) 0.0502(12) Uani 0.45 1 d PGU B 2 C72 C 0.5168(6) 0.3714(4) 0.3201(6) 0.0526(12) Uani 0.45 1 d PGU B 1 H72 H 0.5814 0.3725 0.3450 0.063 Uiso 0.45 1 calc PR B 1 C73 C 0.4630(6) 0.4295(3) 0.3180(6) 0.0551(14) Uani 0.45 1 d PGU B 1 H73 H 0.4915 0.4685 0.3401 0.066 Uiso 0.45 1 calc PR B 1 C74 C 0.3673(6) 0.4305(3) 0.2835(6) 0.0551(14) Uani 0.45 1 d PGU B 1 H74 H 0.3305 0.4702 0.2821 0.066 Uiso 0.45 1 calc PR B 1 C75 C 0.3255(6) 0.3734(4) 0.2512(6) 0.0533(13) Uani 0.45 1 d PGU B 1 H75 H 0.2601 0.3740 0.2276 0.064 Uiso 0.45 1 calc PR B 1 C76 C 0.3793(7) 0.3153(3) 0.2532(7) 0.0511(12) Uani 0.45 1 d PGU B 1 H76 H 0.3513 0.2757 0.2321 0.061 Uiso 0.45 1 calc PR B 1 C77 C 0.4860(4) 0.3168(2) 0.2911(4) 0.0502(12) Uani 0.55 1 d PGU B 1 C78 C 0.5333(4) 0.3626(3) 0.3428(4) 0.0523(12) Uani 0.55 1 d PGU B 2 H78 H 0.5998 0.3540 0.3607 0.063 Uiso 0.55 1 calc PR B 2 C79 C 0.4841(5) 0.4198(3) 0.3656(4) 0.0552(13) Uani 0.55 1 d PGU B 2 H79 H 0.5164 0.4511 0.4010 0.066 Uiso 0.55 1 calc PR B 2 C80 C 0.3876(5) 0.4311(2) 0.3366(4) 0.0564(13) Uani 0.55 1 d PGU B 2 H80 H 0.3539 0.4702 0.3522 0.068 Uiso 0.55 1 calc PR B 2 C81 C 0.3403(4) 0.3853(3) 0.2848(5) 0.0543(13) Uani 0.55 1 d PGU B 2 H81 H 0.2743 0.3931 0.2650 0.065 Uiso 0.55 1 calc PR B 2 C82 C 0.3895(4) 0.3281(3) 0.2621(4) 0.0514(12) Uani 0.55 1 d PGU B 2 H82 H 0.3565 0.2982 0.2252 0.062 Uiso 0.55 1 calc PR B 2 O8 O 0.8934(9) -0.0107(5) 0.0136(7) 0.156(8) Uani 0.50 1 d PG . . HW7A H 0.4702 -0.0892 0.2872 0.188 Uiso 1 1 d GD . . HW7B H 0.4025 -0.1446 0.2809 0.188 Uiso 1 1 d GD . . 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 0.02071(18) 0.02463(19) 0.02659(19) 0.00820(13) -0.00257(12) -0.00284(13) S1 0.0262(5) 0.0239(5) 0.0267(5) 0.0045(4) -0.0012(4) 0.0003(4) S2 0.0367(17) 0.048(2) 0.058(3) -0.010(2) -0.010(2) -0.0032(14) S2A 0.061(5) 0.067(4) 0.059(5) -0.003(5) -0.022(4) 0.000(3) P1 0.0295(6) 0.0282(6) 0.0242(6) 0.0082(4) -0.0039(4) -0.0020(5) P2 0.0234(5) 0.0243(5) 0.0273(6) 0.0008(4) 0.0064(4) 0.0014(4) F1 0.054(2) 0.062(2) 0.074(2) -0.0206(18) 0.0221(17) 0.0084(17) F2 0.0318(17) 0.0418(18) 0.140(4) -0.015(2) 0.0112(19) -0.0083(14) F3 0.055(2) 0.0427(18) 0.097(3) -0.0047(18) -0.0382(19) 0.0188(15) F4 0.074(5) 0.093(6) 0.101(6) -0.031(5) 0.009(4) -0.022(4) F4A 0.059(6) 0.121(9) 0.177(10) 0.006(8) 0.013(7) 0.021(6) F5 0.058(4) 0.123(7) 0.158(8) 0.005(6) -0.012(5) 0.006(4) F5A 1.03(9) 0.043(8) 0.101(13) -0.038(8) 0.18(3) -0.07(2) F6 0.159(8) 0.048(4) 0.188(9) -0.018(5) -0.035(7) -0.001(5) F6A 0.126(8) 0.024(4) 0.167(10) 0.000(6) -0.047(8) -0.004(5) O1 0.0439(19) 0.0309(17) 0.0310(17) -0.0024(13) 0.0030(14) 0.0005(14) O2 0.047(2) 0.0407(19) 0.0348(18) 0.0166(15) -0.0034(15) 0.0041(16) O3 0.0352(17) 0.0290(17) 0.0416(19) 0.0014(14) -0.0030(14) -0.0083(14) O4 0.073(5) 0.057(5) 0.081(7) -0.005(6) -0.017(6) -0.022(4) O4A 0.074(7) 0.057(7) 0.121(11) 0.000(9) -0.015(10) -0.022(6) O5 0.043(3) 0.100(4) 0.163(6) 0.001(4) -0.016(3) -0.017(3) O5A 0.64(10) 0.22(4) 0.14(3) 0.11(3) 0.02(4) 0.07(5) O6 0.053(5) 0.261(17) 0.067(6) 0.042(9) -0.017(4) -0.043(8) O7 0.081(4) 0.095(4) 0.168(6) 0.056(4) -0.038(4) -0.030(3) N1 0.051(3) 0.032(2) 0.034(2) 0.0055(17) -0.0176(18) -0.0045(19) N2 0.029(2) 0.029(2) 0.038(2) 0.0074(16) -0.0087(16) -0.0052(16) N3 0.032(2) 0.038(2) 0.0262(19) -0.0017(16) 0.0084(15) 0.0026(17) N4 0.0215(17) 0.034(2) 0.0301(19) 0.0112(16) 0.0060(15) 0.0006(15) C1 0.025(2) 0.026(2) 0.027(2) -0.0093(17) 0.0026(16) -0.0018(17) C2 0.031(2) 0.025(2) 0.031(2) -0.0055(18) 0.0041(18) -0.0003(18) C3 0.036(3) 0.028(2) 0.039(3) -0.0061(19) 0.009(2) -0.009(2) C4 0.026(2) 0.036(3) 0.046(3) -0.015(2) 0.006(2) -0.008(2) C5 0.027(2) 0.032(2) 0.047(3) -0.013(2) -0.006(2) 0.0012(19) C6 0.031(2) 0.026(2) 0.029(2) -0.0067(17) -0.0045(18) -0.0029(18) C13 0.035(2) 0.037(3) 0.025(2) 0.0046(19) 0.0044(18) -0.001(2) C14 0.059(4) 0.071(4) 0.034(3) 0.022(3) 0.016(2) 0.011(3) C15 0.074(4) 0.088(5) 0.051(4) 0.026(3) 0.033(3) 0.013(4) C16 0.049(3) 0.083(5) 0.049(3) 0.000(3) 0.026(3) 0.007(3) C17 0.035(3) 0.043(3) 0.041(3) -0.006(2) 0.006(2) 0.004(2) C18 0.037(2) 0.028(2) 0.025(2) -0.0057(17) 0.0004(18) 0.0001(19) C19 0.034(2) 0.030(2) 0.033(2) 0.0114(19) -0.0081(19) 0.0003(19) C20 0.032(3) 0.038(3) 0.058(3) 0.023(2) -0.008(2) -0.005(2) C21 0.047(3) 0.036(3) 0.090(5) 0.027(3) -0.014(3) -0.008(2) C22 0.052(3) 0.040(3) 0.089(5) 0.025(3) -0.017(3) 0.006(3) C23 0.035(3) 0.047(3) 0.080(4) 0.020(3) -0.013(3) 0.007(2) C24 0.033(3) 0.037(3) 0.057(3) 0.013(2) -0.010(2) -0.005(2) C25 0.082(4) 0.046(3) 0.036(3) 0.009(2) -0.027(3) 0.000(3) C26 0.082(4) 0.050(3) 0.041(3) -0.003(3) -0.031(3) 0.000(3) C27 0.050(3) 0.041(3) 0.048(3) -0.004(2) -0.024(2) -0.002(2) C28 0.059(4) 0.042(3) 0.061(4) -0.007(3) -0.021(3) -0.008(3) C29 0.052(3) 0.029(3) 0.075(4) 0.001(3) -0.013(3) -0.012(2) C30 0.044(3) 0.032(3) 0.053(3) 0.009(2) -0.009(2) -0.008(2) C31 0.036(3) 0.032(2) 0.039(3) 0.003(2) -0.012(2) -0.002(2) C32 0.049(3) 0.062(4) 0.032(3) -0.015(2) 0.002(2) 0.007(3) C33 0.058(3) 0.079(4) 0.024(3) 0.001(3) 0.006(2) 0.016(3) C34 0.041(3) 0.055(3) 0.034(3) 0.012(2) 0.014(2) 0.019(2) C35 0.061(4) 0.065(4) 0.045(3) 0.030(3) 0.022(3) 0.012(3) C36 0.065(4) 0.053(4) 0.065(4) 0.029(3) 0.024(3) -0.010(3) C37 0.042(3) 0.047(3) 0.053(3) 0.018(3) 0.010(2) -0.017(2) C38 0.025(2) 0.034(2) 0.032(2) 0.0096(19) 0.0086(18) 0.0103(19) C39 0.029(2) 0.030(3) 0.067(4) -0.010(2) -0.002(2) 0.002(2) C40A 0.104(11) 0.056(8) 0.091(11) -0.011(7) -0.015(9) 0.011(7) C40B 0.065(13) 0.067(13) 0.19(3) 0.018(15) 0.070(15) -0.004(10) C71 0.043(2) 0.0304(19) 0.077(3) 0.006(2) 0.028(2) 0.0090(18) C72 0.047(2) 0.0313(19) 0.080(3) 0.004(2) 0.027(2) 0.0094(18) C73 0.051(2) 0.033(2) 0.081(3) 0.005(2) 0.026(3) 0.011(2) C74 0.050(2) 0.036(2) 0.080(3) 0.005(2) 0.026(3) 0.013(2) C75 0.047(2) 0.035(2) 0.078(3) 0.006(2) 0.026(2) 0.013(2) C76 0.045(2) 0.032(2) 0.077(3) 0.008(2) 0.027(2) 0.0104(19) C77 0.043(2) 0.0304(18) 0.077(3) 0.0055(19) 0.028(2) 0.0088(18) C78 0.046(2) 0.031(2) 0.080(3) 0.003(2) 0.028(2) 0.0085(19) C79 0.050(2) 0.033(2) 0.082(3) 0.004(2) 0.027(2) 0.009(2) C80 0.052(2) 0.035(2) 0.083(3) 0.006(2) 0.027(3) 0.011(2) C81 0.048(2) 0.036(2) 0.080(3) 0.007(2) 0.027(2) 0.0117(19) C82 0.045(2) 0.0326(19) 0.077(3) 0.008(2) 0.027(2) 0.0100(18) O8 0.101(9) 0.257(19) 0.112(10) 0.101(11) 0.053(8) 0.096(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N4 2.115(3) . ? Pd1 N2 2.127(4) . ? Pd1 P2 2.2481(12) . ? Pd1 P1 2.2602(11) . ? S1 O2 1.436(3) . ? S1 O1 1.441(3) . ? S1 O3 1.450(3) . ? S1 C39 1.818(5) . ? S2 O4 1.411(13) . ? S2 O5 1.438(8) . ? S2 O6 1.572(14) . ? S2 C40A 1.792(18) . ? S2A O5A 1.07(4) . ? S2A O5 1.414(13) . ? S2A O4A 1.51(2) . ? S2A C40B 1.78(3) . ? P1 N1 1.705(4) . ? P1 C13 1.790(5) . ? P1 C19 1.798(5) . ? P2 N3 1.705(4) . ? P2 C77 1.791(5) . ? P2 C1 1.796(4) . ? P2 C71 1.808(6) . ? F1 C39 1.324(6) . ? F2 C39 1.329(6) . ? F3 C39 1.338(6) . ? F4 C40A 1.316(18) . ? F4A C40B 1.53(3) . ? F5 C40A 1.305(17) . ? F5A C40B 1.30(3) . ? F6 C40A 1.334(15) . ? F6A C40B 1.33(2) . ? N1 C31 1.370(6) . ? N1 C25 1.414(6) . ? N2 C31 1.337(6) . ? N2 C30 1.354(6) . ? N3 C38 1.376(6) . ? N3 C32 1.412(6) . ? N4 C38 1.328(6) . ? N4 C37 1.348(6) . ? C1 C2 1.390(6) . ? C1 C6 1.395(6) . ? C2 C3 1.396(6) . ? C3 C4 1.385(7) . ? C4 C5 1.395(7) . ? C5 C6 1.387(6) . ? C13 C18 1.397(6) . ? C13 C14 1.407(6) . ? C14 C15 1.374(8) . ? C15 C16 1.377(9) . ? C16 C17 1.385(8) . ? C17 C18 1.383(6) . ? C19 C20 1.396(7) . ? C19 C24 1.397(6) . ? C20 C21 1.381(7) . ? C21 C22 1.390(8) . ? C22 C23 1.374(8) . ? C23 C24 1.388(7) . ? C25 C26 1.337(8) . ? C26 C27 1.437(8) . ? C27 C28 1.384(8) . ? C27 C31 1.406(7) . ? C28 C29 1.392(8) . ? C29 C30 1.394(7) . ? C32 C33 1.346(8) . ? C33 C34 1.434(8) . ? C34 C35 1.379(8) . ? C34 C38 1.405(6) . ? C35 C36 1.374(9) . ? C36 C37 1.391(8) . ? C71 C82 1.245(13) . ? C71 C78 1.526(14) . ? C72 C77 1.273(13) . ? C72 C73 1.3900 . ? C73 C74 1.3900 . ? C74 C75 1.3900 . ? C75 C76 1.3900 . ? C76 C77 1.548(14) . ? C78 C79 1.3900 . ? C79 C80 1.3900 . ? C80 C81 1.3900 . ? C81 C82 1.3900 . ? 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 N4 Pd1 N2 97.73(14) . . ? N4 Pd1 P2 84.56(11) . . ? N2 Pd1 P2 172.32(11) . . ? N4 Pd1 P1 174.87(10) . . ? N2 Pd1 P1 83.85(10) . . ? P2 Pd1 P1 94.50(4) . . ? O2 S1 O1 115.3(2) . . ? O2 S1 O3 114.7(2) . . ? O1 S1 O3 114.90(19) . . ? O2 S1 C39 103.2(2) . . ? O1 S1 C39 103.3(2) . . ? O3 S1 C39 103.1(2) . . ? O4 S2 O5 115.1(7) . . ? O4 S2 O6 115.0(8) . . ? O5 S2 O6 116.9(6) . . ? O4 S2 C40A 101.0(7) . . ? O5 S2 C40A 104.3(7) . . ? O6 S2 C40A 101.2(8) . . ? O5A S2A O5 109(3) . . ? O5A S2A O4A 127(3) . . ? O5 S2A O4A 101.6(10) . . ? O5A S2A C40B 119(3) . . ? O5 S2A C40B 94.1(11) . . ? O4A S2A C40B 99.4(11) . . ? N1 P1 C13 107.4(2) . . ? N1 P1 C19 103.0(2) . . ? C13 P1 C19 108.0(2) . . ? N1 P1 Pd1 97.86(14) . . ? C13 P1 Pd1 115.80(15) . . ? C19 P1 Pd1 122.38(16) . . ? N3 P2 C77 107.6(2) . . ? N3 P2 C1 105.0(2) . . ? C77 P2 C1 105.9(2) . . ? N3 P2 C71 107.8(4) . . ? C77 P2 C71 5.3(5) . . ? C1 P2 C71 110.7(3) . . ? N3 P2 Pd1 99.03(14) . . ? C77 P2 Pd1 121.0(2) . . ? C1 P2 Pd1 116.55(13) . . ? C71 P2 Pd1 116.1(3) . . ? S2A O5 S2 22.0(3) . . ? C31 N1 C25 106.8(4) . . ? C31 N1 P1 117.8(3) . . ? C25 N1 P1 131.5(4) . . ? C31 N2 C30 114.1(4) . . ? C31 N2 Pd1 112.8(3) . . ? C30 N2 Pd1 133.1(3) . . ? C38 N3 C32 107.0(4) . . ? C38 N3 P2 118.8(3) . . ? C32 N3 P2 133.9(4) . . ? C38 N4 C37 114.4(4) . . ? C38 N4 Pd1 113.9(3) . . ? C37 N4 Pd1 131.6(3) . . ? C2 C1 C6 120.5(4) . . ? C2 C1 P2 119.8(3) . . ? C6 C1 P2 119.2(3) . . ? C1 C2 C3 119.9(4) . . ? C4 C3 C2 119.7(4) . . ? C3 C4 C5 120.2(4) . . ? C6 C5 C4 120.5(4) . . ? C5 C6 C1 119.2(4) . . ? C18 C13 C14 119.2(4) . . ? C18 C13 P1 118.5(3) . . ? C14 C13 P1 122.3(4) . . ? C15 C14 C13 120.5(5) . . ? C16 C15 C14 119.6(5) . . ? C15 C16 C17 121.1(5) . . ? C18 C17 C16 120.0(5) . . ? C17 C18 C13 119.7(4) . . ? C20 C19 C24 119.5(4) . . ? C20 C19 P1 120.8(3) . . ? C24 C19 P1 119.7(4) . . ? C21 C20 C19 119.9(5) . . ? C20 C21 C22 120.1(5) . . ? C23 C22 C21 120.4(5) . . ? C22 C23 C24 120.1(5) . . ? C23 C24 C19 119.9(5) . . ? C26 C25 N1 109.7(5) . . ? C25 C26 C27 108.4(5) . . ? C28 C27 C31 116.5(5) . . ? C28 C27 C26 137.8(5) . . ? C31 C27 C26 105.5(5) . . ? C27 C28 C29 117.5(5) . . ? C30 C29 C28 121.2(5) . . ? N2 C30 C29 122.8(5) . . ? N2 C31 N1 122.6(4) . . ? N2 C31 C27 127.8(4) . . ? N1 C31 C27 109.5(4) . . ? C33 C32 N3 109.2(5) . . ? C32 C33 C34 108.9(5) . . ? C35 C34 C38 116.1(5) . . ? C35 C34 C33 138.6(5) . . ? C38 C34 C33 105.3(5) . . ? C36 C35 C34 117.7(5) . . ? C35 C36 C37 121.8(5) . . ? N4 C37 C36 122.1(6) . . ? N4 C38 N3 122.5(4) . . ? N4 C38 C34 127.8(5) . . ? N3 C38 C34 109.7(4) . . ? F2 C39 F1 108.2(5) . . ? F2 C39 F3 107.3(4) . . ? F1 C39 F3 107.2(4) . . ? F2 C39 S1 111.7(3) . . ? F1 C39 S1 111.3(3) . . ? F3 C39 S1 110.9(4) . . ? F5 C40A F4 108.8(13) . . ? F5 C40A F6 110.5(12) . . ? F4 C40A F6 106.4(15) . . ? F5 C40A S2 113.0(12) . . ? F4 C40A S2 106.5(10) . . ? F6 C40A S2 111.4(11) . . ? F5A C40B F6A 99(2) . . ? F5A C40B F4A 127(3) . . ? F6A C40B F4A 100.0(18) . . ? F5A C40B S2A 116(2) . . ? F6A C40B S2A 112.9(14) . . ? F4A C40B S2A 101.1(18) . . ? C82 C71 C78 120.3(7) . . ? C82 C71 P2 128.9(8) . . ? C78 C71 P2 110.3(6) . . ? C77 C72 C73 125.0(5) . . ? C74 C73 C72 120.0 . . ? C73 C74 C75 120.0 . . ? C74 C75 C76 120.0 . . ? C75 C76 C77 118.1(4) . . ? C72 C77 C76 116.9(7) . . ? C72 C77 P2 134.1(6) . . ? C76 C77 P2 109.1(4) . . ? C79 C78 C71 116.5(4) . . ? C80 C79 C78 120.0 . . ? C81 C80 C79 120.0 . . ? C82 C81 C80 120.0 . . ? C71 C82 C81 123.1(6) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.685 _refine_diff_density_min -0.564 _refine_diff_density_rms 0.082