Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Kim, Yong-Joo' 'Han, Jin-Taek' 'Han, Won Seok' 'Joo, Young-Seon' 'Lee, Soon-W' _publ_contact_author_name 'Prof Yong-Joo Kim' _publ_contact_author_address ; Department of Chemistry Kangnung National University Kangnung 210-702 KOREA ; _publ_contact_author_email 'YJKIM@KNUSUN.KANGNUNG.AC.KR' _publ_section_title ; Synthesis, structures and properties of bis(carbodiimido) complexes of Ni(II), Pd(II) and Pt(II) ; data_coph _database_code_CSD 184849 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H14 N2 O' _chemical_formula_weight 250.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Orthorhombic' _symmetry_space_group_name_H-M 'Pbca ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 7.570(2) _cell_length_b 15.073(6) _cell_length_c 24.035(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2742.6(14) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5.09 _cell_measurement_theta_max 10.93 _exptl_crystal_description 'BLOCK ' _exptl_crystal_colour 'COLORLESS ' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.212 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 0.077 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'MoK\a' _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4034 _diffrn_reflns_av_R_equivalents 0.2075 _diffrn_reflns_av_sigmaI/netI 0.1231 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2402 _reflns_number_gt 909 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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^)+(0.0636P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0030(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2402 _refine_ls_number_parameters 173 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2009 _refine_ls_R_factor_gt 0.0705 _refine_ls_wR_factor_ref 0.1839 _refine_ls_wR_factor_gt 0.1356 _refine_ls_goodness_of_fit_ref 0.954 _refine_ls_restrained_S_all 0.954 _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 O1 O 0.1548(4) 0.9507(2) 0.04514(13) 0.0778(11) Uani 1 1 d . . . N1 N 0.0294(4) 0.9040(2) 0.12415(15) 0.0545(10) Uani 1 1 d . . . N2 N -0.1850(7) 0.8085(3) 0.17530(19) 0.1002(17) Uani 1 1 d . . . C1 C 0.0753(6) 0.9872(3) 0.15208(17) 0.0529(12) Uani 1 1 d . . . C2 C -0.0377(6) 1.0587(3) 0.1492(2) 0.0636(13) Uani 1 1 d . . . C3 C 0.0163(8) 1.1371(3) 0.1763(2) 0.0810(16) Uani 1 1 d . . . H3 H -0.0550 1.1874 0.1754 0.097 Uiso 1 1 calc R . . C4 C 0.1745(10) 1.1388(4) 0.2039(2) 0.0871(18) Uani 1 1 d . . . H4 H 0.2096 1.1906 0.2218 0.105 Uiso 1 1 calc R . . C5 C 0.2811(7) 1.0665(4) 0.2059(2) 0.0784(16) Uani 1 1 d . . . H5 H 0.3878 1.0698 0.2249 0.094 Uiso 1 1 calc R . . C6 C 0.2346(6) 0.9892(3) 0.18053(18) 0.0602(12) Uani 1 1 d . . . C7 C -0.2121(7) 1.0528(4) 0.1196(2) 0.0986(18) Uani 1 1 d . . . H7A H -0.2720 1.1088 0.1221 0.118 Uiso 1 1 calc R . . H7B H -0.2832 1.0076 0.1366 0.118 Uiso 1 1 calc R . . H7C H -0.1926 1.0383 0.0812 0.118 Uiso 1 1 calc R . . C8 C 0.3544(7) 0.9087(3) 0.1837(2) 0.0971(18) Uani 1 1 d . . . H8A H 0.3021 0.8605 0.1634 0.116 Uiso 1 1 calc R . . H8B H 0.3698 0.8918 0.2218 0.116 Uiso 1 1 calc R . . H8C H 0.4672 0.9230 0.1677 0.116 Uiso 1 1 calc R . . C9 C 0.0881(6) 0.8890(3) 0.06900(19) 0.0590(12) Uani 1 1 d . . . C10 C 0.0741(5) 0.7987(3) 0.04598(18) 0.0501(11) Uani 1 1 d . . . C11 C 0.1050(6) 0.7233(3) 0.0773(2) 0.0668(13) Uani 1 1 d . . . H11 H 0.1230 0.7279 0.1155 0.080 Uiso 1 1 calc R . . C12 C 0.1091(6) 0.6416(3) 0.0520(3) 0.0772(15) Uani 1 1 d . . . H12 H 0.1310 0.5910 0.0731 0.093 Uiso 1 1 calc R . . C13 C 0.0810(7) 0.6342(4) -0.0041(3) 0.0875(18) Uani 1 1 d . . . H13 H 0.0832 0.5786 -0.0209 0.105 Uiso 1 1 calc R . . C14 C 0.0497(7) 0.7081(4) -0.0353(2) 0.0817(16) Uani 1 1 d . . . H14 H 0.0299 0.7027 -0.0734 0.098 Uiso 1 1 calc R . . C15 C 0.0472(6) 0.7907(3) -0.0108(2) 0.0672(13) Uani 1 1 d . . . H15 H 0.0275 0.8410 -0.0324 0.081 Uiso 1 1 calc R . . C16 C -0.0865(7) 0.8503(3) 0.1503(2) 0.0674(13) 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 O1 0.111(3) 0.059(2) 0.063(2) 0.0000(18) 0.013(2) -0.022(2) N1 0.064(2) 0.050(2) 0.050(2) -0.0012(19) 0.0062(19) -0.0152(19) N2 0.121(4) 0.090(3) 0.090(3) -0.011(3) 0.036(3) -0.037(3) C1 0.062(3) 0.049(3) 0.047(3) 0.000(2) 0.007(3) -0.012(2) C2 0.066(3) 0.063(3) 0.062(3) 0.010(3) 0.012(3) 0.003(3) C3 0.112(5) 0.051(3) 0.080(4) 0.006(3) 0.036(4) 0.008(3) C4 0.126(5) 0.070(4) 0.065(4) -0.011(3) 0.022(4) -0.033(4) C5 0.089(4) 0.090(4) 0.056(3) -0.009(3) -0.004(3) -0.019(4) C6 0.068(3) 0.066(3) 0.047(3) -0.006(3) -0.001(3) -0.011(3) C7 0.079(4) 0.100(4) 0.117(5) 0.024(4) 0.009(4) 0.014(3) C8 0.084(4) 0.102(4) 0.105(4) 0.004(4) -0.023(3) 0.004(4) C9 0.067(3) 0.059(3) 0.051(3) 0.001(2) -0.001(3) -0.012(3) C10 0.046(3) 0.052(3) 0.053(3) -0.001(2) 0.003(2) -0.006(2) C11 0.082(3) 0.058(3) 0.060(3) 0.000(3) 0.002(3) 0.001(3) C12 0.074(3) 0.054(3) 0.104(4) -0.004(3) 0.009(3) 0.010(3) C13 0.089(4) 0.070(4) 0.103(5) -0.038(4) 0.024(4) -0.012(3) C14 0.088(4) 0.086(4) 0.071(4) -0.017(4) -0.004(3) -0.020(3) C15 0.067(3) 0.073(4) 0.062(3) -0.001(3) -0.003(3) -0.010(3) C16 0.076(4) 0.071(4) 0.056(3) -0.013(3) 0.011(3) -0.009(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 O1 C9 1.203(4) . ? N1 C16 1.350(6) . ? N1 C9 1.417(5) . ? N1 C1 1.464(5) . ? N2 C16 1.146(5) . ? C1 C2 1.378(6) . ? C1 C6 1.387(6) . ? C2 C3 1.409(6) . ? C2 C7 1.502(6) . ? C3 C4 1.370(7) . ? C4 C5 1.356(7) . ? C5 C6 1.362(6) . ? C6 C8 1.516(6) . ? C9 C10 1.474(6) . ? C10 C11 1.383(6) . ? C10 C15 1.386(6) . ? C11 C12 1.375(6) . ? C12 C13 1.369(7) . ? C13 C14 1.364(7) . ? C14 C15 1.377(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 C16 N1 C9 123.0(4) . . ? C16 N1 C1 117.0(4) . . ? C9 N1 C1 119.4(3) . . ? C2 C1 C6 123.2(4) . . ? C2 C1 N1 120.0(4) . . ? C6 C1 N1 116.8(4) . . ? C1 C2 C3 116.9(5) . . ? C1 C2 C7 121.5(5) . . ? C3 C2 C7 121.5(5) . . ? C4 C3 C2 119.5(5) . . ? C5 C4 C3 121.5(5) . . ? C4 C5 C6 121.2(5) . . ? C5 C6 C1 117.6(5) . . ? C5 C6 C8 120.5(5) . . ? C1 C6 C8 121.8(4) . . ? O1 C9 N1 117.0(4) . . ? O1 C9 C10 124.4(4) . . ? N1 C9 C10 118.4(4) . . ? C11 C10 C15 119.4(5) . . ? C11 C10 C9 122.8(4) . . ? C15 C10 C9 117.4(4) . . ? C12 C11 C10 119.9(5) . . ? C13 C12 C11 120.4(5) . . ? C14 C13 C12 120.1(5) . . ? C13 C14 C15 120.4(5) . . ? C14 C15 C10 119.8(5) . . ? N2 C16 N1 175.6(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.172 _refine_diff_density_min -0.163 _refine_diff_density_rms 0.036 data_2s _database_code_CSD 184850 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H12 N2 O S' _chemical_formula_weight 256.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'Pc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 8.0852(18) _cell_length_b 11.637(2) _cell_length_c 14.389(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.825(17) _cell_angle_gamma 90.00 _cell_volume 1302.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 23 _cell_measurement_theta_min 4.83 _cell_measurement_theta_max 15.90 _exptl_crystal_description 'BLOCK ' _exptl_crystal_colour 'COLORLESS ' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.307 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 0.237 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.4043 _exptl_absorpt_correction_T_max 0.7974 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'MoK\a' _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2240 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0513 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2240 _reflns_number_gt 1275 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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^)+(0.1808P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.1(4) _refine_ls_number_reflns 2240 _refine_ls_number_parameters 325 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1323 _refine_ls_R_factor_gt 0.0824 _refine_ls_wR_factor_ref 0.2710 _refine_ls_wR_factor_gt 0.2218 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.556 _refine_ls_shift/su_mean 0.094 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 S1 S 0.0258(8) 0.5039(4) 0.3356(4) 0.1043(16) Uani 1 1 d . . . S2 S 0.0276(9) 0.0082(5) 0.5117(4) 0.120(2) Uani 1 1 d . . . O1 O 0.1499(15) 0.3597(9) 0.4989(8) 0.089(3) Uani 1 1 d . . . O2 O -0.0949(16) -0.1393(11) 0.3402(7) 0.093(4) Uani 1 1 d . . . N1 N 0.3578(16) 0.2681(9) 0.4590(7) 0.060(3) Uani 1 1 d . . . N2 N 0.392(2) 0.1414(13) 0.5978(12) 0.103(5) Uani 1 1 d . . . N3 N -0.3121(17) -0.2294(10) 0.3856(8) 0.064(3) Uani 1 1 d . . . N4 N -0.341(2) -0.3632(15) 0.2429(8) 0.098(5) Uani 1 1 d . . . C1 C 0.462(2) 0.2356(12) 0.3927(9) 0.068(4) Uani 1 1 d . . . C2 C 0.6353(18) 0.2662(11) 0.4189(8) 0.058(3) Uani 1 1 d . . . C3 C 0.736(2) 0.2249(13) 0.3576(11) 0.081(5) Uani 1 1 d . . . H3 H 0.8519 0.2443 0.3697 0.097 Uiso 1 1 calc R . . C4 C 0.665(2) 0.1628(17) 0.2881(13) 0.086(5) Uani 1 1 d . . . H4 H 0.7345 0.1340 0.2516 0.103 Uiso 1 1 calc R . . C5 C 0.491(4) 0.1310(13) 0.2585(11) 0.108(8) Uani 1 1 d . . . H5 H 0.4477 0.0870 0.2033 0.129 Uiso 1 1 calc R . . C6 C 0.387(2) 0.1663(13) 0.3126(8) 0.068(4) Uani 1 1 d . . . C7 C 0.721(2) 0.3395(13) 0.5011(10) 0.081(5) Uani 1 1 d . . . H7C H 0.6395 0.3616 0.5355 0.097 Uiso 1 1 calc R . . H7B H 0.7650 0.4070 0.4778 0.097 Uiso 1 1 calc R . . H7A H 0.8136 0.2979 0.5435 0.097 Uiso 1 1 calc R . . C8 C 0.193(3) 0.1411(16) 0.2877(11) 0.087(6) Uani 1 1 d . . . H8C H 0.1594 0.0954 0.2300 0.104 Uiso 1 1 calc R . . H8B H 0.1300 0.2122 0.2774 0.104 Uiso 1 1 calc R . . H8A H 0.1673 0.1001 0.3400 0.104 Uiso 1 1 calc R . . C9 C 0.3785(18) 0.2038(15) 0.5383(9) 0.072(4) Uani 1 1 d . . . C10 C 0.2356(16) 0.3579(10) 0.4448(8) 0.048(3) Uani 1 1 d . . . C11 C 0.212(2) 0.4350(11) 0.3655(10) 0.068(4) Uani 1 1 d . . . C12 C 0.3585(17) 0.4657(8) 0.3055(6) 0.043(3) Uani 1 1 d . . . H12 H 0.4696 0.4393 0.3118 0.051 Uiso 1 1 calc R . . C13 C 0.2393(18) 0.5563(8) 0.2337(7) 0.058(3) Uani 1 1 d . . . H13 H 0.2759 0.5944 0.1860 0.070 Uiso 1 1 calc R . . C14 C 0.073(2) 0.5747(15) 0.2477(12) 0.088(5) Uani 1 1 d . . . H14 H -0.0052 0.6249 0.2086 0.106 Uiso 1 1 calc R . . C15 C -0.4072(18) -0.2659(10) 0.4493(8) 0.050(3) Uani 1 1 d . . . C16 C -0.578(2) -0.2362(10) 0.4292(11) 0.069(4) Uani 1 1 d . . . C17 C -0.678(3) -0.2748(13) 0.4820(11) 0.084(5) Uani 1 1 d . . . H17 H -0.7956 -0.2610 0.4644 0.100 Uiso 1 1 calc R . . C18 C -0.589(4) -0.3436(14) 0.5742(11) 0.110(8) Uani 1 1 d . . . H18 H -0.6495 -0.3659 0.6177 0.132 Uiso 1 1 calc R . . C19 C -0.424(3) -0.3698(14) 0.5893(12) 0.082(5) Uani 1 1 d . . . H19 H -0.3718 -0.4173 0.6411 0.098 Uiso 1 1 calc R . . C20 C -0.324(2) -0.3286(10) 0.5304(10) 0.076(5) Uani 1 1 d . . . C21 C -0.656(2) -0.1627(13) 0.3362(10) 0.088(5) Uani 1 1 d . . . H21C H -0.7762 -0.1499 0.3293 0.105 Uiso 1 1 calc R . . H21B H -0.6424 -0.2030 0.2805 0.105 Uiso 1 1 calc R . . H21A H -0.5977 -0.0901 0.3417 0.105 Uiso 1 1 calc R . . C22 C -0.138(3) -0.3558(13) 0.5579(13) 0.100(7) Uani 1 1 d . . . H22C H -0.0862 -0.3227 0.5116 0.120 Uiso 1 1 calc R . . H22B H -0.1228 -0.4376 0.5593 0.120 Uiso 1 1 calc R . . H22A H -0.0849 -0.3246 0.6207 0.120 Uiso 1 1 calc R . . C23 C -0.325(2) -0.3008(12) 0.3065(11) 0.071(4) Uani 1 1 d . . . C24 C -0.187(2) -0.1484(15) 0.3975(10) 0.081(5) Uani 1 1 d . . . C25 C -0.1632(19) -0.0661(11) 0.4812(9) 0.061(4) Uani 1 1 d . . . C26 C -0.283(2) -0.0351(11) 0.5393(8) 0.053(4) Uani 1 1 d . . . H26 H -0.3932 -0.0621 0.5353 0.064 Uiso 1 1 calc R . . C27 C -0.211(4) 0.024(3) 0.584(2) 0.26(2) Uani 1 1 d . . . H27 H -0.2667 0.0519 0.6281 0.316 Uiso 1 1 calc R . . C28 C -0.032(3) 0.0781(11) 0.5980(11) 0.097(7) Uani 1 1 d . . . H28 H 0.0258 0.1335 0.6415 0.117 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 S1 0.106(4) 0.097(3) 0.101(3) 0.013(3) 0.013(3) 0.000(3) S2 0.122(5) 0.097(4) 0.138(4) 0.025(3) 0.028(4) -0.016(3) O1 0.072(8) 0.083(7) 0.108(8) 0.008(6) 0.017(7) -0.001(6) O2 0.094(9) 0.136(10) 0.064(5) 0.011(6) 0.048(6) -0.008(7) N1 0.072(8) 0.067(7) 0.047(5) -0.006(5) 0.028(5) -0.003(6) N2 0.117(13) 0.094(10) 0.108(10) 0.029(9) 0.048(10) -0.019(9) N3 0.067(8) 0.058(6) 0.066(6) -0.013(6) 0.015(6) 0.000(6) N4 0.094(10) 0.142(13) 0.056(6) -0.029(8) 0.016(7) 0.000(10) C1 0.099(14) 0.055(7) 0.054(7) 0.009(6) 0.028(8) -0.001(9) C2 0.057(8) 0.072(8) 0.041(5) 0.021(6) 0.006(5) 0.010(7) C3 0.096(13) 0.083(10) 0.086(10) -0.018(9) 0.062(10) -0.007(9) C4 0.082(11) 0.094(11) 0.094(10) -0.003(9) 0.046(9) -0.008(9) C5 0.22(3) 0.055(8) 0.049(7) 0.007(7) 0.038(12) 0.004(13) C6 0.089(11) 0.074(8) 0.041(6) -0.010(6) 0.019(7) -0.028(8) C7 0.087(11) 0.080(9) 0.093(10) 0.004(8) 0.055(9) 0.024(8) C8 0.098(14) 0.088(11) 0.062(8) 0.004(8) 0.002(9) -0.020(10) C9 0.056(8) 0.115(12) 0.042(6) 0.010(7) 0.008(6) -0.028(8) C10 0.043(6) 0.053(6) 0.058(6) -0.004(6) 0.030(6) 0.005(6) C11 0.091(11) 0.055(7) 0.067(8) -0.009(7) 0.038(8) 0.003(8) C12 0.073(7) 0.020(4) 0.036(5) 0.012(4) 0.016(5) 0.010(5) C13 0.091(9) 0.030(4) 0.042(5) 0.018(4) -0.002(5) 0.020(5) C14 0.085(12) 0.093(12) 0.082(10) 0.007(9) 0.017(9) 0.026(10) C15 0.066(9) 0.037(6) 0.046(6) 0.005(5) 0.016(6) 0.002(6) C16 0.108(13) 0.036(6) 0.085(9) 0.004(6) 0.065(9) -0.005(7) C17 0.086(11) 0.062(9) 0.098(11) -0.021(8) 0.017(9) -0.019(9) C18 0.22(3) 0.073(10) 0.058(8) 0.005(7) 0.079(13) -0.045(13) C19 0.104(14) 0.072(9) 0.077(10) 0.027(8) 0.037(10) -0.008(10) C20 0.115(15) 0.030(5) 0.073(8) -0.001(6) 0.009(9) -0.014(7) C21 0.076(10) 0.063(8) 0.096(10) 0.019(7) -0.023(8) 0.029(7) C22 0.127(18) 0.065(10) 0.098(12) 0.040(9) 0.015(12) 0.014(10) C23 0.086(11) 0.049(7) 0.091(10) 0.013(7) 0.045(9) 0.010(7) C24 0.084(11) 0.098(11) 0.054(8) 0.014(8) 0.010(8) 0.029(10) C25 0.068(10) 0.050(7) 0.059(7) 0.016(6) 0.007(7) -0.005(7) C26 0.086(10) 0.035(5) 0.034(6) -0.018(5) 0.008(6) -0.033(7) C27 0.26(3) 0.36(4) 0.27(3) 0.27(3) 0.24(3) 0.24(3) C28 0.16(2) 0.045(7) 0.068(9) 0.009(7) -0.005(11) 0.012(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C14 1.639(18) . ? S1 C11 1.657(18) . ? S2 C28 1.66(2) . ? S2 C25 1.717(16) . ? O1 C10 1.175(15) . ? O2 C24 1.259(19) . ? N1 C9 1.337(18) . ? N1 C10 1.415(16) . ? N1 C1 1.484(19) . ? N2 C9 1.105(18) . ? N3 C24 1.36(2) . ? N3 C23 1.39(2) . ? N3 C15 1.413(18) . ? N4 C23 1.147(18) . ? C1 C2 1.39(2) . ? C1 C6 1.401(19) . ? C2 C3 1.438(18) . ? C2 C7 1.47(2) . ? C3 C4 1.24(2) . ? C4 C5 1.41(3) . ? C5 C6 1.35(3) . ? C6 C8 1.54(3) . ? C10 C11 1.423(17) . ? C11 C12 1.682(18) . ? C12 C13 1.602(12) . ? C13 C14 1.43(2) . ? C15 C16 1.37(2) . ? C15 C20 1.385(18) . ? C16 C17 1.33(2) . ? C16 C21 1.570(19) . ? C17 C18 1.55(3) . ? C18 C19 1.33(3) . ? C19 C20 1.40(2) . ? C20 C22 1.48(3) . ? C24 C25 1.51(2) . ? C25 C26 1.49(2) . ? C25 C27 1.94(4) . ? C26 C27 1.01(5) . ? C27 C28 1.55(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 C14 S1 C11 93.2(9) . . ? C28 S2 C25 90.9(11) . . ? C9 N1 C10 117.1(11) . . ? C9 N1 C1 116.5(12) . . ? C10 N1 C1 126.3(10) . . ? C24 N3 C23 113.9(13) . . ? C24 N3 C15 130.1(12) . . ? C23 N3 C15 114.9(11) . . ? C2 C1 C6 123.1(14) . . ? C2 C1 N1 117.8(12) . . ? C6 C1 N1 118.8(15) . . ? C1 C2 C3 116.5(13) . . ? C1 C2 C7 125.7(13) . . ? C3 C2 C7 117.8(13) . . ? C4 C3 C2 118.1(16) . . ? C3 C4 C5 127.2(17) . . ? C6 C5 C4 118.2(15) . . ? C5 C6 C1 116.8(17) . . ? C5 C6 C8 124.0(15) . . ? C1 C6 C8 119.0(15) . . ? N2 C9 N1 172.9(17) . . ? O1 C10 N1 115.6(12) . . ? O1 C10 C11 123.2(12) . . ? N1 C10 C11 121.1(11) . . ? C10 C11 S1 115.2(10) . . ? C10 C11 C12 125.9(12) . . ? S1 C11 C12 118.8(9) . . ? C13 C12 C11 95.0(10) . . ? C14 C13 C12 115.5(11) . . ? C13 C14 S1 117.4(12) . . ? C16 C15 C20 122.5(13) . . ? C16 C15 N3 118.8(11) . . ? C20 C15 N3 118.7(13) . . ? C17 C16 C15 121.8(14) . . ? C17 C16 C21 120.3(16) . . ? C15 C16 C21 117.6(12) . . ? C16 C17 C18 116.9(18) . . ? C19 C18 C17 118.0(15) . . ? C18 C19 C20 122.6(16) . . ? C15 C20 C19 117.6(17) . . ? C15 C20 C22 124.1(15) . . ? C19 C20 C22 118.3(15) . . ? N4 C23 N3 176.5(17) . . ? O2 C24 N3 121.9(15) . . ? O2 C24 C25 119.9(17) . . ? N3 C24 C25 118.2(14) . . ? C26 C25 C24 129.8(13) . . ? C26 C25 S2 114.4(9) . . ? C24 C25 S2 115.8(12) . . ? C26 C25 C27 30.8(13) . . ? C24 C25 C27 160.6(17) . . ? S2 C25 C27 83.5(13) . . ? C27 C26 C25 99.9(19) . . ? C26 C27 C28 136(2) . . ? C26 C27 C25 49.2(18) . . ? C28 C27 C25 86.7(11) . . ? C27 C28 S2 98.9(16) . . ? _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.908 _refine_diff_density_max 0.476 _refine_diff_density_min -0.433 _refine_diff_density_rms 0.076 data_ptmix _database_code_CSD 184851 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H36 N6 P2 Pt' _chemical_formula_weight 665.62 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' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P2(1) ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.066(2) _cell_length_b 11.776(2) _cell_length_c 13.601(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.916(16) _cell_angle_gamma 90.00 _cell_volume 1373.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 26 _cell_measurement_theta_min 4.87 _cell_measurement_theta_max 12.50 _cell_measurement_temperature 293(2) _exptl_crystal_description 'CUBE ' _exptl_crystal_colour 'COLORLESS ' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.609 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 660 _exptl_absorpt_coefficient_mu 5.246 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.5818 _exptl_absorpt_correction_T_max 0.8734 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2702 _diffrn_reflns_av_R_equivalents 0.0236 _diffrn_reflns_av_sigmaI/netI 0.0414 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2538 _reflns_number_gt 2352 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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^)+(0.0249P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0020(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.004(10) _refine_ls_number_reflns 2538 _refine_ls_number_parameters 299 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0283 _refine_ls_R_factor_gt 0.0238 _refine_ls_wR_factor_ref 0.0566 _refine_ls_wR_factor_gt 0.0547 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 Pt1 Pt 0.30532(3) 0.25259(5) 0.163291(18) 0.03872(10) Uani 1 1 d . . . P1 P 0.0823(3) 0.3605(2) 0.13138(19) 0.0454(5) Uani 1 1 d . . . P2 P 0.5124(4) 0.1326(3) 0.1742(3) 0.0548(7) Uani 1 1 d . . . N1 N 0.1668(10) 0.1152(7) 0.1557(6) 0.056(2) Uani 1 1 d . . . N2 N 0.0141(13) -0.0306(9) 0.1975(7) 0.099(4) Uani 1 1 d . . . N3 N 0.5517(9) 0.3944(7) 0.1268(8) 0.061(2) Uani 1 1 d . . . N4 N 0.6498(9) 0.4848(7) 0.1721(8) 0.067(2) Uani 1 1 d . . . N5 N 0.6143(9) 0.5259(7) 0.2504(7) 0.066(2) Uani 1 1 d . . . N6 N 0.4901(8) 0.4629(6) 0.2570(6) 0.0499(18) Uani 1 1 d . . . C1 C 0.0829(11) 0.5044(9) 0.0818(8) 0.071(3) Uani 1 1 d . . . H1A H 0.1676 0.5465 0.1284 0.085 Uiso 1 1 calc R . . H1B H -0.0139 0.5411 0.0765 0.085 Uiso 1 1 calc R . . H1C H 0.0954 0.5013 0.0144 0.085 Uiso 1 1 calc R . . C2 C -0.0824(10) 0.2992(9) 0.0332(8) 0.069(3) Uani 1 1 d . . . H2A H -0.0574 0.2887 -0.0296 0.083 Uiso 1 1 calc R . . H2B H -0.1704 0.3491 0.0199 0.083 Uiso 1 1 calc R . . H2C H -0.1072 0.2272 0.0569 0.083 Uiso 1 1 calc R . . C3 C 0.0186(10) 0.3747(11) 0.2440(7) 0.070(3) Uani 1 1 d . . . H3A H 0.1010 0.4074 0.3003 0.084 Uiso 1 1 calc R . . H3B H -0.0074 0.3012 0.2641 0.084 Uiso 1 1 calc R . . H3C H -0.0714 0.4230 0.2272 0.084 Uiso 1 1 calc R . . C4 C 0.4858(17) -0.0132(10) 0.2097(14) 0.110(6) Uani 1 1 d . . . H4A H 0.4671 -0.0140 0.2752 0.132 Uiso 1 1 calc R . . H4B H 0.5780 -0.0564 0.2152 0.132 Uiso 1 1 calc R . . H4C H 0.3982 -0.0461 0.1573 0.132 Uiso 1 1 calc R . . C5 C 0.5458(14) 0.1241(12) 0.0509(9) 0.092(4) Uani 1 1 d . . . H5A H 0.4499 0.1058 -0.0026 0.110 Uiso 1 1 calc R . . H5B H 0.6215 0.0661 0.0539 0.110 Uiso 1 1 calc R . . H5C H 0.5838 0.1958 0.0356 0.110 Uiso 1 1 calc R . . C6 C 0.6998(11) 0.1667(10) 0.2670(8) 0.077(3) Uani 1 1 d . . . H6A H 0.6905 0.1724 0.3351 0.093 Uiso 1 1 calc R . . H6B H 0.7356 0.2378 0.2486 0.093 Uiso 1 1 calc R . . H6C H 0.7731 0.1080 0.2666 0.093 Uiso 1 1 calc R . . C7 C 0.4538(11) 0.3831(9) 0.1819(8) 0.043(2) Uani 1 1 d . . . C8 C 0.4150(8) 0.4986(7) 0.3296(6) 0.050(2) Uani 1 1 d . . . C9 C 0.4122(10) 0.4262(8) 0.4085(6) 0.057(2) Uani 1 1 d . . . C10 C 0.3262(12) 0.4613(11) 0.4728(8) 0.075(3) Uani 1 1 d . . . H10 H 0.3207 0.4143 0.5264 0.090 Uiso 1 1 calc R . . C11 C 0.2521(14) 0.5619(12) 0.4577(9) 0.086(4) Uani 1 1 d . . . H11 H 0.1926 0.5815 0.4995 0.103 Uiso 1 1 calc R . . C12 C 0.2618(12) 0.6367(10) 0.3823(10) 0.082(3) Uani 1 1 d . . . H12 H 0.2121 0.7068 0.3747 0.099 Uiso 1 1 calc R . . C13 C 0.3465(10) 0.6068(8) 0.3176(7) 0.060(2) Uani 1 1 d . . . C14 C 0.4911(13) 0.3145(9) 0.4274(8) 0.077(3) Uani 1 1 d . . . H14A H 0.4737 0.2787 0.4861 0.092 Uiso 1 1 calc R . . H14B H 0.6010 0.3249 0.4412 0.092 Uiso 1 1 calc R . . H14C H 0.4499 0.2673 0.3671 0.092 Uiso 1 1 calc R . . C15 C 0.3657(12) 0.6931(9) 0.2382(10) 0.090(4) Uani 1 1 d . . . H15A H 0.4262 0.6599 0.1994 0.108 Uiso 1 1 calc R . . H15B H 0.4179 0.7594 0.2740 0.108 Uiso 1 1 calc R . . H15C H 0.2649 0.7140 0.1917 0.108 Uiso 1 1 calc R . . C16 C 0.0989(11) 0.0457(8) 0.1856(7) 0.056(2) Uani 1 1 d . . . C17 C 0.0053(10) -0.0828(8) 0.2874(7) 0.055(2) Uani 1 1 d . . . C18 C -0.0964(11) -0.1764(8) 0.2719(9) 0.063(2) Uani 1 1 d . . . C19 C -0.1147(13) -0.2305(12) 0.3555(10) 0.079(4) Uani 1 1 d . . . H19 H -0.1804 -0.2931 0.3454 0.095 Uiso 1 1 calc R . . C20 C -0.0378(16) -0.1940(12) 0.4538(12) 0.098(4) Uani 1 1 d . . . H20 H -0.0529 -0.2317 0.5099 0.117 Uiso 1 1 calc R . . C21 C 0.0607(13) -0.1035(11) 0.4716(8) 0.074(3) Uani 1 1 d . . . H21 H 0.1110 -0.0793 0.5393 0.089 Uiso 1 1 calc R . . C22 C 0.0864(10) -0.0469(9) 0.3881(7) 0.059(2) Uani 1 1 d . . . C23 C -0.1811(14) -0.2180(11) 0.1640(9) 0.098(5) Uani 1 1 d . . . H23A H -0.1554 -0.1706 0.1145 0.117 Uiso 1 1 calc R . . H23B H -0.2915 -0.2151 0.1517 0.117 Uiso 1 1 calc R . . H23C H -0.1506 -0.2948 0.1569 0.117 Uiso 1 1 calc R . . C24 C 0.1991(14) 0.0524(10) 0.4096(8) 0.080(3) Uani 1 1 d . . . H24A H 0.2431 0.0637 0.4833 0.096 Uiso 1 1 calc R . . H24B H 0.1446 0.1198 0.3779 0.096 Uiso 1 1 calc R . . H24C H 0.2811 0.0366 0.3812 0.096 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.03549(14) 0.03502(13) 0.04675(14) 0.0013(3) 0.01485(9) -0.0047(2) P1 0.0343(11) 0.0484(13) 0.0493(12) -0.0033(10) 0.0078(10) -0.0025(11) P2 0.0532(16) 0.0419(15) 0.0753(17) 0.0056(14) 0.0291(14) 0.0053(14) N1 0.056(5) 0.047(5) 0.063(5) 0.001(4) 0.015(4) -0.017(4) N2 0.130(8) 0.102(8) 0.062(5) -0.003(5) 0.025(5) -0.076(7) N3 0.055(5) 0.058(5) 0.079(6) 0.022(5) 0.035(4) 0.007(4) N4 0.051(4) 0.051(5) 0.101(6) 0.021(5) 0.029(4) -0.005(4) N5 0.042(4) 0.048(4) 0.102(6) 0.013(4) 0.014(4) -0.018(4) N6 0.033(3) 0.039(4) 0.077(5) 0.005(4) 0.017(3) -0.013(3) C1 0.060(5) 0.060(6) 0.074(6) 0.015(5) -0.004(5) 0.009(5) C2 0.049(5) 0.074(6) 0.071(6) -0.007(5) 0.001(5) 0.000(4) C3 0.045(5) 0.103(9) 0.066(6) -0.005(6) 0.022(4) 0.006(5) C4 0.106(11) 0.049(7) 0.211(18) 0.040(9) 0.101(12) 0.028(7) C5 0.096(9) 0.103(10) 0.095(8) -0.019(8) 0.056(7) 0.029(8) C6 0.059(6) 0.079(7) 0.087(7) 0.013(6) 0.014(5) 0.017(5) C7 0.037(5) 0.036(5) 0.054(5) 0.011(4) 0.011(4) 0.003(4) C8 0.033(4) 0.047(5) 0.059(5) -0.008(4) 0.001(3) -0.013(4) C9 0.048(5) 0.060(5) 0.049(4) -0.003(4) 0.000(4) -0.015(4) C10 0.073(7) 0.086(8) 0.066(6) -0.016(6) 0.023(5) -0.013(6) C11 0.088(8) 0.097(10) 0.075(7) -0.042(7) 0.029(6) -0.012(7) C12 0.062(6) 0.068(7) 0.104(8) -0.037(7) 0.007(6) 0.007(6) C13 0.052(5) 0.044(5) 0.071(5) -0.014(4) 0.002(4) -0.007(4) C14 0.079(7) 0.084(7) 0.054(5) 0.022(5) 0.004(5) -0.002(6) C15 0.057(6) 0.051(6) 0.137(10) -0.008(7) -0.002(6) 0.001(5) C16 0.059(5) 0.047(5) 0.056(5) -0.003(4) 0.009(4) -0.021(5) C17 0.055(5) 0.051(5) 0.064(5) 0.006(4) 0.025(4) -0.002(4) C18 0.061(5) 0.047(5) 0.093(7) -0.003(5) 0.043(5) -0.012(4) C19 0.082(6) 0.061(11) 0.112(8) 0.011(7) 0.057(6) -0.006(6) C20 0.106(10) 0.099(9) 0.106(10) 0.024(8) 0.058(8) -0.015(8) C21 0.081(7) 0.087(8) 0.062(6) 0.004(5) 0.035(5) 0.012(7) C22 0.057(5) 0.056(5) 0.067(5) -0.007(5) 0.023(4) 0.008(4) C23 0.116(10) 0.076(10) 0.104(9) -0.017(6) 0.039(8) -0.052(7) C24 0.085(7) 0.076(7) 0.067(6) -0.014(6) 0.008(6) -0.015(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 Pt1 C7 2.005(11) . ? Pt1 N1 2.031(8) . ? Pt1 P1 2.307(2) . ? Pt1 P2 2.316(3) . ? P1 C2 1.800(9) . ? P1 C3 1.811(9) . ? P1 C1 1.825(10) . ? P2 C5 1.801(11) . ? P2 C6 1.802(10) . ? P2 C4 1.821(12) . ? N1 C16 1.173(11) . ? N2 C16 1.226(12) . ? N2 C17 1.393(12) . ? N3 C7 1.342(13) . ? N3 N4 1.396(11) . ? N4 N5 1.301(12) . ? N5 N6 1.375(10) . ? N6 C7 1.348(13) . ? N6 C8 1.432(12) . ? C8 C9 1.377(12) . ? C8 C13 1.403(12) . ? C9 C10 1.409(14) . ? C9 C14 1.481(14) . ? C10 C11 1.344(17) . ? C11 C12 1.377(17) . ? C12 C13 1.387(15) . ? C13 C15 1.534(15) . ? C17 C22 1.394(13) . ? C17 C18 1.408(12) . ? C18 C19 1.360(15) . ? C18 C23 1.500(14) . ? C19 C20 1.362(17) . ? C20 C21 1.361(17) . ? C21 C22 1.400(14) . ? C22 C24 1.517(14) . ? 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 C7 Pt1 N1 175.3(4) . . ? C7 Pt1 P1 96.5(3) . . ? N1 Pt1 P1 86.5(3) . . ? C7 Pt1 P2 87.8(3) . . ? N1 Pt1 P2 89.6(3) . . ? P1 Pt1 P2 172.33(11) . . ? C2 P1 C3 104.4(5) . . ? C2 P1 C1 101.5(5) . . ? C3 P1 C1 105.5(6) . . ? C2 P1 Pt1 112.6(4) . . ? C3 P1 Pt1 113.1(3) . . ? C1 P1 Pt1 118.3(4) . . ? C5 P2 C6 105.0(6) . . ? C5 P2 C4 105.7(7) . . ? C6 P2 C4 101.5(7) . . ? C5 P2 Pt1 110.6(4) . . ? C6 P2 Pt1 118.0(4) . . ? C4 P2 Pt1 114.7(4) . . ? C16 N1 Pt1 157.5(8) . . ? C16 N2 C17 131.0(9) . . ? C7 N3 N4 105.7(9) . . ? N5 N4 N3 110.7(7) . . ? N4 N5 N6 106.2(8) . . ? C7 N6 N5 109.2(8) . . ? C7 N6 C8 132.3(7) . . ? N5 N6 C8 118.0(8) . . ? N3 C7 N6 108.2(9) . . ? N3 C7 Pt1 123.0(8) . . ? N6 C7 Pt1 128.3(7) . . ? C9 C8 C13 122.2(9) . . ? C9 C8 N6 119.2(8) . . ? C13 C8 N6 118.5(8) . . ? C8 C9 C10 117.1(10) . . ? C8 C9 C14 123.7(9) . . ? C10 C9 C14 119.1(10) . . ? C11 C10 C9 120.9(12) . . ? C10 C11 C12 121.8(11) . . ? C11 C12 C13 119.5(11) . . ? C12 C13 C8 118.2(10) . . ? C12 C13 C15 119.3(10) . . ? C8 C13 C15 122.5(9) . . ? N1 C16 N2 168.0(10) . . ? N2 C17 C22 124.5(9) . . ? N2 C17 C18 115.8(8) . . ? C22 C17 C18 119.7(9) . . ? C19 C18 C17 119.5(10) . . ? C19 C18 C23 120.2(9) . . ? C17 C18 C23 120.3(9) . . ? C18 C19 C20 120.8(12) . . ? C21 C20 C19 121.3(12) . . ? C20 C21 C22 120.1(11) . . ? C17 C22 C21 118.6(9) . . ? C17 C22 C24 122.1(9) . . ? C21 C22 C24 119.3(9) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.466 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.083 data_2ni _database_code_CSD 184852 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H48 N4 Ni P2' _chemical_formula_weight 585.37 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' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Orthorhombic' _symmetry_space_group_name_H-M 'Pbca ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 9.3848(18) _cell_length_b 14.465(2) _cell_length_c 24.050(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3264.7(9) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 6.19 _cell_measurement_theta_max 12.49 _exptl_crystal_description 'BLOCK ' _exptl_crystal_colour 'RED ' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.191 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 0.716 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.5781 _exptl_absorpt_correction_T_max 0.8720 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'MoK\a' _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2862 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0799 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2862 _reflns_number_gt 1609 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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^)+(0.0648P)^2^+0.1898P] 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 0.0004(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2862 _refine_ls_number_parameters 170 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1170 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1469 _refine_ls_wR_factor_gt 0.1198 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _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 Ni1 Ni 0.0000 0.5000 0.0000 0.0399(2) Uani 1 2 d S . . P1 P -0.15505(13) 0.56003(8) 0.05999(4) 0.0444(3) Uani 1 1 d . . . N1 N 0.1409(4) 0.5271(3) 0.05074(14) 0.0543(11) Uani 1 1 d . . . N2 N 0.2311(4) 0.5219(3) 0.14566(14) 0.0513(11) Uani 1 1 d . . . C1 C -0.1630(6) 0.4991(3) 0.12584(18) 0.0597(13) Uani 1 1 d . . . H1A H -0.0703 0.5025 0.1435 0.072 Uiso 1 1 calc R . . H1B H -0.2307 0.5303 0.1499 0.072 Uiso 1 1 calc R . . C2 C -0.2059(7) 0.3983(4) 0.1208(3) 0.094(2) Uani 1 1 d . . . H2A H -0.2078 0.3706 0.1570 0.112 Uiso 1 1 calc R . . H2B H -0.1382 0.3664 0.0978 0.112 Uiso 1 1 calc R . . H2C H -0.2988 0.3942 0.1042 0.112 Uiso 1 1 calc R . . C3 C -0.3379(5) 0.5671(4) 0.03543(18) 0.0613(14) Uani 1 1 d . . . H3A H -0.3391 0.6051 0.0022 0.074 Uiso 1 1 calc R . . H3B H -0.3682 0.5055 0.0247 0.074 Uiso 1 1 calc R . . C4 C -0.4469(6) 0.6059(4) 0.0760(2) 0.0845(19) Uani 1 1 d . . . H4A H -0.5391 0.6065 0.0588 0.101 Uiso 1 1 calc R . . H4B H -0.4205 0.6678 0.0861 0.101 Uiso 1 1 calc R . . H4C H -0.4497 0.5680 0.1087 0.101 Uiso 1 1 calc R . . C5 C -0.1040(6) 0.6761(3) 0.0809(2) 0.0686(16) Uani 1 1 d . . . H5A H -0.1791 0.7020 0.1038 0.082 Uiso 1 1 calc R . . H5B H -0.0185 0.6724 0.1035 0.082 Uiso 1 1 calc R . . C6 C -0.0765(7) 0.7406(4) 0.0324(3) 0.108(2) Uani 1 1 d . . . H6A H -0.0500 0.8004 0.0462 0.129 Uiso 1 1 calc R . . H6B H -0.1614 0.7459 0.0104 0.129 Uiso 1 1 calc R . . H6C H -0.0008 0.7162 0.0100 0.129 Uiso 1 1 calc R . . C7 C 0.1857(5) 0.5181(3) 0.09613(19) 0.0470(12) Uani 1 1 d . . . C8 C 0.3254(5) 0.4601(3) 0.17151(16) 0.0453(11) Uani 1 1 d . . . C9 C 0.4187(5) 0.4981(4) 0.21117(17) 0.0525(12) Uani 1 1 d . . . C10 C 0.5122(6) 0.4406(5) 0.23905(19) 0.0706(16) Uani 1 1 d . . . H10 H 0.5747 0.4657 0.2650 0.085 Uiso 1 1 calc R . . C11 C 0.5145(6) 0.3478(5) 0.2293(2) 0.0798(18) Uani 1 1 d . . . H11 H 0.5804 0.3104 0.2475 0.096 Uiso 1 1 calc R . . C12 C 0.4186(6) 0.3097(4) 0.1924(2) 0.0737(17) Uani 1 1 d . . . H12 H 0.4181 0.2461 0.1869 0.088 Uiso 1 1 calc R . . C13 C 0.3222(5) 0.3646(4) 0.16303(17) 0.0534(13) Uani 1 1 d . . . C14 C 0.4141(6) 0.5990(4) 0.2238(2) 0.0756(17) Uani 1 1 d . . . H14A H 0.3443 0.6282 0.2005 0.091 Uiso 1 1 calc R . . H14B H 0.5060 0.6257 0.2168 0.091 Uiso 1 1 calc R . . H14C H 0.3891 0.6079 0.2621 0.091 Uiso 1 1 calc R . . C15 C 0.2176(6) 0.3202(4) 0.1240(2) 0.0743(17) Uani 1 1 d . . . H15A H 0.1594 0.3671 0.1072 0.089 Uiso 1 1 calc R . . H15B H 0.1583 0.2780 0.1444 0.089 Uiso 1 1 calc R . . H15C H 0.2683 0.2872 0.0956 0.089 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 Ni1 0.0382(4) 0.0522(4) 0.0293(4) 0.0006(4) -0.0033(4) 0.0027(5) P1 0.0441(7) 0.0515(7) 0.0376(6) -0.0026(6) 0.0023(6) 0.0002(7) N1 0.041(2) 0.084(3) 0.038(2) -0.0084(19) -0.0088(18) 0.009(2) N2 0.048(2) 0.071(3) 0.0346(19) -0.0003(19) -0.0105(19) 0.002(2) C1 0.054(3) 0.081(4) 0.044(3) 0.006(3) 0.004(2) -0.005(3) C2 0.098(5) 0.087(5) 0.096(4) 0.030(4) 0.001(4) -0.019(4) C3 0.042(3) 0.089(4) 0.053(3) 0.001(3) 0.000(3) 0.010(3) C4 0.063(4) 0.114(5) 0.077(4) 0.005(4) 0.016(3) 0.016(4) C5 0.070(4) 0.056(3) 0.080(4) -0.015(3) 0.011(3) -0.008(3) C6 0.137(6) 0.065(4) 0.121(5) -0.003(4) 0.058(5) -0.017(4) C7 0.031(2) 0.061(3) 0.050(3) -0.005(2) -0.001(2) -0.003(2) C8 0.041(3) 0.064(3) 0.030(2) 0.002(2) 0.000(2) -0.003(3) C9 0.047(3) 0.075(3) 0.035(2) 0.002(3) -0.003(2) -0.001(3) C10 0.062(4) 0.110(5) 0.039(3) -0.003(3) -0.011(3) 0.012(4) C11 0.076(4) 0.105(5) 0.058(3) 0.002(3) -0.014(3) 0.038(4) C12 0.089(5) 0.076(4) 0.056(3) 0.010(3) 0.012(3) 0.021(4) C13 0.060(3) 0.062(3) 0.039(2) 0.000(2) 0.003(2) -0.003(3) C14 0.088(5) 0.080(4) 0.059(3) -0.009(3) -0.017(3) -0.016(4) C15 0.101(5) 0.063(3) 0.060(3) 0.006(3) -0.013(3) -0.015(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 Ni1 N1 1.841(4) 5_565 ? Ni1 N1 1.841(4) . ? Ni1 P1 2.2255(12) 5_565 ? Ni1 P1 2.2255(12) . ? P1 C1 1.814(4) . ? P1 C5 1.817(5) . ? P1 C3 1.817(5) . ? N1 C7 1.177(5) . ? N2 C7 1.266(5) . ? N2 C8 1.404(5) . ? C1 C2 1.517(7) . ? C3 C4 1.521(6) . ? C5 C6 1.516(7) . ? C8 C13 1.396(7) . ? C8 C9 1.407(6) . ? C9 C10 1.382(7) . ? C9 C14 1.491(6) . ? C10 C11 1.363(8) . ? C11 C12 1.380(7) . ? C12 C13 1.395(7) . ? C13 C15 1.502(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 N1 Ni1 N1 180.00(15) 5_565 . ? N1 Ni1 P1 87.53(12) 5_565 5_565 ? N1 Ni1 P1 92.47(12) . 5_565 ? N1 Ni1 P1 92.47(12) 5_565 . ? N1 Ni1 P1 87.53(12) . . ? P1 Ni1 P1 180.00(6) 5_565 . ? C1 P1 C5 102.6(2) . . ? C1 P1 C3 105.8(2) . . ? C5 P1 C3 106.7(3) . . ? C1 P1 Ni1 113.80(17) . . ? C5 P1 Ni1 111.58(18) . . ? C3 P1 Ni1 115.38(15) . . ? C7 N1 Ni1 148.0(4) . . ? C7 N2 C8 126.9(4) . . ? C2 C1 P1 114.0(4) . . ? C4 C3 P1 116.6(3) . . ? C6 C5 P1 113.6(4) . . ? N1 C7 N2 171.1(5) . . ? C13 C8 N2 123.5(4) . . ? C13 C8 C9 119.9(4) . . ? N2 C8 C9 116.4(4) . . ? C10 C9 C8 119.3(5) . . ? C10 C9 C14 120.6(5) . . ? C8 C9 C14 120.1(5) . . ? C11 C10 C9 121.4(5) . . ? C10 C11 C12 119.5(5) . . ? C11 C12 C13 121.4(5) . . ? C12 C13 C8 118.4(5) . . ? C12 C13 C15 119.7(5) . . ? C8 C13 C15 121.9(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.345 _refine_diff_density_min -0.273 _refine_diff_density_rms 0.062 data_ptncr2 _database_code_CSD 184853 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H48 N4 P2 Pt' _chemical_formula_weight 721.75 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' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Orthorhombic' _symmetry_space_group_name_H-M 'Pbca ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 9.4547(8) _cell_length_b 14.3442(15) _cell_length_c 24.230(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3286.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 4.86 _cell_measurement_theta_max 14.33 _exptl_crystal_description 'BLOCK ' _exptl_crystal_colour 'COLORLESS ' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 4.391 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.1708 _exptl_absorpt_correction_T_max 0.6429 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'MoK\a' _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2839 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2839 _reflns_number_gt 1750 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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^)+(0.0472P)^2^+6.6260P] 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 0.00016(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2839 _refine_ls_number_parameters 170 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0609 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.1088 _refine_ls_wR_factor_gt 0.0897 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 Pt1 Pt 0.0000 0.0000 0.0000 0.04183(15) Uani 1 2 d S . . P1 P 0.15820(19) -0.06419(10) 0.06188(6) 0.0513(4) Uani 1 1 d . . . N1 N -0.1567(5) -0.0382(4) 0.0518(2) 0.0562(12) Uani 1 1 d . . . N2 N -0.2314(6) -0.0296(4) 0.1472(2) 0.0596(14) Uani 1 1 d . . . C1 C 0.1613(9) -0.0044(4) 0.1278(3) 0.0649(19) Uani 1 1 d . . . H1A H 0.0675 -0.0074 0.1440 0.078 Uiso 1 1 calc R . . H1B H 0.2254 -0.0371 0.1523 0.078 Uiso 1 1 calc R . . C2 C 0.2060(9) 0.0961(5) 0.1245(3) 0.092(3) Uani 1 1 d . . . H2A H 0.2046 0.1231 0.1608 0.110 Uiso 1 1 calc R . . H2B H 0.1420 0.1296 0.1010 0.110 Uiso 1 1 calc R . . H2C H 0.3000 0.0998 0.1097 0.110 Uiso 1 1 calc R . . C3 C 0.1074(9) -0.1817(4) 0.0811(3) 0.077(2) Uani 1 1 d . . . H3A H 0.1787 -0.2071 0.1057 0.092 Uiso 1 1 calc R . . H3B H 0.0189 -0.1791 0.1013 0.092 Uiso 1 1 calc R . . C4 C 0.0898(12) -0.2469(5) 0.0325(4) 0.127(4) Uani 1 1 d . . . H4A H 0.0620 -0.3074 0.0456 0.152 Uiso 1 1 calc R . . H4B H 0.1778 -0.2518 0.0130 0.152 Uiso 1 1 calc R . . H4C H 0.0183 -0.2230 0.0082 0.152 Uiso 1 1 calc R . . C5 C 0.3407(7) -0.0684(5) 0.0375(3) 0.0683(18) Uani 1 1 d . . . H5A H 0.3432 -0.1054 0.0039 0.082 Uiso 1 1 calc R . . H5B H 0.3695 -0.0056 0.0278 0.082 Uiso 1 1 calc R . . C6 C 0.4487(9) -0.1080(6) 0.0775(3) 0.094(3) Uani 1 1 d . . . H6A H 0.5407 -0.1069 0.0607 0.112 Uiso 1 1 calc R . . H6B H 0.4239 -0.1711 0.0865 0.112 Uiso 1 1 calc R . . H6C H 0.4499 -0.0710 0.1105 0.112 Uiso 1 1 calc R . . C7 C -0.1924(7) -0.0269(5) 0.0979(3) 0.0538(16) Uani 1 1 d . . . C8 C -0.3272(7) 0.0347(4) 0.1729(2) 0.0531(15) Uani 1 1 d . . . C9 C -0.4192(8) -0.0026(4) 0.2116(3) 0.0603(18) Uani 1 1 d . . . C10 C -0.5101(8) 0.0577(6) 0.2390(3) 0.078(2) Uani 1 1 d . . . H10 H -0.5732 0.0336 0.2648 0.093 Uiso 1 1 calc R . . C11 C -0.5092(9) 0.1514(7) 0.2292(3) 0.087(3) Uani 1 1 d . . . H11 H -0.5722 0.1904 0.2474 0.104 Uiso 1 1 calc R . . C12 C -0.4137(9) 0.1873(5) 0.1918(3) 0.076(2) Uani 1 1 d . . . H12 H -0.4117 0.2514 0.1858 0.092 Uiso 1 1 calc R . . C13 C -0.3206(9) 0.1307(4) 0.1630(2) 0.0664(19) Uani 1 1 d . . . C14 C -0.4170(10) -0.1044(5) 0.2243(3) 0.084(2) Uani 1 1 d . . . H14A H -0.4872 -0.1181 0.2518 0.101 Uiso 1 1 calc R . . H14B H -0.3253 -0.1215 0.2380 0.101 Uiso 1 1 calc R . . H14C H -0.4372 -0.1392 0.1914 0.101 Uiso 1 1 calc R . . C15 C -0.2160(9) 0.1735(5) 0.1247(3) 0.091(3) Uani 1 1 d . . . H15A H -0.1604 0.1254 0.1078 0.109 Uiso 1 1 calc R . . H15B H -0.1552 0.2147 0.1450 0.109 Uiso 1 1 calc R . . H15C H -0.2650 0.2080 0.0967 0.109 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0408(2) 0.0541(2) 0.0306(2) -0.00076(13) 0.00252(14) 0.00113(15) P1 0.0599(9) 0.0557(8) 0.0384(7) 0.0018(7) -0.0017(9) 0.0002(9) N1 0.041(3) 0.080(3) 0.047(3) 0.007(3) 0.010(3) 0.008(3) N2 0.068(4) 0.076(3) 0.035(3) 0.003(3) 0.008(3) 0.001(3) C1 0.077(5) 0.077(5) 0.040(4) -0.002(3) -0.005(4) -0.007(4) C2 0.120(8) 0.086(5) 0.070(5) -0.017(4) -0.005(5) -0.021(5) C3 0.096(6) 0.060(4) 0.075(5) 0.021(4) -0.016(4) -0.005(4) C4 0.196(11) 0.059(5) 0.124(8) 0.007(5) -0.081(8) -0.011(6) C5 0.057(4) 0.091(5) 0.057(4) -0.006(4) 0.011(4) 0.006(4) C6 0.080(5) 0.118(7) 0.084(6) -0.009(5) -0.015(5) 0.029(5) C7 0.048(4) 0.068(3) 0.046(4) -0.001(3) -0.004(3) 0.001(3) C8 0.058(4) 0.070(3) 0.031(3) -0.005(3) -0.002(3) -0.004(3) C9 0.065(5) 0.077(5) 0.040(4) 0.006(3) 0.003(3) -0.010(4) C10 0.089(6) 0.101(7) 0.043(4) -0.010(4) 0.013(4) 0.009(5) C11 0.104(8) 0.095(6) 0.061(5) -0.011(4) 0.008(5) 0.028(5) C12 0.099(7) 0.072(4) 0.059(4) -0.002(4) -0.003(5) 0.017(4) C13 0.094(6) 0.065(4) 0.041(3) -0.001(3) -0.007(4) -0.002(4) C14 0.115(7) 0.087(5) 0.051(4) 0.007(4) 0.015(5) -0.017(5) C15 0.135(8) 0.068(4) 0.069(5) 0.001(4) 0.017(5) -0.018(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N1 2.018(5) . ? Pt1 N1 2.018(5) 5 ? Pt1 P1 2.3093(16) . ? Pt1 P1 2.3093(16) 5 ? P1 C1 1.814(6) . ? P1 C3 1.814(6) . ? P1 C5 1.825(7) . ? N1 C7 1.178(7) . ? N2 C7 1.250(8) . ? N2 C8 1.435(8) . ? C1 C2 1.505(8) . ? C3 C4 1.512(10) . ? C5 C6 1.518(9) . ? C8 C9 1.387(9) . ? C8 C13 1.399(9) . ? C9 C10 1.388(10) . ? C9 C14 1.493(9) . ? C10 C11 1.365(12) . ? C11 C12 1.378(10) . ? C12 C13 1.387(9) . ? C13 C15 1.487(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pt1 N1 180.0(4) . 5 ? N1 Pt1 P1 87.89(15) . . ? N1 Pt1 P1 92.11(15) 5 . ? N1 Pt1 P1 92.11(15) . 5 ? N1 Pt1 P1 87.89(15) 5 5 ? P1 Pt1 P1 180.00(9) . 5 ? C1 P1 C3 102.6(3) . . ? C1 P1 C5 106.6(4) . . ? C3 P1 C5 107.6(4) . . ? C1 P1 Pt1 113.2(2) . . ? C3 P1 Pt1 111.4(2) . . ? C5 P1 Pt1 114.5(2) . . ? C7 N1 Pt1 139.8(5) . . ? C7 N2 C8 125.6(6) . . ? C2 C1 P1 114.3(5) . . ? C4 C3 P1 113.9(5) . . ? C6 C5 P1 116.2(5) . . ? N1 C7 N2 170.3(8) . . ? C9 C8 C13 121.6(6) . . ? C9 C8 N2 116.2(6) . . ? C13 C8 N2 122.0(6) . . ? C8 C9 C10 118.1(6) . . ? C8 C9 C14 120.6(7) . . ? C10 C9 C14 121.3(6) . . ? C11 C10 C9 121.7(7) . . ? C10 C11 C12 119.2(7) . . ? C11 C12 C13 121.8(7) . . ? C12 C13 C8 117.5(7) . . ? C12 C13 C15 119.6(6) . . ? C8 C13 C15 122.9(7) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.791 _refine_diff_density_min -0.986 _refine_diff_density_rms 0.104 data_pme3ncn _database_code_CSD 184854 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H36 N4 P2 Pd' _chemical_formula_weight 548.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 'P2(1)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.790(3) _cell_length_b 13.920(3) _cell_length_c 17.037(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.279(6) _cell_angle_gamma 90.00 _cell_volume 2845.2(10) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 21 _cell_measurement_theta_min 8.15 _cell_measurement_theta_max 12.50 _exptl_crystal_description 'BLOCK ' _exptl_crystal_colour 'YELLOW ' _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.281 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 0.781 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.5423 _exptl_absorpt_correction_T_max 0.6346 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'MoK\a' _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5154 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0380 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.04 _reflns_number_total 4920 _reflns_number_gt 3841 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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^)+(0.1055P)^2^+7.0495P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4920 _refine_ls_number_parameters 200 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0835 _refine_ls_R_factor_gt 0.0669 _refine_ls_wR_factor_ref 0.1937 _refine_ls_wR_factor_gt 0.1776 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.004 _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 0.45108(4) 0.62019(3) 0.02358(3) 0.0516(2) Uani 1 1 d . . . P1 P 0.27851(15) 0.63133(14) 0.03039(11) 0.0628(5) Uani 1 1 d . . . P2 P 0.53933(15) 0.61252(14) 0.16417(10) 0.0620(5) Uani 1 1 d . . . N1 N 0.3761(5) 0.6452(6) -0.1041(4) 0.0784(18) Uani 1 1 d . . . N2 N 0.2870(7) 0.7809(6) -0.1908(5) 0.100(2) Uani 1 1 d . . . N3 N 0.6041(5) 0.6126(4) 0.0052(4) 0.0694(15) Uani 1 1 d . . . N4 N 0.6959(6) 0.6720(5) -0.0870(4) 0.0806(18) Uani 1 1 d . . . C1 C 0.2473(7) 0.5832(7) 0.1189(5) 0.083(2) Uani 1 1 d . . . H1A H 0.2710 0.5174 0.1277 0.100 Uiso 1 1 calc R . . H1B H 0.1685 0.5867 0.1077 0.100 Uiso 1 1 calc R . . H1C H 0.2860 0.6200 0.1681 0.100 Uiso 1 1 calc R . . C2 C 0.1771(6) 0.5676(8) -0.0558(5) 0.094(3) Uani 1 1 d . . . H2A H 0.1979 0.5012 -0.0541 0.113 Uiso 1 1 calc R . . H2B H 0.1750 0.5953 -0.1079 0.113 Uiso 1 1 calc R . . H2C H 0.1047 0.5726 -0.0509 0.113 Uiso 1 1 calc R . . C3 C 0.2294(8) 0.7541(7) 0.0197(6) 0.098(3) Uani 1 1 d . . . H3A H 0.2431 0.7837 -0.0266 0.117 Uiso 1 1 calc R . . H3B H 0.2682 0.7889 0.0701 0.117 Uiso 1 1 calc R . . H3C H 0.1509 0.7548 0.0101 0.117 Uiso 1 1 calc R . . C4 C 0.5173(7) 0.5076(7) 0.2199(5) 0.086(2) Uani 1 1 d . . . H4A H 0.4389 0.4995 0.2089 0.104 Uiso 1 1 calc R . . H4B H 0.5552 0.5161 0.2789 0.104 Uiso 1 1 calc R . . H4C H 0.5460 0.4516 0.2013 0.104 Uiso 1 1 calc R . . C5 C 0.5120(8) 0.7173(7) 0.2201(5) 0.095(3) Uani 1 1 d . . . H5A H 0.4332 0.7236 0.2079 0.114 Uiso 1 1 calc R . . H5B H 0.5399 0.7743 0.2023 0.114 Uiso 1 1 calc R . . H5C H 0.5487 0.7088 0.2792 0.114 Uiso 1 1 calc R . . C6 C 0.6915(6) 0.6131(7) 0.1929(5) 0.091(3) Uani 1 1 d . . . H6A H 0.7135 0.6668 0.1668 0.109 Uiso 1 1 calc R . . H6B H 0.7151 0.5546 0.1743 0.109 Uiso 1 1 calc R . . H6C H 0.7256 0.6184 0.2525 0.109 Uiso 1 1 calc R . . C7 C 0.3295(6) 0.7082(6) -0.1466(4) 0.0671(18) Uani 1 1 d . . . C8 C 0.1702(6) 0.7917(5) -0.2377(5) 0.0712(18) Uiso 1 1 d . . . C9 C 0.1099(8) 0.7232(7) -0.2926(6) 0.094(2) Uiso 1 1 d . . . C10 C 0.0002(11) 0.7350(10) -0.3496(8) 0.130(4) Uiso 1 1 d . . . H10 H -0.0381 0.6889 -0.3885 0.155 Uiso 1 1 calc R . . C11 C -0.0427(13) 0.8227(11) -0.3407(9) 0.146(5) Uiso 1 1 d . . . H11 H -0.1157 0.8338 -0.3756 0.175 Uiso 1 1 calc R . . C12 C 0.0018(10) 0.8891(9) -0.2927(8) 0.116(3) Uiso 1 1 d . . . H12 H -0.0382 0.9451 -0.2934 0.139 Uiso 1 1 calc R . . C13 C 0.1166(11) 0.8812(8) -0.2349(8) 0.117(4) Uiso 1 1 d . . . C14 C 0.1635(11) 0.6290(8) -0.2995(9) 0.130(4) Uiso 1 1 d . . . H14A H 0.2375 0.6269 -0.2588 0.156 Uiso 1 1 calc R . . H14B H 0.1673 0.6228 -0.3546 0.156 Uiso 1 1 calc R . . H14C H 0.1202 0.5773 -0.2895 0.156 Uiso 1 1 calc R . . C15 C 0.1708(13) 0.9518(12) -0.1830(10) 0.169(6) Uiso 1 1 d . . . H15A H 0.1228 1.0067 -0.1907 0.202 Uiso 1 1 calc R . . H15B H 0.2363 0.9692 -0.1951 0.202 Uiso 1 1 calc R . . H15C H 0.1920 0.9299 -0.1261 0.202 Uiso 1 1 calc R . . C16 C 0.6460(5) 0.6462(5) -0.0376(4) 0.0589(15) Uani 1 1 d . . . C17 C 0.7658(8) 0.7540(7) -0.0782(6) 0.091(2) Uiso 1 1 d . . . C18 C 0.7431(13) 0.8385(11) -0.0444(9) 0.146(4) Uiso 1 1 d . . . C19 C 0.8262(14) 0.9235(13) -0.0437(11) 0.170(6) Uiso 1 1 d . . . H19 H 0.8218 0.9849 -0.0237 0.204 Uiso 1 1 calc R . . C20 C 0.9033(12) 0.8957(10) -0.0755(9) 0.138(4) Uiso 1 1 d . . . H20 H 0.9553 0.9437 -0.0720 0.166 Uiso 1 1 calc R . . C21 C 0.9229(11) 0.8200(10) -0.1093(8) 0.132(4) Uiso 1 1 d . . . H21 H 0.9811 0.8162 -0.1301 0.158 Uiso 1 1 calc R . . C22 C 0.8520(9) 0.7430(8) -0.1133(6) 0.102(3) Uiso 1 1 d . . . C23 C 0.6431(13) 0.8530(12) -0.0189(11) 0.168(6) Uiso 1 1 d . . . H23A H 0.6435 0.9173 0.0016 0.202 Uiso 1 1 calc R . . H23B H 0.6455 0.8080 0.0244 0.202 Uiso 1 1 calc R . . H23C H 0.5765 0.8428 -0.0663 0.202 Uiso 1 1 calc R . . C24 C 0.8652(12) 0.6568(11) -0.1542(10) 0.154(5) Uiso 1 1 d . . . H24A H 0.8123 0.6098 -0.1504 0.185 Uiso 1 1 calc R . . H24B H 0.9394 0.6324 -0.1278 0.185 Uiso 1 1 calc R . . H24C H 0.8529 0.6701 -0.2120 0.185 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 0.0481(3) 0.0657(3) 0.0414(3) 0.0001(2) 0.0159(2) 0.0044(2) P1 0.0506(9) 0.0835(12) 0.0544(9) -0.0076(8) 0.0184(7) 0.0056(8) P2 0.0530(9) 0.0867(12) 0.0427(8) -0.0064(8) 0.0120(7) 0.0007(8) N1 0.069(4) 0.113(5) 0.052(3) 0.006(3) 0.020(3) 0.023(4) N2 0.110(6) 0.103(5) 0.077(5) 0.020(4) 0.019(4) -0.013(5) N3 0.056(3) 0.089(4) 0.069(4) 0.005(3) 0.028(3) 0.006(3) N4 0.081(4) 0.095(5) 0.078(4) -0.001(3) 0.042(4) -0.020(4) C1 0.065(5) 0.118(6) 0.075(5) -0.007(5) 0.036(4) -0.012(5) C2 0.057(4) 0.145(8) 0.074(5) -0.030(5) 0.016(4) -0.006(5) C3 0.087(6) 0.100(6) 0.113(7) 0.004(5) 0.045(6) 0.030(5) C4 0.086(6) 0.113(7) 0.063(4) 0.017(4) 0.030(4) 0.012(5) C5 0.091(6) 0.113(7) 0.071(5) -0.036(5) 0.016(4) -0.005(5) C6 0.056(4) 0.144(8) 0.060(4) -0.005(5) 0.004(3) 0.010(5) C7 0.061(4) 0.088(5) 0.050(4) 0.010(4) 0.016(3) 0.006(4) C16 0.054(4) 0.069(4) 0.054(3) 0.003(3) 0.018(3) -0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 2.080(6) . ? Pd1 N3 2.089(6) . ? Pd1 P1 2.2555(19) . ? Pd1 P2 2.2690(17) . ? P1 C3 1.807(9) . ? P1 C1 1.816(8) . ? P1 C2 1.818(8) . ? P2 C4 1.817(8) . ? P2 C6 1.835(8) . ? P2 C5 1.841(8) . ? N1 C7 1.162(9) . ? N2 C7 1.265(10) . ? N2 C8 1.438(10) . ? N3 C16 1.144(9) . ? N4 C16 1.272(9) . ? N4 C17 1.426(11) . ? C8 C9 1.371(12) . ? C8 C13 1.431(13) . ? C9 C10 1.412(14) . ? C9 C14 1.503(14) . ? C10 C11 1.369(17) . ? C11 C12 1.235(16) . ? C12 C13 1.461(16) . ? C13 C15 1.343(17) . ? C17 C18 1.383(17) . ? C17 C22 1.433(13) . ? C18 C23 1.500(19) . ? C18 C19 1.59(2) . ? C19 C20 1.34(2) . ? C20 C21 1.267(17) . ? C21 C22 1.391(15) . ? C22 C24 1.427(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 N3 88.2(2) . . ? N1 Pd1 P1 86.42(18) . . ? N3 Pd1 P1 174.59(18) . . ? N1 Pd1 P2 172.8(2) . . ? N3 Pd1 P2 90.38(18) . . ? P1 Pd1 P2 94.97(7) . . ? C3 P1 C1 105.3(5) . . ? C3 P1 C2 104.7(5) . . ? C1 P1 C2 100.9(4) . . ? C3 P1 Pd1 111.8(3) . . ? C1 P1 Pd1 121.2(3) . . ? C2 P1 Pd1 111.2(3) . . ? C4 P2 C6 101.9(4) . . ? C4 P2 C5 106.0(5) . . ? C6 P2 C5 103.4(4) . . ? C4 P2 Pd1 118.6(3) . . ? C6 P2 Pd1 112.0(3) . . ? C5 P2 Pd1 113.3(3) . . ? C7 N1 Pd1 136.8(6) . . ? C7 N2 C8 124.3(7) . . ? C16 N3 Pd1 138.1(6) . . ? C16 N4 C17 126.7(7) . . ? N1 C7 N2 174.8(9) . . ? C9 C8 C13 117.7(9) . . ? C9 C8 N2 122.5(8) . . ? C13 C8 N2 119.4(8) . . ? C8 C9 C10 125.4(10) . . ? C8 C9 C14 119.7(9) . . ? C10 C9 C14 114.8(10) . . ? C11 C10 C9 111.6(13) . . ? C12 C11 C10 129.1(16) . . ? C11 C12 C13 121.0(13) . . ? C15 C13 C8 121.0(12) . . ? C15 C13 C12 123.8(12) . . ? C8 C13 C12 115.2(10) . . ? N3 C16 N4 172.3(8) . . ? C18 C17 N4 120.7(10) . . ? C18 C17 C22 124.6(11) . . ? N4 C17 C22 114.5(8) . . ? C17 C18 C23 123.9(14) . . ? C17 C18 C19 113.5(14) . . ? C23 C18 C19 122.3(15) . . ? C20 C19 C18 111.6(16) . . ? C21 C20 C19 135.6(17) . . ? C20 C21 C22 115.8(14) . . ? C21 C22 C24 119.1(12) . . ? C21 C22 C17 118.7(11) . . ? C24 C22 C17 122.2(11) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.043 _refine_diff_density_min -0.544 _refine_diff_density_rms 0.110 data_2pd _database_code_CSD 184855 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H48 N4 P2 Pd' _chemical_formula_weight 633.06 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' _symmetry_cell_setting 'Orthorhombic' _symmetry_space_group_name_H-M 'Pbca ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 9.525(4) _cell_length_b 14.396(5) _cell_length_c 24.183(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3316(2) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 23 _cell_measurement_theta_min 5.63 _cell_measurement_theta_max 15.33 _exptl_crystal_description 'BLOCK ' _exptl_crystal_colour 'YELLOW ' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.268 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 0.680 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.6705 _exptl_absorpt_correction_T_max 0.9049 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'MoK\a' _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2922 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0795 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 25.04 _reflns_number_total 2922 _reflns_number_gt 1514 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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^)+(0.0434P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00035(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2922 _refine_ls_number_parameters 170 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1180 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.1179 _refine_ls_wR_factor_gt 0.0921 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.990 _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 0.0000 0.0000 0.0000 0.03732(18) Uani 1 2 d S . . P1 P 0.15842(15) 0.06490(11) 0.06227(6) 0.0436(4) Uani 1 1 d . . . N1 N -0.1561(5) 0.0449(3) 0.04990(18) 0.0493(12) Uani 1 1 d . . . N2 N -0.2279(5) 0.0334(3) 0.14667(18) 0.0496(13) Uani 1 1 d . . . C1 C 0.1635(6) 0.0049(4) 0.1286(2) 0.0549(14) Uani 1 1 d . . . H1A H 0.2298 0.0364 0.1526 0.066 Uiso 1 1 calc R . . H1B H 0.0716 0.0091 0.1457 0.066 Uiso 1 1 calc R . . C2 C 0.2046(7) -0.0965(4) 0.1245(3) 0.079(2) Uani 1 1 d . . . H2A H 0.2051 -0.1236 0.1607 0.095 Uiso 1 1 calc R . . H2B H 0.2965 -0.1015 0.1085 0.095 Uiso 1 1 calc R . . H2C H 0.1381 -0.1288 0.1016 0.095 Uiso 1 1 calc R . . C3 C 0.3403(5) 0.0693(5) 0.0378(2) 0.0600(16) Uani 1 1 d . . . H3A H 0.3688 0.0069 0.0279 0.072 Uiso 1 1 calc R . . H3B H 0.3429 0.1066 0.0044 0.072 Uiso 1 1 calc R . . C4 C 0.4479(6) 0.1082(6) 0.0781(3) 0.087(2) Uani 1 1 d . . . H4A H 0.5391 0.1073 0.0612 0.104 Uiso 1 1 calc R . . H4B H 0.4491 0.0709 0.1110 0.104 Uiso 1 1 calc R . . H4C H 0.4234 0.1709 0.0875 0.104 Uiso 1 1 calc R . . C5 C 0.1085(7) 0.1829(4) 0.0815(3) 0.0644(18) Uani 1 1 d . . . H5A H 0.0221 0.1807 0.1027 0.077 Uiso 1 1 calc R . . H5B H 0.1808 0.2089 0.1051 0.077 Uiso 1 1 calc R . . C6 C 0.0876(8) 0.2466(5) 0.0319(3) 0.103(3) Uani 1 1 d . . . H6A H 0.0616 0.3075 0.0446 0.123 Uiso 1 1 calc R . . H6B H 0.0145 0.2222 0.0088 0.123 Uiso 1 1 calc R . . H6C H 0.1734 0.2504 0.0112 0.123 Uiso 1 1 calc R . . C7 C -0.1923(6) 0.0323(4) 0.0964(2) 0.0448(14) Uani 1 1 d . . . C8 C -0.3200(6) -0.0302(4) 0.1718(2) 0.0462(15) Uani 1 1 d . . . C9 C -0.4136(6) 0.0069(5) 0.2114(2) 0.0503(14) Uani 1 1 d . . . C10 C -0.5054(8) -0.0522(5) 0.2384(2) 0.0680(17) Uani 1 1 d . . . H10 H -0.5688 -0.0276 0.2637 0.082 Uiso 1 1 calc R . . C11 C -0.5053(8) -0.1457(6) 0.2289(3) 0.078(2) Uani 1 1 d . . . H11 H -0.5680 -0.1842 0.2475 0.094 Uiso 1 1 calc R . . C12 C -0.4117(7) -0.1821(5) 0.1916(3) 0.070(2) Uani 1 1 d . . . H12 H -0.4112 -0.2459 0.1855 0.084 Uiso 1 1 calc R . . C13 C -0.3171(6) -0.1262(4) 0.1624(2) 0.0515(15) Uani 1 1 d . . . C14 C -0.4115(7) 0.1097(4) 0.2251(2) 0.071(2) Uani 1 1 d . . . H14A H -0.3423 0.1402 0.2027 0.085 Uiso 1 1 calc R . . H14B H -0.3887 0.1178 0.2635 0.085 Uiso 1 1 calc R . . H14C H -0.5023 0.1360 0.2178 0.085 Uiso 1 1 calc R . . C15 C -0.2113(7) -0.1699(4) 0.1233(3) 0.078(2) Uani 1 1 d . . . H15A H -0.2257 -0.2358 0.1221 0.093 Uiso 1 1 calc R . . H15B H -0.1179 -0.1570 0.1362 0.093 Uiso 1 1 calc R . . H15C H -0.2233 -0.1443 0.0870 0.093 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 0.0332(3) 0.0473(3) 0.0314(3) 0.0005(3) 0.0033(3) -0.0009(4) P1 0.0392(8) 0.0505(8) 0.0412(7) -0.0015(8) -0.0018(7) 0.0012(8) N1 0.036(3) 0.068(3) 0.045(3) -0.005(2) 0.010(2) -0.003(3) N2 0.045(3) 0.065(3) 0.039(3) -0.004(2) 0.007(2) -0.004(2) C1 0.051(3) 0.070(4) 0.043(3) -0.004(3) 0.004(3) 0.005(4) C2 0.093(6) 0.070(5) 0.075(5) 0.013(4) -0.004(4) 0.022(4) C3 0.037(3) 0.085(4) 0.059(4) 0.004(4) -0.002(3) -0.002(4) C4 0.052(4) 0.129(7) 0.078(5) 0.007(5) -0.017(4) -0.011(4) C5 0.065(4) 0.054(4) 0.074(5) -0.014(3) -0.014(4) 0.003(4) C6 0.141(8) 0.052(4) 0.116(6) -0.007(5) -0.060(6) 0.010(5) C7 0.031(3) 0.051(3) 0.053(4) -0.003(3) 0.000(3) 0.002(3) C8 0.045(3) 0.062(4) 0.032(3) 0.003(2) -0.006(3) 0.002(3) C9 0.051(4) 0.067(4) 0.033(3) -0.001(3) 0.004(3) 0.005(4) C10 0.058(4) 0.103(5) 0.043(3) -0.006(4) 0.006(4) -0.004(5) C11 0.074(5) 0.106(6) 0.055(4) 0.005(4) 0.007(5) -0.025(6) C12 0.088(6) 0.069(5) 0.054(4) 0.008(4) -0.015(4) -0.017(4) C13 0.056(4) 0.059(4) 0.039(3) 0.001(3) -0.004(3) 0.002(4) C14 0.081(5) 0.082(5) 0.050(4) 0.004(4) 0.015(4) 0.022(4) C15 0.089(6) 0.068(4) 0.075(4) 0.004(4) 0.010(4) 0.015(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 N1 2.021(4) . ? Pd1 N1 2.021(4) 5 ? Pd1 P1 2.3276(16) . ? Pd1 P1 2.3276(16) 5 ? P1 C1 1.822(5) . ? P1 C5 1.825(6) . ? P1 C3 1.831(5) . ? N1 C7 1.191(6) . ? N2 C7 1.261(7) . ? N2 C8 1.406(7) . ? C1 C2 1.515(8) . ? C3 C4 1.520(7) . ? C5 C6 1.523(8) . ? C8 C13 1.400(8) . ? C8 C9 1.414(7) . ? C9 C10 1.384(9) . ? C9 C14 1.516(8) . ? C10 C11 1.365(10) . ? C11 C12 1.372(9) . ? C12 C13 1.399(8) . ? C13 C15 1.518(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 N1 180.0(3) . 5 ? N1 Pd1 P1 87.83(13) . . ? N1 Pd1 P1 92.17(13) 5 . ? N1 Pd1 P1 92.17(13) . 5 ? N1 Pd1 P1 87.83(13) 5 5 ? P1 Pd1 P1 180.00(8) . 5 ? C1 P1 C5 102.9(3) . . ? C1 P1 C3 106.0(3) . . ? C5 P1 C3 107.2(3) . . ? C1 P1 Pd1 113.3(2) . . ? C5 P1 Pd1 111.7(2) . . ? C3 P1 Pd1 114.75(19) . . ? C7 N1 Pd1 136.8(4) . . ? C7 N2 C8 125.1(5) . . ? C2 C1 P1 114.0(4) . . ? C4 C3 P1 116.4(4) . . ? C6 C5 P1 113.2(4) . . ? N1 C7 N2 170.4(6) . . ? C13 C8 N2 124.1(5) . . ? C13 C8 C9 119.7(6) . . ? N2 C8 C9 116.1(5) . . ? C10 C9 C8 119.0(6) . . ? C10 C9 C14 120.4(6) . . ? C8 C9 C14 120.6(6) . . ? C11 C10 C9 121.8(7) . . ? C10 C11 C12 119.2(7) . . ? C11 C12 C13 122.0(7) . . ? C12 C13 C8 118.2(6) . . ? C12 C13 C15 120.3(6) . . ? C8 C13 C15 121.5(6) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.307 _refine_diff_density_min -0.338 _refine_diff_density_rms 0.074 data_pdncnet _database_code_CSD 184857 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H44 N4 P2 Pd' _chemical_formula_weight 605.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 'P2(1)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.191(2) _cell_length_b 16.580(4) _cell_length_c 16.660(5) _cell_angle_alpha 90.00 _cell_angle_beta 109.926(15) _cell_angle_gamma 90.00 _cell_volume 3165.9(14) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 23 _cell_measurement_theta_min 7.28 _cell_measurement_theta_max 12.55 _exptl_crystal_description 'BLOCK ' _exptl_crystal_colour 'YELLOW ' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.269 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 0.709 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.3584 _exptl_absorpt_correction_T_max 0.7492 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'MoK\a' _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5765 _diffrn_reflns_av_R_equivalents 0.0393 _diffrn_reflns_av_sigmaI/netI 0.0539 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5490 _reflns_number_gt 3711 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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^)+(0.0822P)^2^+2.3944P] 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 0.0014(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5490 _refine_ls_number_parameters 278 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0906 _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.1596 _refine_ls_wR_factor_gt 0.1371 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _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 Pd1 Pd 0.43499(4) 0.40725(3) 0.02745(3) 0.05826(19) Uani 1 1 d . . . P1 P 0.25380(14) 0.41300(10) 0.03493(11) 0.0693(4) Uani 1 1 d . . . P2 P 0.52911(15) 0.41959(11) 0.17006(10) 0.0723(5) Uani 1 1 d . . . N1 N 0.3539(5) 0.3819(4) -0.1020(3) 0.0815(15) Uani 1 1 d . . . N2 N 0.2886(5) 0.2597(4) -0.1852(4) 0.0982(19) Uani 1 1 d . . . N3 N 0.5959(5) 0.3994(3) 0.0093(3) 0.0759(14) Uani 1 1 d . . . N4 N 0.6857(5) 0.3289(4) -0.0794(4) 0.0943(18) Uani 1 1 d . . . C1 C 0.1912(7) 0.3137(5) 0.0271(7) 0.123(3) Uani 1 1 d . . . H1A H 0.2031 0.2851 -0.0193 0.148 Uiso 1 1 calc R . . H1B H 0.1091 0.3182 0.0171 0.148 Uiso 1 1 calc R . . H1C H 0.2281 0.2849 0.0794 0.148 Uiso 1 1 calc R . . C2 C 0.1554(6) 0.4691(5) -0.0529(5) 0.095(2) Uani 1 1 d . . . H2A H 0.1629 0.4507 -0.1055 0.114 Uiso 1 1 calc R . . H2B H 0.1744 0.5254 -0.0455 0.114 Uiso 1 1 calc R . . H2C H 0.0767 0.4610 -0.0546 0.114 Uiso 1 1 calc R . . C3 C 0.2234(6) 0.4593(6) 0.1231(5) 0.109(3) Uani 1 1 d . . . H3A H 0.2710 0.4348 0.1756 0.130 Uiso 1 1 calc R . . H3B H 0.1425 0.4518 0.1161 0.130 Uiso 1 1 calc R . . H3C H 0.2404 0.5159 0.1245 0.130 Uiso 1 1 calc R . . C4 C 0.5092(7) 0.5116(5) 0.2237(5) 0.101(2) Uani 1 1 d . . . H4A H 0.4275 0.5203 0.2126 0.121 Uiso 1 1 calc R . . H4B H 0.5410 0.5566 0.2026 0.121 Uiso 1 1 calc R . . H4C H 0.5488 0.5063 0.2841 0.121 Uiso 1 1 calc R . . C5 C 0.4969(7) 0.3363(5) 0.2296(5) 0.111(3) Uani 1 1 d . . . H5A H 0.4143 0.3335 0.2181 0.134 Uiso 1 1 calc R . . H5B H 0.5363 0.3447 0.2896 0.134 Uiso 1 1 calc R . . H5C H 0.5233 0.2867 0.2126 0.134 Uiso 1 1 calc R . . C6 C 0.6862(6) 0.4153(5) 0.2001(5) 0.101(2) Uani 1 1 d . . . H6A H 0.7078 0.3687 0.1749 0.121 Uiso 1 1 calc R . . H6B H 0.7204 0.4121 0.2611 0.121 Uiso 1 1 calc R . . H6C H 0.7136 0.4630 0.1803 0.121 Uiso 1 1 calc R . . C7 C 0.3170(5) 0.3240(5) -0.1416(4) 0.0742(17) Uani 1 1 d . . . C8 C 0.1724(6) 0.2345(5) -0.2342(4) 0.0798(18) Uani 1 1 d . . . C9 C 0.0977(7) 0.2829(5) -0.2978(5) 0.099(2) Uani 1 1 d . . . C10 C -0.0088(7) 0.2517(7) -0.3474(5) 0.114(3) Uani 1 1 d . . . H10 H -0.0594 0.2834 -0.3903 0.137 Uiso 1 1 calc R . . C11 C -0.0410(8) 0.1753(8) -0.3348(7) 0.119(3) Uani 1 1 d . . . H11 H -0.1132 0.1556 -0.3691 0.143 Uiso 1 1 calc R . . C12 C 0.0291(10) 0.1286(7) -0.2742(7) 0.117(3) Uani 1 1 d . . . H12 H 0.0056 0.0769 -0.2658 0.141 Uiso 1 1 calc R . . C13 C 0.1385(8) 0.1572(5) -0.2229(5) 0.105(2) Uani 1 1 d . . . C14 C 0.1224(11) 0.3742(8) -0.3118(8) 0.160(4) Uiso 1 1 d . . . H14A H 0.0496 0.4026 -0.3391 0.192 Uiso 1 1 calc R . . H14B H 0.1627 0.3999 -0.2574 0.192 Uiso 1 1 calc R . . C15 C 0.1872(14) 0.3762(11) -0.3605(11) 0.238(7) Uiso 1 1 d . . . H15A H 0.2029 0.4312 -0.3709 0.285 Uiso 1 1 calc R . . H15B H 0.1468 0.3500 -0.4138 0.285 Uiso 1 1 calc R . . H15C H 0.2595 0.3487 -0.3324 0.285 Uiso 1 1 calc R . . C16 C 0.2240(11) 0.1000(7) -0.1592(8) 0.157(4) Uiso 1 1 d . . . H16A H 0.2034 0.0451 -0.1786 0.188 Uiso 1 1 calc R . . H16B H 0.3016 0.1102 -0.1607 0.188 Uiso 1 1 calc R . . C17 C 0.2287(14) 0.1054(10) -0.0729(11) 0.236(8) Uiso 1 1 d . . . H17A H 0.2857 0.0681 -0.0386 0.283 Uiso 1 1 calc R . . H17B H 0.1536 0.0925 -0.0696 0.283 Uiso 1 1 calc R . . H17C H 0.2499 0.1593 -0.0523 0.283 Uiso 1 1 calc R . . C18 C 0.6351(5) 0.3592(4) -0.0322(4) 0.0668(15) Uani 1 1 d . . . C19 C 0.7417(6) 0.2522(4) -0.0686(4) 0.0815(19) Uani 1 1 d . . . C20 C 0.7032(8) 0.1863(5) -0.0347(5) 0.108(3) Uani 1 1 d . . . C21 C 0.7649(12) 0.1122(6) -0.0287(7) 0.143(4) Uani 1 1 d . . . H21 H 0.7413 0.0670 -0.0058 0.172 Uiso 1 1 calc R . . C22 C 0.8601(12) 0.1067(7) -0.0567(8) 0.143(5) Uani 1 1 d . . . H22 H 0.9017 0.0587 -0.0504 0.172 Uiso 1 1 calc R . . C23 C 0.8917(8) 0.1720(8) -0.0934(6) 0.129(4) Uani 1 1 d . . . H23 H 0.9533 0.1668 -0.1140 0.154 Uiso 1 1 calc R . . C24 C 0.8355(7) 0.2468(5) -0.1014(5) 0.103(3) Uani 1 1 d . . . C25 C 0.5954(10) 0.1907(8) -0.0072(7) 0.149(4) Uiso 1 1 d . . . H25A H 0.6052 0.2385 0.0282 0.179 Uiso 1 1 calc R . . H25B H 0.5295 0.2013 -0.0586 0.179 Uiso 1 1 calc R . . C26 C 0.5612(19) 0.1305(14) 0.0350(15) 0.330(12) Uiso 1 1 d . . . H26A H 0.4899 0.1457 0.0434 0.396 Uiso 1 1 calc R . . H26B H 0.6207 0.1215 0.0894 0.396 Uiso 1 1 calc R . . H26C H 0.5489 0.0818 0.0018 0.396 Uiso 1 1 calc R . . C27 C 0.8706(8) 0.3175(6) -0.1429(6) 0.120(3) Uiso 1 1 d . . . H27A H 0.8740 0.3650 -0.1081 0.144 Uiso 1 1 calc R . . H27B H 0.9484 0.3080 -0.1444 0.144 Uiso 1 1 calc R . . C28 C 0.7912(9) 0.3338(7) -0.2304(7) 0.147(4) Uiso 1 1 d . . . H28A H 0.8187 0.3799 -0.2529 0.177 Uiso 1 1 calc R . . H28B H 0.7142 0.3445 -0.2295 0.177 Uiso 1 1 calc R . . H28C H 0.7889 0.2878 -0.2659 0.177 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 0.0571(3) 0.0619(3) 0.0558(3) 0.0030(2) 0.01930(19) 0.0020(2) P1 0.0606(9) 0.0725(10) 0.0796(10) 0.0092(8) 0.0302(8) 0.0005(8) P2 0.0684(9) 0.0900(12) 0.0561(8) 0.0099(8) 0.0182(7) 0.0044(9) N1 0.081(4) 0.096(4) 0.061(3) -0.018(3) 0.015(3) -0.010(3) N2 0.083(4) 0.096(4) 0.100(4) -0.033(4) 0.010(3) 0.005(3) N3 0.085(3) 0.079(4) 0.076(3) -0.003(3) 0.044(3) 0.007(3) N4 0.105(4) 0.094(4) 0.101(4) 0.000(3) 0.058(4) 0.019(4) C1 0.091(5) 0.102(6) 0.190(10) 0.016(6) 0.066(6) -0.019(5) C2 0.064(4) 0.115(6) 0.101(5) 0.023(4) 0.021(4) 0.008(4) C3 0.079(5) 0.156(8) 0.105(6) -0.005(5) 0.050(4) 0.017(5) C4 0.100(5) 0.119(6) 0.083(5) -0.020(4) 0.029(4) -0.006(5) C5 0.114(6) 0.125(7) 0.088(5) 0.046(5) 0.025(5) 0.007(5) C6 0.069(4) 0.139(7) 0.083(5) 0.015(4) 0.008(4) 0.011(4) C7 0.064(4) 0.094(5) 0.058(3) 0.002(4) 0.012(3) 0.012(4) C8 0.078(4) 0.089(5) 0.073(4) -0.028(4) 0.026(3) -0.007(4) C9 0.084(5) 0.111(6) 0.093(5) -0.012(5) 0.017(4) -0.007(5) C10 0.086(6) 0.155(9) 0.093(6) -0.013(6) 0.019(4) 0.002(6) C11 0.085(6) 0.151(10) 0.130(8) -0.053(7) 0.047(6) -0.023(6) C12 0.126(8) 0.114(7) 0.128(8) -0.026(6) 0.064(7) -0.033(6) C13 0.115(6) 0.104(6) 0.103(6) -0.014(5) 0.044(5) -0.003(5) C18 0.063(4) 0.070(4) 0.062(3) 0.006(3) 0.014(3) -0.001(3) C19 0.083(4) 0.083(5) 0.068(4) -0.010(3) 0.012(3) 0.011(4) C20 0.117(7) 0.087(5) 0.101(6) 0.001(4) 0.014(5) 0.016(5) C21 0.191(12) 0.086(7) 0.122(8) 0.004(5) 0.014(8) 0.031(7) C22 0.152(10) 0.110(8) 0.122(8) -0.027(7) -0.012(7) 0.054(8) C23 0.095(6) 0.158(10) 0.107(7) -0.044(7) 0.001(5) 0.042(7) C24 0.082(5) 0.123(7) 0.091(5) -0.039(5) 0.011(4) 0.034(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 2.087(5) . ? Pd1 N3 2.089(5) . ? Pd1 P1 2.2565(17) . ? Pd1 P2 2.2684(18) . ? P1 C1 1.800(8) . ? P1 C2 1.802(7) . ? P1 C3 1.804(7) . ? P2 C6 1.808(7) . ? P2 C5 1.820(7) . ? P2 C4 1.826(7) . ? N1 C7 1.165(8) . ? N2 C7 1.270(9) . ? N2 C8 1.435(8) . ? N3 C18 1.172(8) . ? N4 C18 1.258(8) . ? N4 C19 1.426(9) . ? C8 C13 1.378(10) . ? C8 C9 1.392(10) . ? C9 C10 1.380(11) . ? C9 C14 1.576(14) . ? C10 C11 1.365(13) . ? C11 C12 1.327(13) . ? C12 C13 1.399(12) . ? C13 C16 1.535(13) . ? C14 C15 1.312(16) . ? C16 C17 1.421(18) . ? C19 C20 1.384(11) . ? C19 C24 1.429(10) . ? C20 C21 1.425(12) . ? C20 C25 1.534(13) . ? C21 C22 1.393(16) . ? C22 C23 1.363(15) . ? C23 C24 1.400(12) . ? C24 C27 1.495(12) . ? C25 C26 1.36(2) . ? C27 C28 1.476(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 N3 88.6(2) . . ? N1 Pd1 P1 86.45(16) . . ? N3 Pd1 P1 175.00(16) . . ? N1 Pd1 P2 173.38(18) . . ? N3 Pd1 P2 89.59(16) . . ? P1 Pd1 P2 95.37(7) . . ? C1 P1 C2 105.4(4) . . ? C1 P1 C3 104.4(4) . . ? C2 P1 C3 100.2(4) . . ? C1 P1 Pd1 110.8(3) . . ? C2 P1 Pd1 111.7(2) . . ? C3 P1 Pd1 122.7(3) . . ? C6 P2 C5 103.0(4) . . ? C6 P2 C4 101.6(4) . . ? C5 P2 C4 106.2(4) . . ? C6 P2 Pd1 113.4(3) . . ? C5 P2 Pd1 112.1(3) . . ? C4 P2 Pd1 118.9(3) . . ? C7 N1 Pd1 135.0(5) . . ? C7 N2 C8 126.4(6) . . ? C18 N3 Pd1 135.4(5) . . ? C18 N4 C19 126.4(6) . . ? N1 C7 N2 173.2(7) . . ? C13 C8 C9 119.4(7) . . ? C13 C8 N2 118.5(7) . . ? C9 C8 N2 121.8(7) . . ? C10 C9 C8 118.6(8) . . ? C10 C9 C14 117.3(9) . . ? C8 C9 C14 124.0(8) . . ? C11 C10 C9 121.1(9) . . ? C12 C11 C10 120.9(9) . . ? C11 C12 C13 120.0(10) . . ? C8 C13 C12 120.0(9) . . ? C8 C13 C16 120.3(9) . . ? C12 C13 C16 119.6(10) . . ? C15 C14 C9 107.5(13) . . ? C17 C16 C13 116.4(12) . . ? N3 C18 N4 168.7(7) . . ? C20 C19 N4 122.8(7) . . ? C20 C19 C24 122.3(7) . . ? N4 C19 C24 114.7(7) . . ? C19 C20 C21 117.7(10) . . ? C19 C20 C25 121.9(8) . . ? C21 C20 C25 120.4(10) . . ? C22 C21 C20 120.9(11) . . ? C23 C22 C21 119.5(11) . . ? C22 C23 C24 122.9(11) . . ? C23 C24 C19 116.6(9) . . ? C23 C24 C27 122.1(9) . . ? C19 C24 C27 121.3(7) . . ? C26 C25 C20 124.2(14) . . ? C28 C27 C24 114.0(8) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.858 _refine_diff_density_min -0.466 _refine_diff_density_rms 0.075