Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Joo, Young-Seon' 'Kim, Yong-Joo' 'Kwak, Yong-Su' '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 ; Reactions of Palladium(II) and-Platinum(II) Bisazido Complexes with Isocyanides: Synthesis and Structural Characterisation of Palladium(II) and -Platinum(II) Complexes Containing Carbodiimido (or Biscarbodiimido) and Bistetrazolato ligand ; data_psipd _database_code_CSD 167462 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H36 N6 P2 Pd' _chemical_formula_weight 576.93 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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.078(2) _cell_length_b 11.772(3) _cell_length_c 13.628(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.12(2) _cell_angle_gamma 90.00 _cell_volume 1375.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 596 _exptl_absorpt_coefficient_mu 0.813 _exptl_absorpt_correction_type ? _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 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2704 _diffrn_reflns_av_R_equivalents 0.0368 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _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 2469 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+0.4119P] 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 0.02(4) _refine_ls_number_reflns 2538 _refine_ls_number_parameters 298 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0285 _refine_ls_R_factor_gt 0.0275 _refine_ls_wR_factor_ref 0.0734 _refine_ls_wR_factor_gt 0.0724 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd -0.30407(3) -0.25020(3) -0.16344(2) 0.03870(11) Uani 1 1 d . . . P1 P -0.08087(15) -0.14047(12) -0.12898(10) 0.0453(3) Uani 1 1 d . . . P2 P -0.51515(18) -0.36965(13) -0.17672(14) 0.0551(4) Uani 1 1 d . . . N1 N -0.4896(4) -0.0399(4) -0.2579(3) 0.0482(10) Uani 1 1 d . . . N2 N -0.6151(5) 0.0224(4) -0.2510(5) 0.0678(14) Uani 1 1 d . . . N3 N -0.6471(6) -0.0191(5) -0.1725(5) 0.0712(15) Uani 1 1 d . . . N4 N -0.5491(6) -0.1059(4) -0.1273(4) 0.0597(12) Uani 1 1 d . . . N5 N -0.1658(6) -0.3876(5) -0.1562(4) 0.0637(13) Uani 1 1 d . . . N6 N -0.0144(9) -0.5330(6) -0.1986(4) 0.102(3) Uani 1 1 d . . . C1 C -0.4521(6) -0.1193(4) -0.1809(4) 0.0422(11) Uani 1 1 d . . . C2 C -0.4149(5) -0.0055(4) -0.3305(4) 0.0520(12) Uani 1 1 d . . . C3 C -0.3478(6) 0.1036(5) -0.3192(5) 0.0643(15) Uani 1 1 d . . . C4 C -0.2622(8) 0.1317(7) -0.3835(6) 0.0798(19) Uani 1 1 d . . . H4 H -0.2122 0.2017 -0.3759 0.096 Uiso 1 1 calc R . . C5 C -0.2509(9) 0.0579(8) -0.4572(6) 0.092(3) Uani 1 1 d . . . H5 H -0.1918 0.0780 -0.4988 0.111 Uiso 1 1 calc R . . C6 C -0.3249(9) -0.0462(8) -0.4719(5) 0.083(2) Uani 1 1 d . . . H6 H -0.3189 -0.0940 -0.5248 0.100 Uiso 1 1 calc R . . C7 C -0.4081(6) -0.0794(5) -0.4079(4) 0.0593(14) Uani 1 1 d . . . C8 C -0.3673(9) 0.1906(6) -0.2406(7) 0.091(2) Uani 1 1 d . . . H8A H -0.4291 0.1581 -0.2026 0.136 Uiso 1 1 calc R . . H8B H -0.4183 0.2571 -0.2768 0.136 Uiso 1 1 calc R . . H8C H -0.2666 0.2109 -0.1934 0.136 Uiso 1 1 calc R . . C9 C -0.4897(8) -0.1913(6) -0.4257(5) 0.0769(18) Uani 1 1 d . . . H9A H -0.4704 -0.2296 -0.4825 0.115 Uiso 1 1 calc R . . H9B H -0.5998 -0.1795 -0.4419 0.115 Uiso 1 1 calc R . . H9C H -0.4515 -0.2369 -0.3642 0.115 Uiso 1 1 calc R . . C10 C -0.0984(6) -0.4563(4) -0.1848(4) 0.0481(11) Uani 1 1 d . . . C11 C -0.0048(6) -0.5861(5) -0.2878(4) 0.0558(12) Uani 1 1 d . . . C12 C -0.0854(6) -0.5481(5) -0.3895(4) 0.0557(12) Uani 1 1 d . . . C13 C -0.0638(9) -0.6070(7) -0.4710(6) 0.081(2) Uani 1 1 d . . . H13 H -0.1169 -0.5843 -0.5388 0.097 Uiso 1 1 calc R . . C14 C 0.0333(10) -0.6974(8) -0.4542(7) 0.095(2) Uani 1 1 d . . . H14 H 0.0450 -0.7356 -0.5109 0.114 Uiso 1 1 calc R . . C15 C 0.1140(8) -0.7340(7) -0.3572(6) 0.0795(19) Uani 1 1 d . . . H15 H 0.1810 -0.7958 -0.3479 0.095 Uiso 1 1 calc R . . C16 C 0.0961(7) -0.6790(5) -0.2720(5) 0.0636(14) Uani 1 1 d . . . C17 C 0.1846(8) -0.7206(6) -0.1638(6) 0.095(3) Uani 1 1 d . . . H17A H 0.1597 -0.6738 -0.1138 0.142 Uiso 1 1 calc R . . H17B H 0.2946 -0.7167 -0.1525 0.142 Uiso 1 1 calc R . . H17C H 0.1559 -0.7978 -0.1564 0.142 Uiso 1 1 calc R . . C18 C -0.1986(9) -0.4501(7) -0.4098(5) 0.081(2) Uani 1 1 d . . . H18A H -0.1995 -0.4191 -0.3448 0.122 Uiso 1 1 calc R . . H18B H -0.3012 -0.4764 -0.4487 0.122 Uiso 1 1 calc R . . H18C H -0.1671 -0.3924 -0.4486 0.122 Uiso 1 1 calc R . . C19 C -0.5449(10) -0.3783(9) -0.0531(6) 0.096(3) Uani 1 1 d . . . H19A H -0.4480 -0.3963 -0.0003 0.144 Uiso 1 1 calc R . . H19B H -0.6200 -0.4365 -0.0554 0.144 Uiso 1 1 calc R . . H19C H -0.5826 -0.3067 -0.0374 0.144 Uiso 1 1 calc R . . C20 C -0.4901(11) -0.5143(7) -0.2146(9) 0.111(3) Uani 1 1 d . . . H20A H -0.4738 -0.5138 -0.2807 0.166 Uiso 1 1 calc R . . H20B H -0.5818 -0.5577 -0.2196 0.166 Uiso 1 1 calc R . . H20C H -0.4015 -0.5479 -0.1635 0.166 Uiso 1 1 calc R . . C21 C -0.7051(7) -0.3358(7) -0.2660(6) 0.083(2) Uani 1 1 d . . . H21A H -0.6996 -0.3295 -0.3349 0.124 Uiso 1 1 calc R . . H21B H -0.7399 -0.2650 -0.2463 0.124 Uiso 1 1 calc R . . H21C H -0.7772 -0.3949 -0.2643 0.124 Uiso 1 1 calc R . . C22 C -0.0822(8) 0.0016(6) -0.0820(6) 0.079(2) Uani 1 1 d . . . H22A H -0.1666 0.0433 -0.1295 0.118 Uiso 1 1 calc R . . H22B H 0.0148 0.0381 -0.0763 0.118 Uiso 1 1 calc R . . H22C H -0.0955 -0.0005 -0.0150 0.118 Uiso 1 1 calc R . . C23 C 0.0840(6) -0.2013(6) -0.0291(5) 0.0760(19) Uani 1 1 d . . . H23A H 0.0967 -0.2791 -0.0458 0.114 Uiso 1 1 calc R . . H23B H 0.0662 -0.1976 0.0365 0.114 Uiso 1 1 calc R . . H23C H 0.1765 -0.1593 -0.0250 0.114 Uiso 1 1 calc R . . C24 C -0.0154(7) -0.1296(8) -0.2412(5) 0.0751(19) Uani 1 1 d . . . H24A H -0.0126 -0.2039 -0.2695 0.113 Uiso 1 1 calc R . . H24B H 0.0871 -0.0968 -0.2204 0.113 Uiso 1 1 calc R . . H24C H -0.0861 -0.0822 -0.2928 0.113 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 0.03532(16) 0.03178(16) 0.04668(17) -0.00204(16) 0.01025(11) 0.00492(14) P1 0.0329(6) 0.0467(7) 0.0492(6) 0.0037(5) 0.0040(5) 0.0026(5) P2 0.0507(8) 0.0394(7) 0.0759(9) -0.0036(7) 0.0219(7) -0.0040(7) N1 0.0339(19) 0.038(2) 0.067(2) -0.0067(19) 0.0079(17) 0.0095(16) N2 0.041(2) 0.048(3) 0.103(4) -0.010(3) 0.009(3) 0.018(2) N3 0.052(3) 0.052(3) 0.114(4) -0.023(3) 0.033(3) 0.009(2) N4 0.056(3) 0.054(3) 0.078(3) -0.019(2) 0.034(2) -0.001(2) N5 0.056(3) 0.053(3) 0.071(3) -0.007(2) 0.006(2) 0.014(3) N6 0.131(5) 0.099(5) 0.067(3) 0.001(3) 0.018(3) 0.078(5) C1 0.037(2) 0.030(2) 0.055(3) -0.012(2) 0.009(2) -0.004(2) C2 0.038(2) 0.045(3) 0.060(3) 0.007(2) -0.001(2) 0.003(2) C3 0.051(3) 0.044(3) 0.081(4) 0.017(3) -0.002(3) 0.005(2) C4 0.066(4) 0.066(4) 0.094(5) 0.029(4) 0.007(3) -0.002(3) C5 0.082(5) 0.105(7) 0.082(5) 0.048(5) 0.016(4) 0.001(5) C6 0.091(5) 0.099(6) 0.053(3) 0.010(4) 0.012(3) 0.019(4) C7 0.054(3) 0.063(3) 0.049(3) 0.005(3) 0.000(2) 0.013(3) C8 0.073(4) 0.041(3) 0.130(6) -0.007(4) -0.005(4) 0.003(3) C9 0.078(4) 0.070(4) 0.068(4) -0.018(3) 0.005(3) 0.004(4) C10 0.043(2) 0.038(3) 0.059(3) 0.003(2) 0.010(2) 0.010(2) C11 0.057(3) 0.041(3) 0.072(3) -0.002(2) 0.025(2) 0.004(2) C12 0.050(3) 0.056(3) 0.062(3) -0.001(3) 0.020(2) -0.010(2) C13 0.089(5) 0.089(5) 0.071(4) -0.006(4) 0.035(3) -0.014(4) C14 0.104(6) 0.092(5) 0.100(6) -0.028(5) 0.049(5) 0.007(5) C15 0.074(3) 0.068(5) 0.112(5) -0.016(5) 0.053(3) 0.008(4) C16 0.060(3) 0.049(3) 0.091(4) 0.001(3) 0.036(3) 0.008(3) C17 0.099(5) 0.063(6) 0.115(6) 0.013(4) 0.026(5) 0.044(4) C18 0.089(5) 0.073(4) 0.068(4) 0.016(3) 0.007(3) 0.012(4) C19 0.102(5) 0.104(6) 0.087(5) 0.006(5) 0.039(4) -0.034(5) C20 0.098(6) 0.046(4) 0.200(11) -0.031(5) 0.066(7) -0.022(4) C21 0.052(3) 0.087(5) 0.101(5) -0.020(4) 0.014(3) -0.018(3) C22 0.073(4) 0.053(4) 0.085(4) -0.014(3) -0.008(3) -0.002(3) C23 0.051(3) 0.070(4) 0.084(4) 0.013(3) -0.009(3) 0.004(3) C24 0.047(3) 0.114(6) 0.069(3) 0.013(4) 0.025(3) 0.000(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 2.006(5) . ? Pd1 N5 2.030(5) . ? Pd1 P1 2.3175(14) . ? Pd1 P2 2.3355(16) . ? P1 C22 1.792(7) . ? P1 C23 1.808(6) . ? P1 C24 1.817(6) . ? P2 C19 1.794(8) . ? P2 C21 1.799(7) . ? P2 C20 1.815(8) . ? N1 C1 1.363(7) . ? N1 N2 1.384(6) . ? N1 C2 1.430(7) . ? N2 N3 1.292(8) . ? N3 N4 1.363(7) . ? N4 C1 1.325(7) . ? N5 C10 1.156(7) . ? N6 C10 1.235(8) . ? N6 C11 1.394(8) . ? C2 C7 1.383(8) . ? C2 C3 1.408(8) . ? C3 C4 1.387(10) . ? C3 C8 1.533(10) . ? C4 C5 1.357(13) . ? C5 C6 1.381(12) . ? C6 C7 1.384(10) . ? C7 C9 1.492(9) . ? C11 C16 1.398(8) . ? C11 C12 1.412(8) . ? C12 C13 1.377(9) . ? C12 C18 1.509(9) . ? C13 C14 1.353(11) . ? C14 C15 1.354(11) . ? C15 C16 1.384(9) . ? C16 C17 1.512(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 C1 Pd1 N5 175.6(2) . . ? C1 Pd1 P1 95.92(14) . . ? N5 Pd1 P1 87.04(17) . . ? C1 Pd1 P2 87.28(16) . . ? N5 Pd1 P2 90.17(16) . . ? P1 Pd1 P2 172.72(6) . . ? C22 P1 C23 101.6(3) . . ? C22 P1 C24 106.1(4) . . ? C23 P1 C24 104.1(3) . . ? C22 P1 Pd1 119.0(3) . . ? C23 P1 Pd1 112.6(2) . . ? C24 P1 Pd1 112.0(2) . . ? C19 P2 C21 104.0(4) . . ? C19 P2 C20 106.6(5) . . ? C21 P2 C20 101.4(4) . . ? C19 P2 Pd1 109.5(3) . . ? C21 P2 Pd1 120.0(3) . . ? C20 P2 Pd1 114.3(3) . . ? C1 N1 N2 108.3(5) . . ? C1 N1 C2 132.2(4) . . ? N2 N1 C2 119.0(5) . . ? N3 N2 N1 105.6(5) . . ? N2 N3 N4 111.6(5) . . ? C1 N4 N3 107.0(5) . . ? C10 N5 Pd1 158.2(5) . . ? C10 N6 C11 132.7(6) . . ? N4 C1 N1 107.4(5) . . ? N4 C1 Pd1 124.5(4) . . ? N1 C1 Pd1 127.4(4) . . ? C7 C2 C3 122.1(6) . . ? C7 C2 N1 120.0(5) . . ? C3 C2 N1 117.9(5) . . ? C4 C3 C2 117.4(7) . . ? C4 C3 C8 119.9(7) . . ? C2 C3 C8 122.8(6) . . ? C5 C4 C3 120.5(7) . . ? C4 C5 C6 121.6(8) . . ? C5 C6 C7 119.9(7) . . ? C6 C7 C2 118.2(7) . . ? C6 C7 C9 119.4(6) . . ? C2 C7 C9 122.4(6) . . ? N5 C10 N6 169.7(6) . . ? N6 C11 C16 116.2(5) . . ? N6 C11 C12 123.6(5) . . ? C16 C11 C12 120.1(5) . . ? C13 C12 C11 117.9(6) . . ? C13 C12 C18 120.4(6) . . ? C11 C12 C18 121.6(5) . . ? C14 C13 C12 121.1(7) . . ? C13 C14 C15 122.0(7) . . ? C14 C15 C16 119.7(7) . . ? C15 C16 C11 119.2(6) . . ? C15 C16 C17 119.7(6) . . ? C11 C16 C17 121.0(6) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.330 _refine_diff_density_min -0.406 _refine_diff_density_rms 0.056 data_pd1 _database_code_CSD 167463 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H40 N6 P2 Pd' _chemical_formula_weight 701.06 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 ? _symmetry_space_group_name_H-M ? 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 10.0638(10) _cell_length_b 16.446(3) _cell_length_c 40.816(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6755.5(16) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.379 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2896 _exptl_absorpt_coefficient_mu 0.677 _exptl_absorpt_correction_type ? _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 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5827 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0984 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 25.14 _reflns_number_total 5827 _reflns_number_gt 3044 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0516P)^2^+22.7974P] 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 0.00006(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5827 _refine_ls_number_parameters 389 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1502 _refine_ls_R_factor_gt 0.0669 _refine_ls_wR_factor_ref 0.1717 _refine_ls_wR_factor_gt 0.1344 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _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 0.78139(6) 0.19804(4) 0.107452(14) 0.0463(2) Uani 1 1 d . . . P1 P 0.9604(2) 0.18715(13) 0.07139(5) 0.0496(6) Uani 1 1 d . . . P2 P 0.6248(2) 0.21823(13) 0.14865(5) 0.0512(6) Uani 1 1 d . . . N1 N 0.9180(8) 0.2068(5) 0.14245(18) 0.076(2) Uani 1 1 d . . . N2 N 1.0577(9) 0.1829(5) 0.18963(18) 0.083(3) Uani 1 1 d . . . N3 N 0.5826(9) 0.1250(5) 0.06012(18) 0.068(2) Uani 1 1 d . . . N4 N 0.4634(10) 0.1463(6) 0.0450(2) 0.086(3) Uani 1 1 d . . . N5 N 0.4417(10) 0.2226(6) 0.0525(2) 0.089(3) Uani 1 1 d . . . N6 N 0.5424(10) 0.2499(5) 0.0713(2) 0.082(2) Uani 1 1 d . . . C1 C 1.0782(10) 0.2692(5) 0.0780(2) 0.072(3) Uani 1 1 d . . . H1A H 1.0987 0.2729 0.1010 0.107 Uiso 1 1 calc R . . H1B H 1.0400 0.3195 0.0708 0.107 Uiso 1 1 calc R . . H1C H 1.1580 0.2585 0.0659 0.107 Uiso 1 1 calc R . . C2 C 0.9336(10) 0.1895(6) 0.02765(18) 0.072(3) Uani 1 1 d . . . H2A H 0.8840 0.2373 0.0220 0.108 Uiso 1 1 calc R . . H2B H 0.8849 0.1420 0.0211 0.108 Uiso 1 1 calc R . . H2C H 1.0178 0.1904 0.0166 0.108 Uiso 1 1 calc R . . C3 C 1.0538(9) 0.0950(5) 0.07854(19) 0.053(2) Uani 1 1 d . . . C4 C 1.0168(10) 0.0236(5) 0.0633(2) 0.067(3) Uani 1 1 d . . . H4 H 0.9465 0.0239 0.0486 0.080 Uiso 1 1 calc R . . C5 C 1.0821(13) -0.0474(6) 0.0696(3) 0.084(3) Uani 1 1 d . . . H5 H 1.0559 -0.0948 0.0591 0.101 Uiso 1 1 calc R . . C6 C 1.1848(13) -0.0495(7) 0.0912(4) 0.098(4) Uani 1 1 d . . . H6 H 1.2283 -0.0984 0.0952 0.118 Uiso 1 1 calc R . . C7 C 1.2247(11) 0.0196(8) 0.1069(3) 0.098(4) Uani 1 1 d . . . H7 H 1.2959 0.0179 0.1215 0.118 Uiso 1 1 calc R . . C8 C 1.1583(10) 0.0927(6) 0.1012(2) 0.075(3) Uani 1 1 d . . . H8 H 1.1833 0.1396 0.1123 0.090 Uiso 1 1 calc R . . C9 C 0.6527(10) 0.1542(5) 0.18336(19) 0.068(3) Uani 1 1 d . . . H9A H 0.6512 0.0983 0.1766 0.101 Uiso 1 1 calc R . . H9B H 0.5842 0.1633 0.1993 0.101 Uiso 1 1 calc R . . H9C H 0.7376 0.1666 0.1928 0.101 Uiso 1 1 calc R . . C10 C 0.4478(8) 0.2031(6) 0.1413(2) 0.076(3) Uani 1 1 d . . . H10A H 0.4205 0.2350 0.1228 0.114 Uiso 1 1 calc R . . H10B H 0.3986 0.2196 0.1604 0.114 Uiso 1 1 calc R . . H10C H 0.4311 0.1466 0.1370 0.114 Uiso 1 1 calc R . . C11 C 0.6297(8) 0.3220(5) 0.16400(18) 0.045(2) Uani 1 1 d . . . C12 C 0.5676(10) 0.3828(5) 0.1466(2) 0.074(3) Uani 1 1 d . . . H12 H 0.5286 0.3715 0.1264 0.089 Uiso 1 1 calc R . . C13 C 0.5635(11) 0.4610(6) 0.1592(3) 0.082(3) Uani 1 1 d . . . H13 H 0.5193 0.5017 0.1477 0.098 Uiso 1 1 calc R . . C14 C 0.6224(11) 0.4787(6) 0.1877(3) 0.077(3) Uani 1 1 d . . . H14 H 0.6198 0.5315 0.1959 0.092 Uiso 1 1 calc R . . C15 C 0.6846(12) 0.4204(6) 0.2043(2) 0.087(3) Uani 1 1 d . . . H15 H 0.7253 0.4334 0.2241 0.105 Uiso 1 1 calc R . . C16 C 0.6908(9) 0.3415(6) 0.1932(2) 0.068(3) Uani 1 1 d . . . H16 H 0.7354 0.3020 0.2052 0.081 Uiso 1 1 calc R . . C17 C 0.9893(9) 0.1999(5) 0.1643(2) 0.057(2) Uani 1 1 d . . . C18 C 1.1679(9) 0.2204(5) 0.20364(19) 0.056(2) Uani 1 1 d . . . C19 C 1.1968(9) 0.3032(6) 0.19949(19) 0.061(2) Uani 1 1 d . . . C20 C 1.3086(10) 0.3342(7) 0.2153(2) 0.078(3) Uani 1 1 d . . . H20 H 1.3307 0.3887 0.2127 0.094 Uiso 1 1 calc R . . C21 C 1.3878(11) 0.2848(10) 0.2349(2) 0.093(4) Uani 1 1 d . . . H21 H 1.4620 0.3062 0.2454 0.112 Uiso 1 1 calc R . . C22 C 1.3561(11) 0.2052(8) 0.2386(2) 0.080(3) Uani 1 1 d . . . H22 H 1.4089 0.1728 0.2520 0.096 Uiso 1 1 calc R . . C23 C 1.2483(10) 0.1710(6) 0.2232(2) 0.068(3) Uani 1 1 d . . . C24 C 1.2184(14) 0.0832(6) 0.2269(2) 0.106(4) Uani 1 1 d . . . H24A H 1.1400 0.0700 0.2146 0.159 Uiso 1 1 calc R . . H24B H 1.2040 0.0710 0.2496 0.159 Uiso 1 1 calc R . . H24C H 1.2919 0.0518 0.2189 0.159 Uiso 1 1 calc R . . C25 C 1.1110(13) 0.3593(6) 0.1802(3) 0.107(4) Uani 1 1 d . . . H25A H 1.0382 0.3294 0.1710 0.160 Uiso 1 1 calc R . . H25B H 1.1622 0.3837 0.1630 0.160 Uiso 1 1 calc R . . H25C H 1.0771 0.4011 0.1944 0.160 Uiso 1 1 calc R . . C26 C 0.6353(9) 0.1902(6) 0.07551(19) 0.061(2) Uani 1 1 d . . . C27 C 0.6383(10) 0.0465(5) 0.0512(2) 0.063(3) Uani 1 1 d . . . C28 C 0.6685(9) 0.0329(6) 0.0179(2) 0.063(2) Uani 1 1 d . . . C29 C 0.7228(11) -0.0411(6) 0.0105(2) 0.076(3) Uani 1 1 d . . . H29 H 0.7433 -0.0522 -0.0112 0.091 Uiso 1 1 calc R . . C30 C 0.7479(10) -0.0984(6) 0.0331(3) 0.075(3) Uani 1 1 d . . . H30 H 0.7870 -0.1473 0.0269 0.090 Uiso 1 1 calc R . . C31 C 0.7159(10) -0.0849(5) 0.0651(2) 0.068(3) Uani 1 1 d . . . H31 H 0.7320 -0.1255 0.0805 0.082 Uiso 1 1 calc R . . C32 C 0.6605(9) -0.0126(5) 0.0751(2) 0.059(2) Uani 1 1 d . . . C33 C 0.6404(10) 0.0960(6) -0.0077(2) 0.082(3) Uani 1 1 d . . . H33A H 0.6016 0.1430 0.0025 0.123 Uiso 1 1 calc R . . H33B H 0.5797 0.0742 -0.0236 0.123 Uiso 1 1 calc R . . H33C H 0.7218 0.1111 -0.0183 0.123 Uiso 1 1 calc R . . C34 C 0.6243(11) 0.0006(6) 0.1100(2) 0.084(3) Uani 1 1 d . . . H34A H 0.5877 0.0541 0.1126 0.126 Uiso 1 1 calc R . . H34B H 0.7021 -0.0047 0.1234 0.126 Uiso 1 1 calc R . . H34C H 0.5596 -0.0392 0.1165 0.126 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 0.0454(4) 0.0503(4) 0.0431(3) -0.0039(3) -0.0017(3) 0.0044(4) P1 0.0491(13) 0.0444(12) 0.0554(12) 0.0017(11) 0.0062(11) -0.0016(11) P2 0.0504(14) 0.0560(14) 0.0472(12) -0.0082(10) 0.0032(11) 0.0023(11) N1 0.067(5) 0.106(7) 0.056(4) -0.011(5) -0.011(4) -0.024(5) N2 0.104(7) 0.080(6) 0.064(5) 0.011(4) -0.031(5) -0.034(5) N3 0.077(6) 0.076(6) 0.051(4) 0.001(4) 0.007(4) 0.034(5) N4 0.088(7) 0.088(7) 0.081(6) -0.009(5) -0.008(5) 0.001(6) N5 0.104(8) 0.078(6) 0.085(6) -0.002(5) -0.011(6) 0.027(6) N6 0.093(7) 0.089(6) 0.064(5) -0.004(5) -0.005(5) 0.011(6) C1 0.087(7) 0.046(5) 0.082(7) 0.002(5) 0.008(6) -0.018(5) C2 0.080(7) 0.081(7) 0.055(5) 0.005(5) 0.015(5) -0.002(6) C3 0.055(6) 0.053(5) 0.051(5) 0.003(4) 0.019(5) -0.003(5) C4 0.068(7) 0.053(6) 0.080(7) -0.003(5) 0.012(6) 0.002(5) C5 0.096(10) 0.061(7) 0.095(8) -0.012(6) 0.021(8) -0.007(7) C6 0.081(10) 0.063(7) 0.150(12) 0.023(8) 0.048(9) 0.022(7) C7 0.063(7) 0.101(9) 0.132(10) 0.029(8) -0.015(8) 0.008(7) C8 0.062(6) 0.058(6) 0.106(8) -0.004(6) -0.023(6) -0.001(5) C9 0.089(7) 0.056(5) 0.059(5) -0.003(4) 0.021(5) 0.003(5) C10 0.055(6) 0.091(7) 0.084(7) -0.019(6) -0.002(5) -0.010(6) C11 0.044(5) 0.048(5) 0.044(4) -0.007(4) 0.003(4) 0.001(4) C12 0.102(8) 0.054(6) 0.066(6) -0.003(5) -0.013(6) 0.018(6) C13 0.089(8) 0.049(6) 0.107(9) 0.002(6) -0.005(7) 0.016(6) C14 0.085(8) 0.042(5) 0.104(8) -0.012(6) 0.005(7) -0.009(6) C15 0.120(10) 0.068(7) 0.073(6) -0.022(6) -0.021(7) -0.006(7) C16 0.083(8) 0.057(5) 0.063(5) -0.015(5) -0.020(5) 0.004(5) C17 0.056(6) 0.058(5) 0.056(5) -0.021(5) 0.015(5) -0.014(5) C18 0.059(6) 0.068(6) 0.042(4) -0.004(4) -0.003(4) -0.004(5) C19 0.059(6) 0.073(6) 0.052(5) 0.001(5) 0.002(4) -0.012(6) C20 0.078(8) 0.087(7) 0.071(6) -0.028(6) 0.009(6) -0.036(6) C21 0.059(7) 0.162(13) 0.060(6) -0.031(8) -0.005(6) -0.013(9) C22 0.067(7) 0.116(9) 0.056(6) -0.008(6) -0.004(5) 0.019(8) C23 0.065(7) 0.089(7) 0.050(5) -0.008(5) -0.006(5) 0.008(5) C24 0.151(12) 0.078(7) 0.090(7) 0.014(6) -0.025(8) 0.006(8) C25 0.156(12) 0.058(6) 0.106(9) 0.005(6) -0.030(9) -0.005(8) C26 0.061(6) 0.075(6) 0.047(5) -0.005(5) -0.002(4) 0.025(6) C27 0.067(7) 0.058(6) 0.064(6) -0.002(5) -0.003(5) 0.011(5) C28 0.062(6) 0.073(6) 0.054(5) -0.001(5) 0.000(5) 0.008(5) C29 0.082(8) 0.074(7) 0.072(6) -0.018(5) 0.010(6) -0.010(7) C30 0.079(8) 0.047(5) 0.100(7) -0.013(5) -0.002(7) -0.006(5) C31 0.088(7) 0.054(5) 0.062(5) 0.001(5) -0.004(6) -0.015(6) C32 0.061(6) 0.054(5) 0.063(6) 0.001(5) 0.003(5) 0.001(5) C33 0.078(7) 0.124(9) 0.044(5) 0.011(6) 0.003(5) 0.010(7) C34 0.106(9) 0.073(7) 0.073(7) 0.013(6) 0.008(7) 0.002(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C26 1.969(9) . ? Pd1 N1 1.988(8) . ? Pd1 P2 2.329(2) . ? Pd1 P1 2.334(2) . ? P1 C2 1.806(8) . ? P1 C3 1.807(9) . ? P1 C1 1.816(8) . ? P2 C9 1.787(8) . ? P2 C11 1.819(7) . ? P2 C10 1.823(8) . ? N1 C17 1.150(11) . ? N2 C17 1.274(11) . ? N2 C18 1.392(11) . ? N3 C26 1.352(11) . ? N3 N4 1.393(10) . ? N3 C27 1.454(10) . ? N4 N5 1.309(11) . ? N5 N6 1.350(11) . ? N6 C26 1.367(11) . ? C3 C4 1.379(11) . ? C3 C8 1.401(12) . ? C4 C5 1.364(13) . ? C5 C6 1.357(15) . ? C6 C7 1.367(16) . ? C7 C8 1.395(14) . ? C11 C12 1.377(11) . ? C11 C16 1.380(10) . ? C12 C13 1.385(12) . ? C13 C14 1.339(13) . ? C14 C15 1.332(13) . ? C15 C16 1.375(12) . ? C18 C23 1.398(12) . ? C18 C19 1.404(12) . ? C19 C20 1.393(12) . ? C19 C25 1.489(13) . ? C20 C21 1.391(15) . ? C21 C22 1.356(14) . ? C22 C23 1.374(14) . ? C23 C24 1.482(13) . ? C27 C32 1.397(11) . ? C27 C28 1.409(11) . ? C28 C29 1.368(12) . ? C28 C33 1.498(12) . ? C29 C30 1.341(13) . ? C30 C31 1.365(12) . ? C31 C32 1.376(12) . ? C32 C34 1.485(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C26 Pd1 N1 175.5(3) . . ? C26 Pd1 P2 89.0(3) . . ? N1 Pd1 P2 86.5(2) . . ? C26 Pd1 P1 98.9(2) . . ? N1 Pd1 P1 85.7(2) . . ? P2 Pd1 P1 171.54(8) . . ? C2 P1 C3 104.8(4) . . ? C2 P1 C1 103.3(4) . . ? C3 P1 C1 105.1(4) . . ? C2 P1 Pd1 120.4(3) . . ? C3 P1 Pd1 111.3(3) . . ? C1 P1 Pd1 110.6(3) . . ? C9 P2 C11 106.0(4) . . ? C9 P2 C10 101.7(5) . . ? C11 P2 C10 102.2(4) . . ? C9 P2 Pd1 112.5(3) . . ? C11 P2 Pd1 111.4(3) . . ? C10 P2 Pd1 121.6(3) . . ? C17 N1 Pd1 168.9(8) . . ? C17 N2 C18 131.9(8) . . ? C26 N3 N4 110.1(8) . . ? C26 N3 C27 132.1(9) . . ? N4 N3 C27 116.4(8) . . ? N5 N4 N3 106.4(9) . . ? N4 N5 N6 109.0(9) . . ? N5 N6 C26 110.2(8) . . ? C4 C3 C8 118.5(9) . . ? C4 C3 P1 120.1(7) . . ? C8 C3 P1 121.3(7) . . ? C5 C4 C3 120.9(10) . . ? C6 C5 C4 120.8(11) . . ? C5 C6 C7 120.5(11) . . ? C6 C7 C8 119.8(11) . . ? C7 C8 C3 119.6(10) . . ? C12 C11 C16 118.6(8) . . ? C12 C11 P2 119.4(6) . . ? C16 C11 P2 121.9(6) . . ? C11 C12 C13 119.7(9) . . ? C14 C13 C12 120.8(10) . . ? C15 C14 C13 119.6(9) . . ? C14 C15 C16 122.2(10) . . ? C15 C16 C11 119.0(9) . . ? N1 C17 N2 171.4(10) . . ? N2 C18 C23 116.0(9) . . ? N2 C18 C19 123.1(8) . . ? C23 C18 C19 120.9(9) . . ? C20 C19 C18 117.8(9) . . ? C20 C19 C25 119.1(10) . . ? C18 C19 C25 123.0(9) . . ? C21 C20 C19 121.1(10) . . ? C22 C21 C20 119.5(11) . . ? C21 C22 C23 122.0(11) . . ? C22 C23 C18 118.7(10) . . ? C22 C23 C24 120.8(10) . . ? C18 C23 C24 120.4(9) . . ? N3 C26 N6 104.1(8) . . ? N3 C26 Pd1 130.7(7) . . ? N6 C26 Pd1 123.1(8) . . ? C32 C27 C28 122.0(8) . . ? C32 C27 N3 120.2(8) . . ? C28 C27 N3 117.8(8) . . ? C29 C28 C27 116.0(9) . . ? C29 C28 C33 122.6(9) . . ? C27 C28 C33 121.4(8) . . ? C30 C29 C28 123.4(9) . . ? C29 C30 C31 119.9(9) . . ? C30 C31 C32 121.4(9) . . ? C31 C32 C27 117.3(8) . . ? C31 C32 C34 120.7(8) . . ? C27 C32 C34 122.0(8) . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 25.14 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 1.279 _refine_diff_density_min -1.165 _refine_diff_density_rms 0.094 data_pdcnr _database_code_CSD 167464 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H36 N8 P2 Pd' _chemical_formula_weight 508.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.3758(8) _cell_length_b 15.6567(13) _cell_length_c 12.6709(15) _cell_angle_alpha 90.00 _cell_angle_beta 92.422(9) _cell_angle_gamma 90.00 _cell_volume 1263.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.337 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 528 _exptl_absorpt_coefficient_mu 0.877 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2399 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0280 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2192 _reflns_number_gt 2009 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+0.7286P] 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 0.0089(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2192 _refine_ls_number_parameters 125 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0308 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0784 _refine_ls_wR_factor_gt 0.0760 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.022 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.0000 0.5000 0.5000 0.03311(13) Uani 1 d S . . P1 P 0.13054(11) 0.39761(4) 0.38945(5) 0.04083(18) Uani 1 d . . . N1 N 0.0357(4) 0.63836(15) 0.33267(18) 0.0508(6) Uani 1 d . . . N2 N 0.1651(5) 0.70108(17) 0.3014(2) 0.0720(8) Uani 1 d . . . N3 N 0.3310(5) 0.69592(19) 0.3615(3) 0.0758(8) Uani 1 d . . . N4 N 0.3137(4) 0.63206(16) 0.4340(2) 0.0620(7) Uani 1 d . . . C1 C 0.2105(5) 0.29715(18) 0.4485(2) 0.0608(8) Uani 1 d . . . H1A H 0.0995 0.2753 0.4897 0.091 Uiso 1 calc R . . H1B H 0.3339 0.3057 0.4933 0.091 Uiso 1 calc R . . H1C H 0.2408 0.2570 0.3939 0.091 Uiso 1 calc R . . C2 C -0.0654(6) 0.3656(2) 0.2896(3) 0.0705(10) Uani 1 d . . . H2A H -0.1188 0.4153 0.2530 0.106 Uiso 1 calc R . . H2B H -0.1784 0.3369 0.3227 0.106 Uiso 1 calc R . . H2C H -0.0031 0.3277 0.2403 0.106 Uiso 1 calc R . . C3 C 0.3572(6) 0.4272(2) 0.3169(3) 0.0734(10) Uani 1 d . . . H3A H 0.3311 0.4808 0.2818 0.110 Uiso 1 calc R . . H3B H 0.3840 0.3840 0.2655 0.110 Uiso 1 calc R . . H3C H 0.4771 0.4327 0.3649 0.110 Uiso 1 calc R . . C4 C 0.1268(4) 0.59606(16) 0.4154(2) 0.0423(6) Uani 1 d . . . C5 C -0.1698(6) 0.6276(3) 0.2823(3) 0.0713(9) Uani 1 d . . . H5A H -0.2548 0.6775 0.2955 0.086 Uiso 1 calc R . . H5B H -0.2379 0.5784 0.3123 0.086 Uiso 1 calc R . . C6 C -0.1545(9) 0.6150(4) 0.1623(4) 0.1159(17) Uani 1 d . . . H6A H -0.0964 0.6664 0.1324 0.139 Uiso 1 calc R . . H6B H -0.0577 0.5686 0.1501 0.139 Uiso 1 calc R . . C7 C -0.3528(11) 0.5962(4) 0.1074(4) 0.144(2) Uani 1 d . . . H7A H -0.4543 0.6408 0.1201 0.173 Uiso 1 calc R . . H7B H -0.4084 0.5423 0.1313 0.173 Uiso 1 calc R . . C8 C -0.3070(19) 0.5916(5) -0.0122(5) 0.214(5) Uani 1 d . . . H8A H -0.4340 0.5777 -0.0520 0.321 Uiso 1 calc R . . H8B H -0.2036 0.5483 -0.0232 0.321 Uiso 1 calc R . . H8C H -0.2553 0.6458 -0.0351 0.321 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.03966(19) 0.02841(18) 0.03199(18) 0.00017(8) 0.01017(11) 0.00016(9) P1 0.0453(4) 0.0377(3) 0.0403(3) -0.0068(3) 0.0111(3) 0.0035(3) N1 0.0634(14) 0.0457(12) 0.0441(12) 0.0114(10) 0.0129(11) -0.0038(11) N2 0.092(2) 0.0551(16) 0.0704(18) 0.0254(13) 0.0243(16) -0.0115(15) N3 0.0765(19) 0.0646(18) 0.088(2) 0.0217(15) 0.0179(17) -0.0205(15) N4 0.0576(15) 0.0536(14) 0.0757(17) 0.0121(12) 0.0108(13) -0.0114(12) C1 0.078(2) 0.0458(16) 0.0596(18) -0.0077(13) 0.0088(15) 0.0156(14) C2 0.071(2) 0.074(2) 0.065(2) -0.0290(17) -0.0114(16) 0.0153(17) C3 0.072(2) 0.071(2) 0.080(2) -0.0136(17) 0.0426(18) -0.0023(16) C4 0.0477(14) 0.0356(13) 0.0445(13) 0.0005(11) 0.0137(11) 0.0012(11) C5 0.080(2) 0.076(2) 0.0575(19) 0.0194(16) -0.0044(16) -0.0029(18) C6 0.140(4) 0.132(4) 0.074(3) 0.021(3) -0.017(3) -0.033(3) C7 0.177(6) 0.152(6) 0.100(4) 0.020(4) -0.034(4) -0.012(5) C8 0.394(15) 0.174(7) 0.070(3) 0.008(4) -0.040(6) -0.026(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C4 2.034(3) 3_566 ? Pd1 C4 2.034(3) . ? Pd1 P1 2.3072(6) 3_566 ? Pd1 P1 2.3072(6) . ? P1 C3 1.806(3) . ? P1 C1 1.806(3) . ? P1 C2 1.811(3) . ? N1 C4 1.350(4) . ? N1 N2 1.352(3) . ? N1 C5 1.443(4) . ? N2 N3 1.280(4) . ? N3 N4 1.365(4) . ? N4 C4 1.331(4) . ? C5 C6 1.540(6) . ? C6 C7 1.447(8) . ? C7 C8 1.557(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 C4 Pd1 C4 180.0 3_566 . ? C4 Pd1 P1 91.84(8) 3_566 3_566 ? C4 Pd1 P1 88.16(8) . 3_566 ? C4 Pd1 P1 88.16(8) 3_566 . ? C4 Pd1 P1 91.84(8) . . ? P1 Pd1 P1 180.0 3_566 . ? C3 P1 C1 102.50(17) . . ? C3 P1 C2 105.01(18) . . ? C1 P1 C2 102.88(17) . . ? C3 P1 Pd1 116.58(11) . . ? C1 P1 Pd1 117.16(10) . . ? C2 P1 Pd1 111.12(11) . . ? C4 N1 N2 109.6(3) . . ? C4 N1 C5 129.7(2) . . ? N2 N1 C5 120.6(3) . . ? N3 N2 N1 106.2(2) . . ? N2 N3 N4 111.0(2) . . ? C4 N4 N3 106.8(3) . . ? N4 C4 N1 106.4(2) . . ? N4 C4 Pd1 126.3(2) . . ? N1 C4 Pd1 127.2(2) . . ? N1 C5 C6 111.0(3) . . ? C7 C6 C5 114.2(5) . . ? C6 C7 C8 106.4(6) . . ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 0.621 _refine_diff_density_min -0.379 _refine_diff_density_rms 0.059 data_lsc296 _database_code_CSD 167465 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H36 N8 P2 Pt' _chemical_formula_weight 597.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.3686(8) _cell_length_b 15.6425(14) _cell_length_c 12.6859(14) _cell_angle_alpha 90.00 _cell_angle_beta 92.498(10) _cell_angle_gamma 90.00 _cell_volume 1262.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.572 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 5.700 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2382 _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_sigmaI/netI 0.0397 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2174 _reflns_number_gt 1607 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0282P)^2^+1.5251P] 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(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2174 _refine_ls_number_parameters 125 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0478 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0788 _refine_ls_wR_factor_gt 0.0705 _refine_ls_goodness_of_fit_ref 1.133 _refine_ls_restrained_S_all 1.133 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.0000 0.0000 0.0000 0.03404(14) Uani 1 2 d S . . P1 P 0.1302(3) 0.10165(11) -0.11118(13) 0.0417(4) Uani 1 1 d . . . N1 N 0.0338(10) -0.1389(4) -0.1670(4) 0.0497(14) Uani 1 1 d . . . N2 N 0.1607(12) -0.2009(4) -0.2000(5) 0.073(2) Uani 1 1 d . . . N3 N 0.3290(12) -0.1974(4) -0.1393(6) 0.080(2) Uani 1 1 d . . . N4 N 0.3119(10) -0.1324(4) -0.0656(5) 0.0603(16) Uani 1 1 d . . . C1 C 0.3564(13) 0.0708(5) -0.1839(6) 0.075(2) Uani 1 1 d . . . H1A H 0.3277 0.0177 -0.2198 0.113 Uiso 1 1 calc R . . H1B H 0.4759 0.0639 -0.1359 0.113 Uiso 1 1 calc R . . H1C H 0.3855 0.1143 -0.2346 0.113 Uiso 1 1 calc R . . C2 C 0.2125(13) 0.2013(4) -0.0507(6) 0.062(2) Uani 1 1 d . . . H2A H 0.3184 0.1904 0.0038 0.093 Uiso 1 1 calc R . . H2B H 0.0939 0.2286 -0.0207 0.093 Uiso 1 1 calc R . . H2C H 0.2688 0.2381 -0.1031 0.093 Uiso 1 1 calc R . . C3 C -0.0646(13) 0.1345(5) -0.2102(6) 0.068(2) Uani 1 1 d . . . H3A H -0.1179 0.0851 -0.2476 0.102 Uiso 1 1 calc R . . H3B H -0.0019 0.1728 -0.2589 0.102 Uiso 1 1 calc R . . H3C H -0.1778 0.1629 -0.1770 0.102 Uiso 1 1 calc R . . C4 C 0.1234(10) -0.0964(4) -0.0851(4) 0.0402(14) Uani 1 1 d . . . C5 C -0.1739(14) -0.1269(5) -0.2183(6) 0.068(2) Uani 1 1 d . . . H5A H -0.2406 -0.0770 -0.1891 0.081 Uiso 1 1 calc R . . H5B H -0.2612 -0.1762 -0.2053 0.081 Uiso 1 1 calc R . . C6 C -0.1538(19) -0.1151(8) -0.3379(7) 0.120(4) Uani 1 1 d . . . H6A H -0.0548 -0.0693 -0.3494 0.144 Uiso 1 1 calc R . . H6B H -0.0957 -0.1670 -0.3666 0.144 Uiso 1 1 calc R . . C7 C -0.334(3) -0.0973(10) -0.3912(9) 0.189(8) Uani 1 1 d . . . H7A H -0.3871 -0.0432 -0.3663 0.227 Uiso 1 1 calc R . . H7B H -0.4360 -0.1411 -0.3765 0.227 Uiso 1 1 calc R . . C8 C -0.310(4) -0.0918(10) -0.5133(8) 0.228(10) Uani 1 1 d . . . H8A H -0.4440 -0.0801 -0.5475 0.341 Uiso 1 1 calc R . . H8B H -0.2567 -0.1451 -0.5386 0.341 Uiso 1 1 calc R . . H8C H -0.2133 -0.0467 -0.5288 0.341 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 0.04197(19) 0.02691(18) 0.03405(19) 0.00008(15) 0.01093(11) -0.00023(18) P1 0.0487(10) 0.0356(8) 0.0418(8) 0.0058(8) 0.0127(7) -0.0051(8) N1 0.056(4) 0.046(3) 0.048(3) -0.012(3) 0.009(3) 0.001(3) N2 0.092(5) 0.058(4) 0.070(4) -0.026(3) 0.024(4) 0.012(4) N3 0.091(6) 0.060(4) 0.091(5) -0.021(4) 0.023(4) 0.029(4) N4 0.053(4) 0.053(4) 0.076(4) -0.009(3) 0.015(3) 0.011(3) C1 0.077(6) 0.070(5) 0.082(5) 0.010(4) 0.042(5) -0.005(4) C2 0.089(6) 0.041(4) 0.057(4) 0.003(3) 0.009(4) -0.018(4) C3 0.062(5) 0.071(5) 0.071(5) 0.029(4) -0.008(4) -0.016(4) C4 0.048(4) 0.031(3) 0.043(3) -0.002(3) 0.014(3) -0.005(3) C5 0.079(6) 0.065(5) 0.060(4) -0.018(4) -0.001(4) 0.000(5) C6 0.152(11) 0.131(10) 0.073(6) -0.011(7) -0.043(7) 0.040(9) C7 0.30(2) 0.168(14) 0.093(9) -0.002(10) -0.038(12) -0.007(16) C8 0.44(3) 0.180(16) 0.061(7) 0.000(9) -0.018(12) 0.02(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C4 2.033(6) 3 ? Pt1 C4 2.033(6) . ? Pt1 P1 2.3037(16) . ? Pt1 P1 2.3037(16) 3 ? P1 C3 1.802(8) . ? P1 C2 1.806(6) . ? P1 C1 1.810(7) . ? N1 C4 1.340(8) . ? N1 N2 1.341(8) . ? N1 C5 1.460(10) . ? N2 N3 1.294(9) . ? N3 N4 1.389(8) . ? N4 C4 1.338(8) . ? C5 C6 1.539(11) . ? C6 C7 1.333(17) . ? C7 C8 1.566(15) . ? 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 C4 Pt1 C4 180.0(4) 3 . ? C4 Pt1 P1 88.32(17) 3 . ? C4 Pt1 P1 91.68(17) . . ? C4 Pt1 P1 91.68(17) 3 3 ? C4 Pt1 P1 88.32(17) . 3 ? P1 Pt1 P1 180.00(8) . 3 ? C3 P1 C2 103.2(4) . . ? C3 P1 C1 105.0(4) . . ? C2 P1 C1 103.0(4) . . ? C3 P1 Pt1 111.6(3) . . ? C2 P1 Pt1 116.2(2) . . ? C1 P1 Pt1 116.3(3) . . ? C4 N1 N2 111.0(6) . . ? C4 N1 C5 129.0(6) . . ? N2 N1 C5 120.0(6) . . ? N3 N2 N1 106.2(6) . . ? N2 N3 N4 110.1(6) . . ? C4 N4 N3 106.2(6) . . ? N4 C4 N1 106.5(6) . . ? N4 C4 Pt1 125.3(5) . . ? N1 C4 Pt1 128.2(5) . . ? N1 C5 C6 110.0(7) . . ? C7 C6 C5 114.7(12) . . ? C6 C7 C8 113.2(16) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.890 _refine_diff_density_min -0.682 _refine_diff_density_rms 0.103 data_ptcnr3 _database_code_CSD 167466 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H48 N8 P2 Pt' _chemical_formula_weight 681.71 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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1528(15) _cell_length_b 11.8719(16) _cell_length_c 12.910(2) _cell_angle_alpha 94.864(9) _cell_angle_beta 102.154(8) _cell_angle_gamma 93.323(9) _cell_volume 1511.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 4.773 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5584 _diffrn_reflns_av_R_equivalents 0.0190 _diffrn_reflns_av_sigmaI/netI 0.0388 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5261 _reflns_number_gt 4784 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0431P)^2^+0.4293P] 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 0.0000(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5261 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0349 _refine_ls_R_factor_gt 0.0295 _refine_ls_wR_factor_ref 0.0745 _refine_ls_wR_factor_gt 0.0719 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 1.797 _refine_ls_shift/su_mean 0.006 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt Pt 0.213496(16) 0.688252(14) 0.807257(12) 0.04045(8) Uani 1 d . . . P1 P 0.19973(13) 0.68709(11) 0.98324(9) 0.0479(3) Uani 1 d . . . P2 P 0.23925(14) 0.65065(12) 0.63503(10) 0.0535(3) Uani 1 d . . . N1 N -0.0935(5) 0.6374(5) 0.7419(4) 0.0673(13) Uani 1 d . . . N2 N -0.1901(6) 0.5514(7) 0.7124(4) 0.0868(18) Uani 1 d . . . N3 N -0.1296(7) 0.4603(6) 0.7155(4) 0.0834(18) Uani 1 d . . . N4 N 0.0085(5) 0.4835(4) 0.7468(4) 0.0667(12) Uani 1 d . . . N5 N 0.5187(4) 0.7392(4) 0.8696(4) 0.0629(11) Uani 1 d . . . N6 N 0.6114(5) 0.8304(6) 0.8910(4) 0.0763(15) Uani 1 d . . . N7 N 0.5528(5) 0.9229(5) 0.8840(5) 0.0782(15) Uani 1 d . . . N8 N 0.4181(5) 0.8914(4) 0.8573(4) 0.0595(11) Uani 1 d . . . C1 C 0.1931(6) 0.5413(4) 1.0158(4) 0.0584(12) Uani 1 d . . . H1A H 0.1829 0.5404 1.0888 0.070 Uiso 1 calc R . . H1B H 0.1142 0.4997 0.9700 0.070 Uiso 1 calc R . . C2 C 0.3187(9) 0.4812(8) 1.0033(8) 0.119(3) Uani 1 d . . . H2A H 0.3190 0.4670 0.9290 0.178 Uiso 1 calc R . . H2B H 0.3179 0.4106 1.0343 0.178 Uiso 1 calc R . . H2C H 0.3982 0.5283 1.0386 0.178 Uiso 1 calc R . . C3 C 0.0498(7) 0.7382(5) 1.0212(5) 0.0674(15) Uani 1 d . . . H3A H -0.0294 0.6984 0.9741 0.081 Uiso 1 calc R . . H3B H 0.0495 0.7198 1.0929 0.081 Uiso 1 calc R . . C4 C 0.0390(10) 0.8643(6) 1.0175(7) 0.109(3) Uani 1 d . . . H4A H 0.1038 0.9045 1.0758 0.163 Uiso 1 calc R . . H4B H -0.0504 0.8824 1.0230 0.163 Uiso 1 calc R . . H4C H 0.0566 0.8860 0.9515 0.163 Uiso 1 calc R . . C5 C 0.3394(7) 0.7638(6) 1.0796(4) 0.081(2) Uani 1 d . . . H5A H 0.4231 0.7349 1.0679 0.097 Uiso 1 calc R . . H5B H 0.3419 0.8430 1.0662 0.097 Uiso 1 calc R . . C6 C 0.3340(8) 0.7566(8) 1.1976(5) 0.104(3) Uani 1 d . . . H6A H 0.4040 0.8076 1.2422 0.155 Uiso 1 calc R . . H6B H 0.3469 0.6806 1.2153 0.155 Uiso 1 calc R . . H6C H 0.2476 0.7773 1.2087 0.155 Uiso 1 calc R . . C7 C 0.3813(6) 0.7262(5) 0.5986(4) 0.0649(14) Uani 1 d . . . H7A H 0.3679 0.8066 0.6033 0.078 Uiso 1 calc R . . H7B H 0.4629 0.7157 0.6502 0.078 Uiso 1 calc R . . C8 C 0.4030(7) 0.6897(7) 0.4867(5) 0.096(2) Uani 1 d . . . H8A H 0.4796 0.7335 0.4742 0.144 Uiso 1 calc R . . H8B H 0.3240 0.7019 0.4344 0.144 Uiso 1 calc R . . H8C H 0.4190 0.6107 0.4814 0.144 Uiso 1 calc R . . C9 C 0.0947(7) 0.6713(8) 0.5311(5) 0.095(3) Uani 1 d . . . H9A H 0.1081 0.6366 0.4637 0.114 Uiso 1 calc R . . H9B H 0.0147 0.6330 0.5459 0.114 Uiso 1 calc R . . C10 C 0.0712(9) 0.7946(11) 0.5210(8) 0.148(5) Uani 1 d . . . H10A H -0.0109 0.8002 0.4696 0.222 Uiso 1 calc R . . H10B H 0.1456 0.8311 0.4982 0.222 Uiso 1 calc R . . H10C H 0.0641 0.8308 0.5887 0.222 Uiso 1 calc R . . C11 C 0.2653(9) 0.5002(6) 0.6136(6) 0.094(2) Uani 1 d . . . H11A H 0.1891 0.4555 0.6277 0.113 Uiso 1 calc R . . H11B H 0.2688 0.4815 0.5397 0.113 Uiso 1 calc R . . C12 C 0.3970(12) 0.4687(9) 0.6859(9) 0.134(4) Uani 1 d . . . H12A H 0.4732 0.5085 0.6684 0.202 Uiso 1 calc R . . H12B H 0.4043 0.3885 0.6751 0.202 Uiso 1 calc R . . H12C H 0.3954 0.4897 0.7591 0.202 Uiso 1 calc R . . C13 C 0.0297(5) 0.5956(4) 0.7633(3) 0.0509(11) Uani 1 d . . . C14 C -0.1289(7) 0.7550(7) 0.7508(6) 0.088(2) Uani 1 d . . . H14A H -0.0462 0.8045 0.7665 0.105 Uiso 1 calc R . . H14B H -0.1725 0.7665 0.8104 0.105 Uiso 1 calc R . . C15 C -0.2198(7) 0.7893(7) 0.6537(7) 0.095(2) Uani 1 d . . . H15A H -0.3074 0.7476 0.6427 0.114 Uiso 1 calc R . . H15B H -0.1820 0.7703 0.5920 0.114 Uiso 1 calc R . . C16 C -0.2374(10) 0.9179(10) 0.6647(8) 0.129(4) Uani 1 d . . . H16A H -0.2736 0.9356 0.7274 0.155 Uiso 1 calc R . . H16B H -0.1488 0.9582 0.6768 0.155 Uiso 1 calc R . . C17 C -0.3249(11) 0.9613(10) 0.5741(10) 0.164(5) Uani 1 d . . . H17A H -0.3158 1.0427 0.5826 0.246 Uiso 1 calc R . . H17B H -0.4171 0.9352 0.5706 0.246 Uiso 1 calc R . . H17C H -0.2991 0.9345 0.5095 0.246 Uiso 1 calc R . . C18 C 0.3962(5) 0.7787(4) 0.8479(3) 0.0469(10) Uani 1 d . . . C19 C 0.3193(7) 0.9797(5) 0.8480(6) 0.0781(17) Uani 1 d . . . H19A H 0.2301 0.9446 0.8463 0.094 Uiso 1 calc R . . H19B H 0.3437 1.0348 0.9101 0.094 Uiso 1 calc R . . C20 C 0.3153(11) 1.0366(10) 0.7544(9) 0.146(4) Uani 1 d . . . H20A H 0.3015 0.9812 0.6926 0.175 Uiso 1 calc R . . H20B H 0.4009 1.0800 0.7599 0.175 Uiso 1 calc R . . C21 C 0.196(2) 1.1194(14) 0.7401(15) 0.255(12) Uani 1 d . . . H21A H 0.1743 1.1353 0.6662 0.306 Uiso 1 calc R . . H21B H 0.1164 1.0793 0.7542 0.306 Uiso 1 calc R . . C22 C 0.2161(17) 1.2066(14) 0.7940(15) 0.230(10) Uani 1 d . . . H22A H 0.1315 1.2376 0.7971 0.345 Uiso 1 calc R . . H22B H 0.2704 1.2585 0.7642 0.345 Uiso 1 calc R . . H22C H 0.2628 1.1948 0.8645 0.345 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt 0.04124(12) 0.04308(11) 0.03677(11) 0.00147(6) 0.00989(7) -0.00050(7) P1 0.0554(7) 0.0498(7) 0.0391(6) 0.0030(5) 0.0141(5) -0.0038(6) P2 0.0509(7) 0.0668(8) 0.0412(6) -0.0059(6) 0.0151(5) -0.0099(6) N1 0.046(3) 0.092(4) 0.061(3) -0.005(2) 0.010(2) -0.006(2) N2 0.056(3) 0.135(6) 0.060(3) -0.008(3) 0.013(2) -0.040(4) N3 0.089(4) 0.101(4) 0.053(3) -0.008(3) 0.019(3) -0.049(4) N4 0.073(3) 0.074(3) 0.051(2) 0.001(2) 0.016(2) -0.020(2) N5 0.042(2) 0.072(3) 0.073(3) 0.013(2) 0.006(2) 0.006(2) N6 0.041(3) 0.108(4) 0.075(3) 0.003(3) 0.007(2) -0.008(3) N7 0.055(3) 0.083(4) 0.088(4) -0.001(3) 0.007(3) -0.018(3) N8 0.050(3) 0.059(3) 0.064(3) 0.002(2) 0.005(2) -0.008(2) C1 0.064(3) 0.057(3) 0.056(3) 0.013(2) 0.016(2) 0.002(2) C2 0.121(7) 0.110(7) 0.148(8) 0.053(6) 0.048(6) 0.060(6) C3 0.087(4) 0.064(3) 0.060(3) 0.004(3) 0.035(3) 0.013(3) C4 0.161(8) 0.078(5) 0.106(6) 0.001(4) 0.065(6) 0.038(5) C5 0.087(4) 0.102(5) 0.044(3) 0.004(3) 0.007(3) -0.043(4) C6 0.114(6) 0.137(7) 0.047(3) -0.004(3) 0.008(3) -0.047(5) C7 0.061(3) 0.083(4) 0.050(3) -0.004(3) 0.022(2) -0.018(3) C8 0.093(5) 0.138(6) 0.059(4) -0.018(4) 0.044(3) -0.037(4) C9 0.057(4) 0.176(9) 0.044(3) 0.000(4) 0.005(3) -0.018(4) C10 0.077(6) 0.234(14) 0.142(9) 0.104(9) 0.006(5) 0.025(7) C11 0.126(7) 0.074(4) 0.090(5) -0.028(4) 0.064(5) -0.015(4) C12 0.178(11) 0.113(7) 0.147(8) 0.031(6) 0.092(8) 0.072(7) C13 0.054(3) 0.061(3) 0.037(2) -0.002(2) 0.014(2) -0.012(2) C14 0.062(4) 0.106(6) 0.091(5) -0.008(4) 0.011(3) 0.014(4) C15 0.063(4) 0.117(6) 0.105(5) 0.028(5) 0.013(4) 0.002(4) C16 0.101(7) 0.167(10) 0.130(8) 0.046(7) 0.027(6) 0.041(7) C17 0.140(10) 0.156(11) 0.188(12) 0.069(9) -0.001(9) 0.001(8) C18 0.051(3) 0.055(3) 0.035(2) 0.0035(19) 0.0111(19) -0.001(2) C19 0.080(4) 0.058(3) 0.094(5) -0.001(3) 0.020(4) 0.003(3) C20 0.159(10) 0.146(9) 0.148(9) 0.059(8) 0.035(7) 0.073(8) C21 0.41(3) 0.163(15) 0.192(16) 0.037(12) 0.027(18) 0.16(2) C22 0.22(2) 0.192(19) 0.32(3) 0.08(2) 0.11(2) 0.069(17) _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 Pt C18 2.033(5) . ? Pt C13 2.056(5) . ? Pt P2 2.3025(13) . ? Pt P1 2.3065(12) . ? P1 C3 1.815(6) . ? P1 C1 1.816(5) . ? P1 C5 1.818(6) . ? P2 C9 1.812(7) . ? P2 C7 1.820(5) . ? P2 C11 1.827(7) . ? N1 N2 1.345(8) . ? N1 C13 1.356(7) . ? N1 C14 1.463(9) . ? N2 N3 1.275(9) . ? N3 N4 1.379(8) . ? N4 C13 1.327(7) . ? N5 C18 1.338(7) . ? N5 N6 1.362(7) . ? N6 N7 1.280(8) . ? N7 N8 1.360(7) . ? N8 C18 1.334(7) . ? N8 C19 1.487(8) . ? C1 C2 1.528(9) . ? C3 C4 1.511(9) . ? C5 C6 1.546(8) . ? C7 C8 1.537(7) . ? C9 C10 1.508(14) . ? C11 C12 1.546(13) . ? C14 C15 1.494(9) . ? C15 C16 1.545(13) . ? C16 C17 1.463(13) . ? C19 C20 1.427(11) . ? C20 C21 1.597(18) . ? C21 C22 1.18(2) . ? 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 C18 Pt C13 178.82(16) . . ? C18 Pt P2 90.82(12) . . ? C13 Pt P2 88.02(13) . . ? C18 Pt P1 91.84(12) . . ? C13 Pt P1 89.25(12) . . ? P2 Pt P1 167.88(5) . . ? C3 P1 C1 102.3(3) . . ? C3 P1 C5 104.3(3) . . ? C1 P1 C5 106.9(3) . . ? C3 P1 Pt 117.7(2) . . ? C1 P1 Pt 108.84(18) . . ? C5 P1 Pt 115.53(19) . . ? C9 P2 C7 104.7(3) . . ? C9 P2 C11 104.3(4) . . ? C7 P2 C11 105.6(3) . . ? C9 P2 Pt 116.0(2) . . ? C7 P2 Pt 116.95(17) . . ? C11 P2 Pt 108.1(2) . . ? N2 N1 C13 109.7(6) . . ? N2 N1 C14 120.8(6) . . ? C13 N1 C14 129.4(5) . . ? N3 N2 N1 106.5(5) . . ? N2 N3 N4 111.0(5) . . ? C13 N4 N3 106.2(5) . . ? C18 N5 N6 107.4(5) . . ? N7 N6 N5 110.8(5) . . ? N6 N7 N8 105.6(5) . . ? C18 N8 N7 110.7(5) . . ? C18 N8 C19 129.6(5) . . ? N7 N8 C19 119.6(5) . . ? C2 C1 P1 113.2(5) . . ? C4 C3 P1 114.2(5) . . ? C6 C5 P1 115.3(4) . . ? C8 C7 P2 115.1(4) . . ? C10 C9 P2 113.1(6) . . ? C12 C11 P2 112.2(6) . . ? N4 C13 N1 106.6(5) . . ? N4 C13 Pt 126.8(4) . . ? N1 C13 Pt 126.5(4) . . ? N1 C14 C15 114.7(6) . . ? C14 C15 C16 111.1(8) . . ? C17 C16 C15 116.0(10) . . ? N8 C18 N5 105.6(4) . . ? N8 C18 Pt 126.5(4) . . ? N5 C18 Pt 127.9(4) . . ? C20 C19 N8 112.0(6) . . ? C19 C20 C21 110.2(11) . . ? C22 C21 C20 117(2) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.178 _refine_diff_density_min -1.078 _refine_diff_density_rms 0.094