data_4 _audit_creation_method 'SHELXL-2017/1' _shelx_SHELXL_version_number '2017/1' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H84 F18 N8 O8 P3 Pd Pt2' _chemical_formula_weight 1688.60 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' 'Pd' 'Pd' -0.9988 1.0072 '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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 2/c' _space_group_name_Hall '-C 2yc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 30.731(13) _cell_length_b 11.615(4) _cell_length_c 22.369(10) _cell_angle_alpha 90 _cell_angle_beta 128.996(5) _cell_angle_gamma 90 _cell_volume 6205(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7125 _cell_measurement_theta_min 1.7 _cell_measurement_theta_max 31.0 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.807 _exptl_crystal_F_000 3316 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.370 _exptl_crystal_size_mid 0.320 _exptl_crystal_size_min 0.250 _exptl_absorpt_coefficient_mu 4.963 _shelx_estimated_absorpt_T_min 0.261 _shelx_estimated_absorpt_T_max 0.370 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.503 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_source 'Rotating Anode' _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 14.6199 _diffrn_reflns_number 24270 _diffrn_reflns_av_unetI/netI 0.0748 _diffrn_reflns_av_R_equivalents 0.0649 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.102 _diffrn_reflns_theta_max 27.482 _diffrn_reflns_theta_full 25.241 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_point_group_measured_fraction_full 0.996 _reflns_number_total 7069 _reflns_number_gt 4658 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'CRYSTALCLEAR' _computing_cell_refinement 'CRYSTALCLEAR' _computing_data_reduction 'CRYSTALCLEAR' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _computing_molecular_graphics 'Yadokari-XG 2009 (Wakita, Nemoto et al., 2009)' _computing_publication_material 'Yadokari-XG 2009 (Wakita, Nemoto et al., 2009)' _publ_section_references ; Wakita, K. (2001). Yadokari-XG. Software for Crystal Structure Analyses. Release of Software (Yadokari-XG 2009) for Crystal Structure Analyses, Kabuto, C., Akine, S., Nemoto, T. & Kwon, E. (2009). J. Cryst. Soc. Jpn., 51, 218-224. ; _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+40.0000P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 7069 _refine_ls_number_parameters 354 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1027 _refine_ls_R_factor_gt 0.0699 _refine_ls_wR_factor_ref 0.1729 _refine_ls_wR_factor_gt 0.1533 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.40383(2) 0.00659(3) 0.35697(2) 0.04664(15) Uani 1 1 d . . . . . Pd1 Pd 0.500000 0.000000 0.500000 0.0390(2) Uani 1 2 d S . P . . P1 P 0.22844(17) 0.1540(3) 0.2593(2) 0.0783(10) Uani 1 1 d . . . . . O2 O 0.4573(3) -0.0762(7) 0.5288(4) 0.0576(18) Uani 1 1 d . . . . . N3 N 0.4011(4) 0.1632(7) 0.3924(4) 0.061(2) Uani 1 1 d . . . . . H3 H 0.373572 0.206377 0.358171 0.073 Uiso 1 1 calc R U . . . N1 N 0.4054(4) -0.1529(7) 0.3202(4) 0.061(2) Uani 1 1 d . . . . . H1 H 0.382622 -0.154125 0.269005 0.092 Uiso 1 1 calc R U . . . H1A H 0.394232 -0.205125 0.337063 0.092 Uiso 1 1 calc R U . . . H1B H 0.440149 -0.169160 0.338428 0.092 Uiso 1 1 calc R U . . . N2 N 0.4316(4) 0.0759(9) 0.3026(5) 0.072(3) Uani 1 1 d . . . . . H2 H 0.427041 0.151945 0.299621 0.107 Uiso 1 1 calc R U . . . H2A H 0.412057 0.046590 0.255478 0.107 Uiso 1 1 calc R U . . . H2B H 0.467671 0.059439 0.329067 0.107 Uiso 1 1 calc R U . . . N4 N 0.3756(4) -0.0618(8) 0.4084(5) 0.060(2) Uani 1 1 d . . . . . H4 H 0.339965 -0.071084 0.380234 0.072 Uiso 1 1 calc R U . . . C6 C 0.4048(5) -0.0938(8) 0.4794(6) 0.053(2) Uani 1 1 d . . . . . C7 C 0.3782(5) -0.1576(11) 0.5092(6) 0.071(3) Uani 1 1 d . . . . . C8 C 0.3146(6) -0.1554(14) 0.4544(8) 0.103(5) Uani 1 1 d . . . . . H8 H 0.301882 -0.077142 0.441171 0.154 Uiso 1 1 calc R U . . . H8A H 0.301033 -0.190097 0.478787 0.154 Uiso 1 1 calc R U . . . H8B H 0.300846 -0.197571 0.408651 0.154 Uiso 1 1 calc R U . . . P2 P 0.000000 0.3318(5) 0.250000 0.0791(14) Uani 1 2 d S T P . . F6 F 0.2126(5) 0.2850(8) 0.2437(8) 0.166(5) Uani 1 1 d . . . . . F4 F 0.2782(5) 0.1819(10) 0.2608(7) 0.158(4) Uani 1 1 d . . . . . C1 C 0.4359(4) 0.2072(8) 0.4608(5) 0.051(2) Uani 1 1 d . . . . . C10 C 0.3984(6) -0.2850(11) 0.5210(8) 0.096(5) Uani 1 1 d . . . . . H10 H 0.388598 -0.314192 0.473749 0.144 Uiso 1 1 calc R U . . . H10A H 0.380774 -0.330943 0.536021 0.144 Uiso 1 1 calc R U . . . H10B H 0.438315 -0.288088 0.560431 0.144 Uiso 1 1 calc R U . . . C2 C 0.4236(5) 0.3235(9) 0.4804(6) 0.067(3) Uani 1 1 d . . . . . C5 C 0.3906(6) 0.2933(13) 0.5092(8) 0.100(5) Uani 1 1 d . . . . . H5 H 0.409618 0.233098 0.546838 0.150 Uiso 1 1 calc R U . . . H5A H 0.353641 0.267935 0.466631 0.150 Uiso 1 1 calc R U . . . H5B H 0.387967 0.360305 0.531913 0.150 Uiso 1 1 calc R U . . . C4 C 0.4783(6) 0.3796(11) 0.5452(8) 0.107(5) Uani 1 1 d . . . . . H4A H 0.497885 0.330821 0.589777 0.160 Uiso 1 1 calc R U . . . H4B H 0.470876 0.452586 0.557349 0.160 Uiso 1 1 calc R U . . . H4C H 0.500898 0.391134 0.529769 0.160 Uiso 1 1 calc R U . . . C9 C 0.4005(7) -0.1045(17) 0.5863(9) 0.137(8) Uani 1 1 d . . . . . H9 H 0.440679 -0.108582 0.621264 0.205 Uiso 1 1 calc R U . . . H9A H 0.385944 -0.146089 0.607366 0.205 Uiso 1 1 calc R U . . . H9B H 0.389015 -0.025437 0.578779 0.205 Uiso 1 1 calc R U . . . F7 F -0.0046(5) 0.3507(12) 0.1782(6) 0.178(5) Uani 1 1 d . . . . . F5 F 0.2420(6) 0.0253(8) 0.2707(8) 0.184(6) Uani 1 1 d . . . . . C3 C 0.3892(7) 0.4012(11) 0.4106(7) 0.107(5) Uani 1 1 d . . . . . H3A H 0.382748 0.473255 0.424919 0.160 Uiso 1 1 calc R U . . . H3B H 0.353931 0.365052 0.371578 0.160 Uiso 1 1 calc R U . . . H3C H 0.409020 0.414590 0.391092 0.160 Uiso 1 1 calc R U . . . F2 F 0.1789(6) 0.1346(12) 0.2574(11) 0.235(8) Uani 1 1 d . . . . . F1 F 0.1927(6) 0.1386(11) 0.1737(6) 0.227(7) Uani 1 1 d . . . . . F3 F 0.2663(7) 0.1725(13) 0.3444(6) 0.225(7) Uani 1 1 d . . . . . F10 F 0.000000 0.4632(19) 0.250000 0.282(17) Uani 1 2 d S T P . . O4 O 0.1660(4) 0.4502(11) 0.3400(5) 0.104(3) Uani 1 1 d . . . . . O3 O 0.4016(7) 0.3117(12) 0.2511(9) 0.147(5) Uani 1 1 d . . . . . C18 C 0.2097(8) 0.5123(18) 0.3522(11) 0.143(8) Uani 1 1 d . . . . . H18 H 0.199455 0.592955 0.340886 0.171 Uiso 1 1 calc R U . . . H18A H 0.216499 0.484463 0.317852 0.171 Uiso 1 1 calc R U . . . C15 C 0.1908(8) 0.3700(15) 0.4008(9) 0.118(6) Uani 1 1 d . . . . . H15 H 0.188221 0.293281 0.381670 0.141 Uiso 1 1 calc R U . . . H15A H 0.171101 0.370403 0.421627 0.141 Uiso 1 1 calc R U . . . C17 C 0.2585(10) 0.5003(17) 0.4287(13) 0.171(11) Uani 1 1 d . . . . . H17 H 0.265156 0.569277 0.457897 0.205 Uiso 1 1 calc R U . . . H17A H 0.290614 0.486865 0.430958 0.205 Uiso 1 1 calc R U . . . C16 C 0.2487(7) 0.3997(18) 0.4602(9) 0.141(8) Uani 1 1 d . . . . . H16 H 0.273036 0.336107 0.470451 0.169 Uiso 1 1 calc R U . . . H16A H 0.255448 0.420084 0.507446 0.169 Uiso 1 1 calc R U . . . C12 C 0.4090(18) 0.479(3) 0.214(3) 0.30(3) Uani 1 1 d . . . . . H12 H 0.410876 0.545093 0.242432 0.363 Uiso 1 1 calc R U . . . H12A H 0.425807 0.500951 0.190958 0.363 Uiso 1 1 calc R U . . . C13 C 0.3560(16) 0.451(3) 0.1597(14) 0.23(2) Uani 1 1 d . . . . . H13 H 0.349538 0.426801 0.113133 0.270 Uiso 1 1 calc R U . . . H13A H 0.331139 0.514289 0.147738 0.270 Uiso 1 1 calc R U . . . C14 C 0.3489(9) 0.3551(19) 0.1953(15) 0.167(9) Uani 1 1 d . . . . . H14 H 0.332264 0.381804 0.217972 0.201 Uiso 1 1 calc R U . . . H14A H 0.324846 0.296461 0.157351 0.201 Uiso 1 1 calc R U . . . C11 C 0.4385(10) 0.389(3) 0.2643(14) 0.200(12) Uani 1 1 d . . . . . H11 H 0.463098 0.355035 0.255812 0.240 Uiso 1 1 calc R U . . . H11A H 0.461124 0.415620 0.317032 0.240 Uiso 1 1 calc R U . . . F8 F 0.0626(5) 0.3304(18) 0.2988(7) 0.226(8) Uani 1 1 d . . . . . O1 O 0.4799(3) 0.1542(6) 0.5160(4) 0.0582(18) Uani 1 1 d . . . . . F9 F 0.000000 0.2132(17) 0.250000 0.360(19) Uani 1 2 d S T P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0374(2) 0.0478(2) 0.0445(2) -0.00002(15) 0.02090(18) 0.00135(17) Pd1 0.0323(5) 0.0345(5) 0.0434(5) 0.0012(3) 0.0206(4) 0.0011(4) P1 0.067(2) 0.065(2) 0.085(2) 0.0018(16) 0.039(2) 0.0110(18) O2 0.038(4) 0.071(5) 0.056(4) 0.013(3) 0.026(4) 0.000(4) N3 0.063(6) 0.056(6) 0.051(5) 0.008(4) 0.029(5) 0.017(5) N1 0.066(6) 0.057(6) 0.056(5) -0.008(4) 0.036(5) -0.007(5) N2 0.074(7) 0.078(7) 0.069(6) 0.014(5) 0.047(6) 0.008(6) N4 0.036(5) 0.070(6) 0.053(5) -0.003(4) 0.018(4) -0.006(4) C6 0.058(7) 0.039(5) 0.066(6) -0.002(4) 0.041(6) 0.000(5) C7 0.071(9) 0.089(9) 0.073(7) -0.009(6) 0.056(7) -0.018(7) C8 0.082(11) 0.119(13) 0.142(13) -0.011(10) 0.087(11) -0.028(9) P2 0.067(3) 0.102(4) 0.086(3) 0.000 0.057(3) 0.000 F6 0.130(9) 0.074(7) 0.264(13) 0.023(7) 0.111(10) 0.022(6) F4 0.101(8) 0.168(11) 0.205(11) -0.002(8) 0.097(9) 0.019(8) C1 0.052(7) 0.040(5) 0.054(5) 0.002(4) 0.030(5) 0.000(4) C10 0.105(12) 0.065(9) 0.114(11) 0.020(7) 0.067(10) -0.012(8) C2 0.072(9) 0.040(6) 0.080(7) -0.004(5) 0.044(7) 0.015(6) C5 0.084(11) 0.108(12) 0.093(10) -0.007(8) 0.049(9) 0.031(9) C4 0.115(14) 0.048(8) 0.106(10) -0.005(7) 0.045(10) 0.022(8) C9 0.145(17) 0.20(2) 0.129(12) -0.085(13) 0.115(13) -0.097(14) F7 0.181(12) 0.260(16) 0.127(8) -0.035(9) 0.113(9) -0.035(11) F5 0.225(15) 0.068(7) 0.244(14) 0.026(7) 0.140(13) 0.046(8) C3 0.135(14) 0.050(8) 0.088(9) 0.020(6) 0.047(9) 0.043(8) F2 0.183(14) 0.198(14) 0.43(2) 0.131(14) 0.242(16) 0.065(11) F1 0.246(16) 0.177(13) 0.099(7) -0.011(7) 0.033(9) -0.076(11) F3 0.245(17) 0.281(19) 0.110(8) -0.034(9) 0.093(10) 0.016(13) F10 0.48(5) 0.138(19) 0.23(3) 0.000 0.23(3) 0.000 O4 0.076(7) 0.142(10) 0.078(6) 0.028(6) 0.041(6) -0.004(7) O3 0.124(12) 0.099(10) 0.211(14) 0.059(9) 0.102(12) 0.028(9) C18 0.087(14) 0.20(2) 0.107(14) 0.037(12) 0.043(12) -0.008(14) C15 0.138(17) 0.107(14) 0.105(12) 0.016(10) 0.075(12) -0.011(12) C17 0.13(2) 0.141(19) 0.147(18) 0.037(13) 0.044(16) -0.064(14) C16 0.086(14) 0.143(19) 0.106(12) 0.024(12) 0.018(11) -0.006(12) C12 0.25(5) 0.15(3) 0.42(7) 0.10(4) 0.17(5) -0.03(3) C13 0.40(5) 0.18(3) 0.16(2) 0.11(2) 0.20(3) 0.17(3) C14 0.110(18) 0.13(2) 0.20(2) -0.003(17) 0.065(17) 0.026(15) C11 0.11(2) 0.21(3) 0.17(2) 0.05(2) 0.030(16) -0.02(2) F8 0.073(8) 0.43(3) 0.167(10) -0.014(13) 0.071(8) 0.003(11) O1 0.058(5) 0.044(4) 0.056(4) -0.002(3) 0.028(4) 0.008(3) F9 0.32(4) 0.062(13) 0.55(5) 0.000 0.20(4) 0.000 _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 N4 1.991(9) . ? Pt1 N3 2.007(8) . ? Pt1 N2 2.038(8) . ? Pt1 N1 2.041(8) . ? Pt1 Pd1 2.6601(9) . ? Pd1 O2 1.996(7) . ? Pd1 O2 1.996(7) 5_656 ? Pd1 O1 1.999(6) 5_656 ? Pd1 O1 1.999(6) . ? P1 F3 1.494(11) . ? P1 F1 1.503(10) . ? P1 F2 1.513(11) . ? P1 F5 1.529(10) . ? P1 F4 1.544(11) . ? P1 F6 1.568(10) . ? O2 C6 1.274(12) . ? N3 C1 1.299(12) . ? N4 C6 1.293(12) . ? C6 C7 1.533(14) . ? C7 C8 1.518(17) . ? C7 C9 1.528(15) . ? C7 C10 1.562(17) . ? P2 F9 1.38(2) . ? P2 F8 1.499(11) 2 ? P2 F8 1.499(11) . ? P2 F10 1.53(2) . ? P2 F7 1.537(9) 2 ? P2 F7 1.537(9) . ? C1 O1 1.277(11) . ? C1 C2 1.538(13) . ? C2 C3 1.514(14) . ? C2 C4 1.512(17) . ? C2 C5 1.546(17) . ? O4 C18 1.39(2) . ? O4 C15 1.411(16) . ? O3 C11 1.32(3) . ? O3 C14 1.38(2) . ? C18 C17 1.40(3) . ? C15 C16 1.44(2) . ? C17 C16 1.49(2) . ? C12 C13 1.32(5) . ? C12 C11 1.38(4) . ? C13 C14 1.46(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Pt1 N3 89.5(3) . . ? N4 Pt1 N2 179.1(4) . . ? N3 Pt1 N2 90.8(4) . . ? N4 Pt1 N1 90.0(3) . . ? N3 Pt1 N1 179.2(4) . . ? N2 Pt1 N1 89.6(4) . . ? N4 Pt1 Pd1 81.5(2) . . ? N3 Pt1 Pd1 80.9(2) . . ? N2 Pt1 Pd1 99.4(3) . . ? N1 Pt1 Pd1 99.7(2) . . ? O2 Pd1 O2 180.0(4) . 5_656 ? O2 Pd1 O1 90.0(3) . 5_656 ? O2 Pd1 O1 90.0(3) 5_656 5_656 ? O2 Pd1 O1 90.0(3) . . ? O2 Pd1 O1 90.0(3) 5_656 . ? O1 Pd1 O1 180.0 5_656 . ? O2 Pd1 Pt1 86.72(19) . . ? O2 Pd1 Pt1 93.29(19) 5_656 . ? O1 Pd1 Pt1 92.57(19) 5_656 . ? O1 Pd1 Pt1 87.43(19) . . ? O2 Pd1 Pt1 93.28(19) . 5_656 ? O2 Pd1 Pt1 86.72(19) 5_656 5_656 ? O1 Pd1 Pt1 87.44(19) 5_656 5_656 ? O1 Pd1 Pt1 92.57(19) . 5_656 ? Pt1 Pd1 Pt1 180.0 . 5_656 ? F3 P1 F1 176.8(10) . . ? F3 P1 F2 91.3(9) . . ? F1 P1 F2 91.7(10) . . ? F3 P1 F5 90.9(8) . . ? F1 P1 F5 90.0(8) . . ? F2 P1 F5 91.4(8) . . ? F3 P1 F4 88.6(8) . . ? F1 P1 F4 88.4(8) . . ? F2 P1 F4 176.4(7) . . ? F5 P1 F4 92.2(7) . . ? F3 P1 F6 91.7(8) . . ? F1 P1 F6 87.4(7) . . ? F2 P1 F6 88.4(7) . . ? F5 P1 F6 177.4(8) . . ? F4 P1 F6 88.0(6) . . ? C6 O2 Pd1 121.4(6) . . ? C1 N3 Pt1 127.9(7) . . ? C6 N4 Pt1 127.3(8) . . ? O2 C6 N4 122.8(10) . . ? O2 C6 C7 115.5(9) . . ? N4 C6 C7 121.7(10) . . ? C8 C7 C9 109.9(11) . . ? C8 C7 C6 114.1(10) . . ? C9 C7 C6 108.2(10) . . ? C8 C7 C10 109.0(11) . . ? C9 C7 C10 110.1(12) . . ? C6 C7 C10 105.4(9) . . ? F9 P2 F8 89.4(8) . 2 ? F9 P2 F8 89.4(8) . . ? F8 P2 F8 178.8(17) 2 . ? F9 P2 F10 180.0 . . ? F8 P2 F10 90.6(8) 2 . ? F8 P2 F10 90.6(8) . . ? F9 P2 F7 98.2(6) . 2 ? F8 P2 F7 89.8(6) 2 2 ? F8 P2 F7 90.4(6) . 2 ? F10 P2 F7 81.8(6) . 2 ? F9 P2 F7 98.2(6) . . ? F8 P2 F7 90.4(6) 2 . ? F8 P2 F7 89.8(6) . . ? F10 P2 F7 81.8(6) . . ? F7 P2 F7 163.5(11) 2 . ? O1 C1 N3 122.4(9) . . ? O1 C1 C2 116.7(9) . . ? N3 C1 C2 120.9(9) . . ? C3 C2 C4 111.4(11) . . ? C3 C2 C1 111.6(9) . . ? C4 C2 C1 109.1(10) . . ? C3 C2 C5 110.4(11) . . ? C4 C2 C5 108.8(11) . . ? C1 C2 C5 105.2(10) . . ? C18 O4 C15 106.4(13) . . ? C11 O3 C14 108.0(18) . . ? O4 C18 C17 110.3(15) . . ? O4 C15 C16 109.6(14) . . ? C18 C17 C16 106.0(16) . . ? C15 C16 C17 104.5(14) . . ? C13 C12 C11 111(3) . . ? C12 C13 C14 102(2) . . ? O3 C14 C13 106(2) . . ? O3 C11 C12 107(2) . . ? C1 O1 Pd1 121.1(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Pd1 O2 C6 N4 -1.6(14) . . . . ? Pd1 O2 C6 C7 177.6(7) . . . . ? Pt1 N4 C6 O2 6.0(15) . . . . ? Pt1 N4 C6 C7 -173.1(8) . . . . ? O2 C6 C7 C8 167.9(10) . . . . ? N4 C6 C7 C8 -12.9(16) . . . . ? O2 C6 C7 C9 45.3(15) . . . . ? N4 C6 C7 C9 -135.6(13) . . . . ? O2 C6 C7 C10 -72.5(12) . . . . ? N4 C6 C7 C10 106.6(12) . . . . ? Pt1 N3 C1 O1 3.2(16) . . . . ? Pt1 N3 C1 C2 -172.6(8) . . . . ? O1 C1 C2 C3 154.0(11) . . . . ? N3 C1 C2 C3 -29.9(16) . . . . ? O1 C1 C2 C4 30.4(14) . . . . ? N3 C1 C2 C4 -153.5(11) . . . . ? O1 C1 C2 C5 -86.3(12) . . . . ? N3 C1 C2 C5 89.8(12) . . . . ? C15 O4 C18 C17 -18(2) . . . . ? C18 O4 C15 C16 13(2) . . . . ? O4 C18 C17 C16 16(3) . . . . ? O4 C15 C16 C17 -4(2) . . . . ? C18 C17 C16 C15 -7(3) . . . . ? C11 C12 C13 C14 22(5) . . . . ? C11 O3 C14 C13 16(3) . . . . ? C12 C13 C14 O3 -23(4) . . . . ? C14 O3 C11 C12 -3(4) . . . . ? C13 C12 C11 O3 -13(5) . . . . ? N3 C1 O1 Pd1 2.1(14) . . . . ? C2 C1 O1 Pd1 178.1(7) . . . . ? _refine_diff_density_max 2.300 _refine_diff_density_min -2.454 _refine_diff_density_rms 0.174 _shelx_res_file ; TITL I161102 I161102.res created by SHELXL-2017/1 at 12:39:04 on 13-Sep-2018 REM Yadorkari-X generated CELL 0.71070 30.7310 11.6150 22.3693 90.0000 128.9963 90.0000 ZERR 4.0 0.0133 0.0043 0.0097 0.0000 0.0049 0.0000 LATT 7 SYMM -X, +Y, 1/2-Z REM SPGR C2/c monoclinic SFAC C H N O Pd Pt P F UNIT 144 336 32 32 4 8 12 72 SIZE 0.37 0.32 0.25 TEMP 20.1 L.S. 20 FMAP 2 PLAN -1 ACTA CONF LIST 4 MERG 2 OMIT -10.000000 55.000000 WGHT 0.050000 40.000000 FVAR 0.61177 PT1 6 0.403834 0.006593 0.356970 11.00000 0.03744 0.04778 = 0.04451 -0.00002 0.02090 0.00135 PD1 5 0.500000 0.000000 0.500000 10.50000 0.03231 0.03454 = 0.04340 0.00122 0.02062 0.00113 P1 7 0.228441 0.154007 0.259336 11.00000 0.06703 0.06451 = 0.08474 0.00181 0.03881 0.01099 O2 4 0.457303 -0.076173 0.528826 11.00000 0.03825 0.07101 = 0.05562 0.01328 0.02569 -0.00017 N3 3 0.401125 0.163161 0.392435 11.00000 0.06293 0.05600 = 0.05080 0.00848 0.02913 0.01678 AFIX 43 H3 2 0.373572 0.206377 0.358171 11.00000 -1.20000 AFIX 0 N1 3 0.405435 -0.152944 0.320180 11.00000 0.06644 0.05712 = 0.05630 -0.00833 0.03647 -0.00666 AFIX 137 H1 2 0.382622 -0.154125 0.269005 11.00000 -1.50000 H1A 2 0.394232 -0.205125 0.337063 11.00000 -1.50000 H1B 2 0.440149 -0.169160 0.338428 11.00000 -1.50000 AFIX 0 N2 3 0.431555 0.075903 0.302631 11.00000 0.07352 0.07777 = 0.06896 0.01425 0.04747 0.00780 AFIX 137 H2 2 0.427041 0.151945 0.299621 11.00000 -1.50000 H2A 2 0.412057 0.046590 0.255478 11.00000 -1.50000 H2B 2 0.467671 0.059439 0.329067 11.00000 -1.50000 AFIX 0 N4 3 0.375603 -0.061789 0.408406 11.00000 0.03554 0.07049 = 0.05319 -0.00334 0.01842 -0.00550 AFIX 43 H4 2 0.339965 -0.071084 0.380234 11.00000 -1.20000 AFIX 0 C6 1 0.404807 -0.093790 0.479381 11.00000 0.05811 0.03901 = 0.06603 -0.00247 0.04114 -0.00030 C7 1 0.378188 -0.157582 0.509221 11.00000 0.07090 0.08948 = 0.07329 -0.00896 0.05598 -0.01796 C8 1 0.314650 -0.155397 0.454423 11.00000 0.08195 0.11864 = 0.14167 -0.01119 0.08651 -0.02773 AFIX 137 H8 2 0.301882 -0.077142 0.441171 11.00000 -1.50000 H8A 2 0.301033 -0.190097 0.478787 11.00000 -1.50000 H8B 2 0.300846 -0.197571 0.408651 11.00000 -1.50000 AFIX 0 P2 7 0.000000 0.331758 0.250000 10.50000 0.06739 0.10215 = 0.08633 0.00000 0.05721 0.00000 F6 8 0.212613 0.284953 0.243662 11.00000 0.13034 0.07446 = 0.26378 0.02347 0.11053 0.02214 F4 8 0.278201 0.181879 0.260766 11.00000 0.10129 0.16769 = 0.20535 -0.00229 0.09718 0.01933 C1 1 0.435916 0.207178 0.460833 11.00000 0.05163 0.03965 = 0.05425 0.00167 0.02996 0.00014 C10 1 0.398418 -0.284973 0.520989 11.00000 0.10543 0.06510 = 0.11379 0.01964 0.06749 -0.01160 AFIX 137 H10 2 0.388598 -0.314192 0.473749 11.00000 -1.50000 H10A 2 0.380774 -0.330943 0.536021 11.00000 -1.50000 H10B 2 0.438315 -0.288088 0.560431 11.00000 -1.50000 AFIX 0 C2 1 0.423609 0.323460 0.480359 11.00000 0.07236 0.04036 = 0.07988 -0.00450 0.04449 0.01549 C5 1 0.390577 0.293345 0.509166 11.00000 0.08432 0.10814 = 0.09334 -0.00679 0.04942 0.03147 AFIX 137 H5 2 0.409618 0.233098 0.546838 11.00000 -1.50000 H5A 2 0.353641 0.267935 0.466631 11.00000 -1.50000 H5B 2 0.387967 0.360305 0.531913 11.00000 -1.50000 AFIX 0 C4 1 0.478312 0.379629 0.545238 11.00000 0.11509 0.04751 = 0.10609 -0.00481 0.04457 0.02212 AFIX 137 H4A 2 0.497885 0.330821 0.589777 11.00000 -1.50000 H4B 2 0.470876 0.452586 0.557349 11.00000 -1.50000 H4C 2 0.500898 0.391134 0.529769 11.00000 -1.50000 AFIX 0 C9 1 0.400534 -0.104486 0.586327 11.00000 0.14506 0.19628 = 0.12932 -0.08504 0.11523 -0.09745 AFIX 137 H9 2 0.440679 -0.108582 0.621264 11.00000 -1.50000 H9A 2 0.385944 -0.146089 0.607366 11.00000 -1.50000 H9B 2 0.389015 -0.025437 0.578779 11.00000 -1.50000 AFIX 0 F7 8 -0.004634 0.350690 0.178190 11.00000 0.18080 0.25958 = 0.12697 -0.03513 0.11317 -0.03505 F5 8 0.242013 0.025325 0.270690 11.00000 0.22480 0.06790 = 0.24429 0.02625 0.14008 0.04595 C3 1 0.389178 0.401199 0.410608 11.00000 0.13493 0.04953 = 0.08771 0.01997 0.04725 0.04279 AFIX 137 H3A 2 0.382748 0.473255 0.424919 11.00000 -1.50000 H3B 2 0.353931 0.365052 0.371578 11.00000 -1.50000 H3C 2 0.409020 0.414590 0.391092 11.00000 -1.50000 AFIX 0 F2 8 0.178853 0.134614 0.257362 11.00000 0.18334 0.19769 = 0.42695 0.13117 0.24161 0.06463 F1 8 0.192698 0.138629 0.173695 11.00000 0.24633 0.17750 = 0.09866 -0.01087 0.03263 -0.07574 F3 8 0.266327 0.172481 0.344351 11.00000 0.24479 0.28137 = 0.11006 -0.03356 0.09267 0.01608 F10 8 0.000000 0.463202 0.250000 10.50000 0.48092 0.13754 = 0.23395 0.00000 0.22740 0.00000 O4 4 0.165981 0.450211 0.339999 11.00000 0.07639 0.14208 = 0.07755 0.02806 0.04082 -0.00406 O3 4 0.401623 0.311665 0.251088 11.00000 0.12369 0.09942 = 0.21075 0.05851 0.10224 0.02789 C18 1 0.209662 0.512262 0.352174 11.00000 0.08676 0.19594 = 0.10718 0.03749 0.04250 -0.00775 AFIX 23 H18 2 0.199455 0.592955 0.340886 11.00000 -1.20000 H18A 2 0.216499 0.484463 0.317852 11.00000 -1.20000 AFIX 0 C15 1 0.190814 0.370050 0.400757 11.00000 0.13751 0.10681 = 0.10549 0.01625 0.07479 -0.01145 AFIX 23 H15 2 0.188221 0.293281 0.381670 11.00000 -1.20000 H15A 2 0.171101 0.370403 0.421627 11.00000 -1.20000 AFIX 0 C17 1 0.258465 0.500310 0.428726 11.00000 0.13237 0.14105 = 0.14681 0.03704 0.04402 -0.06353 AFIX 23 H17 2 0.265156 0.569277 0.457897 11.00000 -1.20000 H17A 2 0.290614 0.486865 0.430958 11.00000 -1.20000 AFIX 0 C16 1 0.248738 0.399737 0.460203 11.00000 0.08634 0.14258 = 0.10626 0.02426 0.01814 -0.00557 AFIX 23 H16 2 0.273036 0.336107 0.470451 11.00000 -1.20000 H16A 2 0.255448 0.420084 0.507446 11.00000 -1.20000 AFIX 0 C12 1 0.408954 0.479223 0.214194 11.00000 0.25140 0.14702 = 0.42276 0.09722 0.17029 -0.02870 AFIX 23 H12 2 0.410876 0.545093 0.242432 11.00000 -1.20000 H12A 2 0.425807 0.500951 0.190958 11.00000 -1.20000 AFIX 0 C13 1 0.356022 0.450917 0.159673 11.00000 0.39650 0.17667 = 0.15629 0.10519 0.19950 0.16886 AFIX 23 H13 2 0.349538 0.426801 0.113133 11.00000 -1.20000 H13A 2 0.331139 0.514289 0.147738 11.00000 -1.20000 AFIX 0 C14 1 0.348891 0.355096 0.195294 11.00000 0.11018 0.12810 = 0.19765 -0.00276 0.06538 0.02579 AFIX 23 H14 2 0.332264 0.381804 0.217972 11.00000 -1.20000 H14A 2 0.324846 0.296461 0.157351 11.00000 -1.20000 AFIX 0 C11 1 0.438500 0.388826 0.264258 11.00000 0.10552 0.21097 = 0.16748 0.04934 0.02962 -0.01511 AFIX 23 H11 2 0.463098 0.355035 0.255812 11.00000 -1.20000 H11A 2 0.461124 0.415620 0.317032 11.00000 -1.20000 AFIX 0 F8 8 0.062574 0.330405 0.298845 11.00000 0.07315 0.42863 = 0.16692 -0.01365 0.07083 0.00307 O1 4 0.479919 0.154211 0.516024 11.00000 0.05819 0.04409 = 0.05576 -0.00172 0.02786 0.00822 F9 8 0.000000 0.213234 0.250000 10.50000 0.31882 0.06213 = 0.55161 0.00000 0.20344 0.00000 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM I161102 REM R1 = 0.0699 for 4658 Fo > 4sig(Fo) and 0.1027 for all 7069 data REM 354 parameters refined using 0 restraints END WGHT 0.0601 25.1354 REM Highest difference peak 2.300, deepest hole -2.454, 1-sigma level 0.174 Q1 1 0.4428 0.0063 0.3811 11.00000 0.05 2.30 ; _shelx_res_checksum 71517 _shelx_hkl_file ; 0 0 -3 113.98 67.93 0 0 3 -30.53 49.61 0 0 3 -35.01 61.29 0 0 -3 -66.27 86.59 0 0 3 7.51 36.87 0 0 3 34.45 14.96 0 0 -3 135.01 56.42 0 0 -411531.11 638.68 0 0 411003.45 600.94 0 0 411746.74 673.20 0 0 -4 9311.60 545.96 0 0 410275.78 707.08 0 0 4 9519.95 547.46 0 0 -410362.29 610.19 0 0 -5 24.01 58.50 0 0 5 -59.63 63.68 0 0 5 26.10 53.36 0 0 -5 18.56 42.25 0 0 5 39.85 52.47 0 0 5 -13.06 72.42 0 0 -5 -66.04 121.97 0 0 -668762.86 1846.01 0 0 663546.83 1672.78 0 0 665163.99 1802.94 0 0 -661192.98 1700.12 0 0 667910.95 1855.17 0 0 664307.87 1782.72 0 0 -664380.06 1807.17 0 0 -7 -28.49 91.32 0 0 7 299.03 106.63 0 0 -7 180.56 119.88 0 0 7 38.71 100.98 0 0 7 120.24 90.84 0 0 -7 301.78 108.95 0 0 -875388.77 2434.15 0 0 869290.76 2218.75 0 0 862239.18 2089.84 0 0 -871220.74 2378.08 0 0 -870615.28 2378.64 0 0 -9 108.54 84.54 0 0 9 21.43 43.21 0 0 -9 -118.70 164.81 0 0 -9 35.94 68.53 0 0 -1024440.01 1180.50 0 0 1024480.41 1156.40 0 0 -1024585.95 1475.48 0 0 -1022874.12 1197.22 0 0 -1025856.65 1316.92 0 0 -11 97.55 130.85 0 0 11 -136.49 84.15 0 0 -11 172.95 150.80 0 0 -11 136.83 133.87 0 0 -12 3905.29 662.61 0 0 12 3940.10 646.08 0 0 -12 4320.51 1185.69 0 0 -12 4148.45 958.44 0 0 -12 3942.79 1015.64 0 0 -13 10.65 61.99 0 0 13 -47.84 84.96 0 0 -13 -92.38 173.28 0 0 -13 -9.36 222.20 0 0 -1415849.74 1222.94 0 0 14 9574.81 427.71 0 0 -1416871.02 1775.96 0 0 15 620.80 271.90 0 0 -15 209.36 174.07 0 0 16 196.90 96.13 0 0 -16 -32.31 171.27 0 0 -16 359.21 175.22 0 0 17 42.31 60.12 0 0 -17 72.81 135.00 0 0 -17 268.09 182.67 0 0 -18 4899.61 1199.43 0 0 -18 4011.40 643.18 0 0 -19 -50.76 227.21 0 0 -19 252.01 155.10 0 0 -20 4721.97 1358.31 0 0 -20 3210.98 718.10 0 0 -21 238.83 210.07 0 0 -21 212.94 147.11 0 0 -22 1226.88 408.16 0 0 -22 812.59 444.42 0 2 0165978.7 4115.48 0 -2 0157120.6 3891.90 0 2 -1 272.22 70.81 0 -2 1 152.92 75.47 0 -2 -1 -29.77 75.08 0 2 -2 2607.78 432.20 0 -2 2 2039.35 601.66 0 2 2 2071.08 209.35 0 -2 -2 2217.37 377.46 0 -2 -2 2124.61 409.51 0 2 2 2082.51 251.55 0 -2 -2 2385.42 492.59 0 2 -3 1074.52 294.33 0 -2 3 1382.19 300.60 0 2 3 1284.48 325.79 0 -2 -3 1354.60 299.28 0 2 3 1145.28 231.84 0 -2 -3 1174.89 267.20 0 2 3 1226.81 289.15 0 -2 -3 1305.36 323.13 0 2 4101673.3 2565.34 0 2 -4106827.7 2760.26 0 -2 497340.24 2509.53 0 2 4101689.1 2567.28 0 2 4105914.2 2702.43 0 -2 -4115568.0 2936.49 0 2 4109505.7 2785.36 0 -2 -4105490.6 2699.50 0 2 5 332.65 74.76 0 2 -5 503.85 181.33 0 -2 5 330.98 273.79 0 2 5 256.55 59.83 0 2 -5 456.18 245.38 0 2 5 382.77 80.32 0 -2 -5 374.49 151.56 0 -2 5 549.38 160.96 0 -2 -5 407.17 142.07 0 2 659142.56 1889.36 0 2 -662406.03 2017.41 0 -2 660588.99 1960.78 0 2 658855.38 2079.11 0 2 667105.44 2166.47 0 -2 -663068.58 2049.98 0 -2 658891.43 1916.12 0 -2 -665820.72 2205.13 0 -2 -7 956.13 181.16 0 2 7 781.63 196.10 0 2 -7 1145.00 345.79 0 -2 7 1086.08 245.35 0 2 -7 1192.70 343.76 0 2 7 882.86 237.30 0 -2 -7 998.82 336.90 0 -2 7 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