# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Pan, Baofei' 'Bezpalko, Mark' 'Foxman, Bruce' 'Thomas, Christine' _publ_contact_author_name 'Thomas, Christine' _publ_contact_author_email thomasc@brandeis.edu _publ_section_title ; Heterolytic Activation of E-H Bonds Across Pt-P Bonds in Pt NHP (N-heterocyclic Phosphenium/Phosphido) Complexes ; # Attachment '- combined_bf.cif' data_4 _database_code_depnum_ccdc_archive 'CCDC 869435' #TrackingRef '- combined_bf.cif' _audit_creation_date 11-10-05 _audit_creation_method CRYSTALS_ver_14.30 _oxford_structure_analysis_title 'bfpan_614_0ma in P2(1)/c' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 14.8742(10) _cell_length_b 35.625(3) _cell_length_c 11.9635(9) _cell_angle_alpha 90 _cell_angle_beta 107.599(4) _cell_angle_gamma 90 _cell_volume 6042.7(8) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall '-P 2ybc ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Pt -1.7033 8.3905 27.0059 1.5129 17.7639 8.8117 15.7131 0.4246 5.7837 38.6103 11.6883 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C64 H57 Cl4 F6 N2 O1 P5 Pt1 # Dc = 1.62 Fooo = 2952.00 Mu = 26.95 M = 1475.93 # Found Formula = C64 H57 Cl4 F6 N2 O1 P5 Pt1 # Dc = 1.62 FOOO = 2952.00 Mu = 26.95 M = 1475.93 _chemical_formula_sum 'C64 H57 Cl4 F6 N2 O1 P5 Pt1' _chemical_formula_moiety 'C62 H53 N2 O P4 Pt, F6 P,2(C H2 Cl2)' _chemical_compound_source ? _chemical_formula_weight 1475.93 _cell_measurement_reflns_used 9788 _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 _cell_measurement_temperature 120 _exptl_crystal_description 'plate fragment' _exptl_crystal_colour 'light yellow' _exptl_crystal_size_min 0.064 _exptl_crystal_size_mid 0.140 _exptl_crystal_size_max 0.750 _exptl_crystal_density_diffrn 1.622 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2952 _exptl_absorpt_coefficient_mu 2.695 # Sheldrick geometric approximatio 0.69 0.84 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Analytical Absorption (De Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_min 0.69 _exptl_absorpt_correction_T_max 0.84 _diffrn_measurement_device_type 'Bruker Kappa Apex2' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 120 _diffrn_reflns_number 86823 _reflns_number_total 17579 _diffrn_reflns_av_R_equivalents 0.048 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 17579 # Theoretical number of reflections is about 35504 _diffrn_reflns_theta_min 1.436 _diffrn_reflns_theta_max 30.079 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 29.477 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -50 _diffrn_reflns_limit_k_max 50 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _reflns_limit_h_min -20 _reflns_limit_h_max 19 _reflns_limit_k_min 0 _reflns_limit_k_max 50 _reflns_limit_l_min 0 _reflns_limit_l_max 16 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -2.76 _refine_diff_density_max 1.59 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 17579 _refine_ls_number_restraints 6 _refine_ls_number_parameters 743 _oxford_refine_ls_R_factor_ref 0.0550 _refine_ls_wR_factor_ref 0.1067 _refine_ls_goodness_of_fit_ref 0.9711 _refine_ls_shift/su_max 0.0041448 _refine_ls_shift/su_mean 0.0000778 # The values computed with all filters except I/sigma _oxford_reflns_number_all 17579 _refine_ls_R_factor_all 0.0550 _refine_ls_wR_factor_all 0.1067 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 14355 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_gt 0.1021 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.05P)^2^ +28.72P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Bruker Analytical X-ray Systems, Inc., 2006. Apex2, Version 2 User Manual, M86-E01078, Madison, WI. De Meulenaer, J. & Tompa, H. (1965). Acta Cryst. 19, 1014. Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Pt1 Pt 0.300430(9) 0.400414(4) -0.006385(11) 0.0116 1.0000 Uani . . . . . . Cl1 Cl -0.1779(2) 0.27365(10) -0.2481(3) 0.1135 1.0000 Uani . U . . . . Cl2 Cl -0.2230(2) 0.29523(9) -0.0342(3) 0.1064 1.0000 Uani . . . . . . Cl3 Cl 0.6786(3) 0.36651(7) 0.7295(2) 0.1123 1.0000 Uani . . . . . . Cl4 Cl 0.59619(17) 0.31908(7) 0.5362(2) 0.0907 1.0000 Uani . . . . . . P1 P -0.13112(10) 0.36750(4) -0.59037(13) 0.0353 1.0000 Uani . . . . . . P2 P 0.19384(7) 0.35472(3) -0.07349(8) 0.0131 1.0000 Uani . . . . . . P3 P 0.36122(7) 0.39028(3) -0.16140(8) 0.0142 1.0000 Uani . . . . . . P4 P 0.39693(7) 0.37382(3) 0.16945(8) 0.0132 1.0000 Uani . . . . . . P5 P 0.18096(6) 0.44129(3) -0.00483(8) 0.0128 1.0000 Uani . . . . . . F10 F -0.2389(5) 0.3620(2) -0.6051(7) 0.066(2) 0.588(7) Uiso . . P 1 1 . F11 F -0.2334(8) 0.3840(4) -0.6095(9) 0.063(3) 0.412(7) Uiso . . P 1 2 . F20 F -0.1281(8) 0.4026(3) -0.5146(11) 0.112(4) 0.588(7) Uiso . . P 1 1 . F21 F -0.1174(10) 0.3801(4) -0.4577(13) 0.097(4) 0.412(7) Uiso . . P 1 2 . F30 F -0.1065(5) 0.34262(19) -0.4755(6) 0.0564(19) 0.588(7) Uiso . . P 1 1 . F31 F -0.1818(9) 0.3293(4) -0.5660(12) 0.090(4) 0.412(7) Uiso . . P 1 2 . F40 F -0.1334(5) 0.3315(2) -0.6680(7) 0.069(2) 0.588(7) Uiso . . P 1 1 . F41 F -0.1506(10) 0.3553(4) -0.7202(13) 0.096(4) 0.412(7) Uiso . . P 1 2 . F50 F -0.1591(6) 0.3905(3) -0.7091(8) 0.082(3) 0.588(7) Uiso . . P 1 1 . F51 F -0.0884(8) 0.4052(3) -0.6154(10) 0.073(3) 0.412(7) Uiso . . P 1 2 . F60 F -0.0220(9) 0.3727(4) -0.5769(11) 0.124(4) 0.588(7) Uiso . . P 1 1 . F61 F -0.0256(8) 0.3507(3) -0.5553(9) 0.064(3) 0.412(7) Uiso . . P 1 2 . O1 O 0.2029(2) 0.32130(8) 0.0217(2) 0.0187 1.0000 Uani . . . . . . N1 N 0.0816(2) 0.36889(9) -0.1213(3) 0.0173 1.0000 Uani . . . . . . N2 N 0.1888(2) 0.33568(9) -0.2014(3) 0.0167 1.0000 Uani . . . . . . C1 C 0.2119(3) 0.47882(10) 0.1037(3) 0.0141 1.0000 Uani . . . . . . C2 C 0.1592(3) 0.51208(11) 0.0891(3) 0.0178 1.0000 Uani . . . . . . C3 C 0.1849(3) 0.54029(11) 0.1716(4) 0.0207 1.0000 Uani . . . . . . C4 C 0.2619(3) 0.53582(12) 0.2712(4) 0.0225 1.0000 Uani . . . . . . C5 C 0.3146(3) 0.50325(12) 0.2859(4) 0.0237 1.0000 Uani . . . . . . C6 C 0.2903(3) 0.47483(11) 0.2031(3) 0.0178 1.0000 Uani . . . . . . C7 C 0.1319(3) 0.46802(10) -0.1394(3) 0.0158 1.0000 Uani . . . . . . C8 C 0.0397(3) 0.46423(12) -0.2109(4) 0.0214 1.0000 Uani . . . . . . C9 C 0.0061(3) 0.48565(14) -0.3125(4) 0.0267 1.0000 Uani . . . . . . C10 C 0.0647(3) 0.51179(13) -0.3412(4) 0.0257 1.0000 Uani . . . . . . C11 C 0.1571(3) 0.51562(12) -0.2707(4) 0.0224 1.0000 Uani . . . . . . C12 C 0.1911(3) 0.49370(11) -0.1710(3) 0.0201 1.0000 Uani . . . . . . C13 C 0.0791(3) 0.41834(10) 0.0205(3) 0.0156 1.0000 Uani . . . . . . C14 C 0.0399(3) 0.43225(11) 0.1058(4) 0.0198 1.0000 Uani . . . . . . C15 C -0.0373(3) 0.41517(13) 0.1252(4) 0.0251 1.0000 Uani . . . . . . C16 C -0.0786(3) 0.38437(12) 0.0589(4) 0.0253 1.0000 Uani . . . . . . C17 C -0.0410(3) 0.36978(12) -0.0247(4) 0.0223 1.0000 Uani . . . . . . C18 C 0.0396(3) 0.38566(11) -0.0415(3) 0.0165 1.0000 Uani . . . . . . C19 C 0.0256(3) 0.34619(14) -0.2212(4) 0.0266 1.0000 Uani . . . . . . C20 C 0.0941(3) 0.33488(14) -0.2873(4) 0.0269 1.0000 Uani . . . . . . C21 C 0.2686(3) 0.32088(11) -0.2299(3) 0.0167 1.0000 Uani . . . . . . C22 C 0.2617(3) 0.28480(12) -0.2759(4) 0.0217 1.0000 Uani . . . . . . C23 C 0.3363(3) 0.26879(12) -0.3065(4) 0.0241 1.0000 Uani . . . . . . C24 C 0.4179(3) 0.28927(12) -0.2928(4) 0.0262 1.0000 Uani . . . . . . C25 C 0.4247(3) 0.32557(12) -0.2495(4) 0.0227 1.0000 Uani . . . . . . C26 C 0.3517(3) 0.34174(11) -0.2150(3) 0.0160 1.0000 Uani . . . . . . C27 C 0.3080(3) 0.41437(11) -0.3000(3) 0.0186 1.0000 Uani . . . . . . C28 C 0.2115(3) 0.42035(12) -0.3348(4) 0.0230 1.0000 Uani . . . . . . C29 C 0.1654(4) 0.43485(14) -0.4456(4) 0.0307 1.0000 Uani . . . . . . C30 C 0.2168(4) 0.44461(14) -0.5200(4) 0.0332 1.0000 Uani . . . . . . C31 C 0.3129(4) 0.43877(14) -0.4861(4) 0.0306 1.0000 Uani . . . . . . C32 C 0.3589(3) 0.42321(12) -0.3780(4) 0.0244 1.0000 Uani . . . . . . C33 C 0.4858(3) 0.40301(11) -0.1153(3) 0.0174 1.0000 Uani . . . . . . C34 C 0.5093(3) 0.44094(12) -0.1219(4) 0.0230 1.0000 Uani . . . . . . C35 C 0.6002(3) 0.45337(13) -0.0676(4) 0.0284 1.0000 Uani . . . . . . C36 C 0.6693(3) 0.42843(14) -0.0044(4) 0.0278 1.0000 Uani . . . . . . C37 C 0.6457(3) 0.39089(13) 0.0029(4) 0.0263 1.0000 Uani . . . . . . C38 C 0.5548(3) 0.37851(12) -0.0516(4) 0.0209 1.0000 Uani . . . . . . C39 C 0.4752(3) 0.33616(11) 0.1516(3) 0.0169 1.0000 Uani . . . . . . C40 C 0.5710(3) 0.33606(13) 0.2113(4) 0.0267 1.0000 Uani . . . . . . C41 C 0.6296(3) 0.30860(14) 0.1876(5) 0.0385 1.0000 Uani . . . . . . C42 C 0.5928(3) 0.28169(13) 0.1027(5) 0.0344 1.0000 Uani . . . . . . C43 C 0.4973(3) 0.28100(12) 0.0447(4) 0.0248 1.0000 Uani . . . . . . C44 C 0.4388(3) 0.30833(11) 0.0688(3) 0.0182 1.0000 Uani . . . . . . C45 C 0.4786(3) 0.40735(11) 0.2642(3) 0.0169 1.0000 Uani . . . . . . C46 C 0.5286(3) 0.43170(11) 0.2137(4) 0.0203 1.0000 Uani . . . . . . C47 C 0.5909(3) 0.45760(12) 0.2825(4) 0.0250 1.0000 Uani . . . . . . C48 C 0.6019(3) 0.46012(14) 0.4010(4) 0.0308 1.0000 Uani . . . . . . C49 C 0.5524(4) 0.43632(14) 0.4516(4) 0.0319 1.0000 Uani . . . . . . C50 C 0.4916(3) 0.40943(12) 0.3840(3) 0.0229 1.0000 Uani . . . . . . C51 C 0.3349(3) 0.35352(11) 0.2654(3) 0.0167 1.0000 Uani . . . . . . C52 C 0.3658(3) 0.32138(13) 0.3307(4) 0.0261 1.0000 Uani . . . . . . C53 C 0.3184(4) 0.30784(14) 0.4058(4) 0.0346 1.0000 Uani . . . . . . C54 C 0.2405(4) 0.32635(13) 0.4173(4) 0.0292 1.0000 Uani . . . . . . C55 C 0.2074(3) 0.35773(13) 0.3511(4) 0.0273 1.0000 Uani . . . . . . C56 C 0.2539(3) 0.37138(12) 0.2747(4) 0.0216 1.0000 Uani . . . . . . C57 C 0.1340(3) 0.29400(12) 0.0171(4) 0.0223 1.0000 Uani . . . . . . C58 C 0.0822(3) 0.29751(13) 0.0946(4) 0.0282 1.0000 Uani . . . . . . C59 C 0.0145(4) 0.27121(15) 0.0945(5) 0.0377 1.0000 Uani . . . . . . C60 C -0.0009(4) 0.24130(14) 0.0147(5) 0.0386 1.0000 Uani . . . . . . C61 C 0.0525(4) 0.23794(14) -0.0598(5) 0.0360 1.0000 Uani . . . . . . C62 C 0.1218(4) 0.26397(13) -0.0586(4) 0.0292 1.0000 Uani . . . . . . C63 C -0.2466(9) 0.2640(4) -0.1508(11) 0.1240 1.0000 Uani . U . . . . C64 C 0.6878(5) 0.3504(2) 0.5959(6) 0.0585 1.0000 Uani . . . . . . H1 H 0.3571 0.4349 0.0175 0.0447 1.0000 Uiso R . . . . . H21 H 0.1068 0.5154 0.0232 0.0230 1.0000 Uiso R . . . . . H31 H 0.1502 0.5622 0.1589 0.0257 1.0000 Uiso R . . . . . H41 H 0.2784 0.5547 0.3268 0.0282 1.0000 Uiso R . . . . . H51 H 0.3667 0.5003 0.3518 0.0288 1.0000 Uiso R . . . . . H61 H 0.3257 0.4530 0.2133 0.0221 1.0000 Uiso R . . . . . H81 H -0.0002 0.4469 -0.1903 0.0271 1.0000 Uiso R . . . . . H91 H -0.0554 0.4819 -0.3611 0.0329 1.0000 Uiso R . . . . . H101 H 0.0416 0.5267 -0.4081 0.0319 1.0000 Uiso R . . . . . H111 H 0.1975 0.5330 -0.2903 0.0281 1.0000 Uiso R . . . . . H121 H 0.2536 0.4961 -0.1246 0.0262 1.0000 Uiso R . . . . . H141 H 0.0668 0.4535 0.1502 0.0246 1.0000 Uiso R . . . . . H151 H -0.0620 0.4244 0.1822 0.0312 1.0000 Uiso R . . . . . H161 H -0.1304 0.3732 0.0711 0.0322 1.0000 Uiso R . . . . . H171 H -0.0693 0.3491 -0.0685 0.0281 1.0000 Uiso R . . . . . H191 H -0.0257 0.3613 -0.2703 0.0342 1.0000 Uiso R . . . . . H192 H 0.0002 0.3239 -0.1927 0.0340 1.0000 Uiso R . . . . . H201 H 0.0918 0.3524 -0.3498 0.0339 1.0000 Uiso R . . . . . H202 H 0.0801 0.3101 -0.3202 0.0341 1.0000 Uiso R . . . . . H221 H 0.2064 0.2710 -0.2855 0.0268 1.0000 Uiso R . . . . . H231 H 0.3310 0.2444 -0.3359 0.0302 1.0000 Uiso R . . . . . H241 H 0.4682 0.2791 -0.3125 0.0327 1.0000 Uiso R . . . . . H251 H 0.4793 0.3395 -0.2443 0.0278 1.0000 Uiso R . . . . . H281 H 0.1770 0.4152 -0.2838 0.0289 1.0000 Uiso R . . . . . H291 H 0.1001 0.4378 -0.4693 0.0390 1.0000 Uiso R . . . . . H301 H 0.1870 0.4549 -0.5930 0.0410 1.0000 Uiso R . . . . . H311 H 0.3471 0.4455 -0.5372 0.0380 1.0000 Uiso R . . . . . H321 H 0.4239 0.4187 -0.3566 0.0300 1.0000 Uiso R . . . . . H341 H 0.4634 0.4579 -0.1628 0.0290 1.0000 Uiso R . . . . . H351 H 0.6147 0.4785 -0.0741 0.0360 1.0000 Uiso R . . . . . H361 H 0.7311 0.4369 0.0328 0.0350 1.0000 Uiso R . . . . . H371 H 0.6909 0.3741 0.0452 0.0330 1.0000 Uiso R . . . . . H381 H 0.5392 0.3532 -0.0457 0.0258 1.0000 Uiso R . . . . . H401 H 0.5959 0.3545 0.2671 0.0341 1.0000 Uiso R . . . . . H411 H 0.6937 0.3081 0.2296 0.0478 1.0000 Uiso R . . . . . H421 H 0.6323 0.2647 0.0835 0.0429 1.0000 Uiso R . . . . . H431 H 0.4732 0.2625 -0.0101 0.0311 1.0000 Uiso R . . . . . H441 H 0.3746 0.3083 0.0294 0.0231 1.0000 Uiso R . . . . . H461 H 0.5200 0.4308 0.1335 0.0259 1.0000 Uiso R . . . . . H471 H 0.6260 0.4731 0.2491 0.0320 1.0000 Uiso R . . . . . H481 H 0.6427 0.4778 0.4468 0.0381 1.0000 Uiso R . . . . . H491 H 0.5593 0.4383 0.5315 0.0399 1.0000 Uiso R . . . . . H501 H 0.4600 0.3929 0.4191 0.0288 1.0000 Uiso R . . . . . H521 H 0.4180 0.3087 0.3238 0.0330 1.0000 Uiso R . . . . . H531 H 0.3402 0.2863 0.4500 0.0430 1.0000 Uiso R . . . . . H541 H 0.2107 0.3176 0.4698 0.0361 1.0000 Uiso R . . . . . H551 H 0.1533 0.3699 0.3564 0.0343 1.0000 Uiso R . . . . . H561 H 0.2304 0.3923 0.2287 0.0269 1.0000 Uiso R . . . . . H581 H 0.0929 0.3176 0.1465 0.0348 1.0000 Uiso R . . . . . H591 H -0.0203 0.2737 0.1474 0.0467 1.0000 Uiso R . . . . . H601 H -0.0479 0.2233 0.0122 0.0480 1.0000 Uiso R . . . . . H611 H 0.0416 0.2179 -0.1122 0.0445 1.0000 Uiso R . . . . . H621 H 0.1589 0.2615 -0.1088 0.0358 1.0000 Uiso R . . . . . H631 H -0.3153 0.2659 -0.1956 0.1523 1.0000 Uiso R . . . . . H632 H -0.2317 0.2379 -0.1190 0.1525 1.0000 Uiso R . . . . . H641 H 0.6872 0.3711 0.5423 0.0711 1.0000 Uiso R . . . . . H642 H 0.7467 0.3367 0.6118 0.0711 1.0000 Uiso 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 0.01179(6) 0.01162(6) 0.01174(6) -0.00069(5) 0.00389(4) -0.00021(5) Cl1 0.0889(19) 0.143(3) 0.0981(19) -0.0108(18) 0.0128(15) 0.0079(18) Cl2 0.0926(18) 0.0970(19) 0.140(2) -0.0164(18) 0.0511(18) -0.0104(15) Cl3 0.200(3) 0.0758(15) 0.0932(17) -0.0252(13) 0.092(2) -0.0498(18) Cl4 0.0809(15) 0.0773(14) 0.0883(15) 0.0259(12) -0.0126(12) -0.0313(12) P1 0.0297(6) 0.0338(7) 0.0397(7) 0.0054(5) 0.0066(5) -0.0024(5) P2 0.0124(4) 0.0130(4) 0.0136(4) -0.0018(3) 0.0034(3) -0.0011(3) P3 0.0169(4) 0.0137(4) 0.0134(4) -0.0004(3) 0.0067(3) -0.0005(3) P4 0.0133(4) 0.0133(4) 0.0126(4) 0.0003(3) 0.0031(3) -0.0007(3) P5 0.0125(4) 0.0127(4) 0.0132(4) 0.0000(3) 0.0040(3) 0.0004(3) O1 0.0201(14) 0.0157(13) 0.0184(13) 0.0016(10) 0.0029(11) -0.0042(11) N1 0.0126(15) 0.0195(16) 0.0185(15) -0.0056(12) 0.0027(12) -0.0023(12) N2 0.0150(15) 0.0191(15) 0.0149(14) -0.0071(12) 0.0031(12) -0.0006(12) C1 0.0159(17) 0.0135(16) 0.0144(15) 0.0005(13) 0.0070(13) 0.0002(13) C2 0.0154(17) 0.0157(17) 0.0213(18) -0.0004(14) 0.0042(14) 0.0017(14) C3 0.0213(19) 0.0153(17) 0.028(2) -0.0011(15) 0.0115(16) 0.0022(15) C4 0.030(2) 0.0181(18) 0.0215(19) -0.0075(15) 0.0109(17) -0.0029(16) C5 0.028(2) 0.023(2) 0.0178(18) -0.0010(15) 0.0038(16) 0.0021(17) C6 0.0214(19) 0.0163(17) 0.0158(16) 0.0010(13) 0.0057(14) 0.0016(15) C7 0.0177(18) 0.0139(16) 0.0159(16) -0.0004(13) 0.0053(14) 0.0028(14) C8 0.0163(18) 0.025(2) 0.0215(18) 0.0024(15) 0.0040(15) 0.0025(16) C9 0.018(2) 0.037(2) 0.0210(19) 0.0016(17) -0.0003(16) 0.0058(18) C10 0.030(2) 0.029(2) 0.0170(18) 0.0041(16) 0.0058(16) 0.0106(18) C11 0.029(2) 0.0205(19) 0.0193(18) 0.0037(15) 0.0090(16) 0.0038(16) C12 0.0211(19) 0.0198(18) 0.0175(17) 0.0008(14) 0.0030(15) 0.0013(15) C13 0.0133(17) 0.0133(16) 0.0208(17) 0.0013(13) 0.0060(14) 0.0024(13) C14 0.0207(19) 0.0173(18) 0.0241(19) 0.0001(15) 0.0110(16) 0.0040(15) C15 0.024(2) 0.025(2) 0.033(2) 0.0026(17) 0.0182(18) 0.0061(17) C16 0.019(2) 0.022(2) 0.040(2) 0.0026(18) 0.0151(18) -0.0017(16) C17 0.0155(18) 0.0204(19) 0.032(2) -0.0003(16) 0.0088(16) -0.0017(15) C18 0.0128(17) 0.0172(17) 0.0202(17) 0.0011(14) 0.0059(14) 0.0026(14) C19 0.0167(19) 0.034(2) 0.025(2) -0.0117(18) -0.0005(15) -0.0021(17) C20 0.020(2) 0.038(2) 0.0181(18) -0.0118(17) -0.0018(15) 0.0008(18) C21 0.0199(18) 0.0173(17) 0.0140(16) -0.0021(13) 0.0067(14) 0.0009(14) C22 0.027(2) 0.0186(18) 0.0215(18) -0.0042(15) 0.0107(16) -0.0024(16) C23 0.034(2) 0.0158(18) 0.025(2) -0.0060(15) 0.0120(18) 0.0028(17) C24 0.028(2) 0.025(2) 0.030(2) -0.0072(17) 0.0137(18) 0.0047(17) C25 0.023(2) 0.023(2) 0.0243(19) -0.0049(16) 0.0105(16) -0.0008(16) C26 0.0209(18) 0.0153(17) 0.0134(15) -0.0004(13) 0.0074(14) 0.0007(14) C27 0.026(2) 0.0174(17) 0.0140(16) 0.0003(14) 0.0081(15) 0.0026(15) C28 0.027(2) 0.023(2) 0.0186(18) -0.0011(15) 0.0069(16) 0.0049(17) C29 0.034(2) 0.035(2) 0.021(2) -0.0003(18) 0.0034(18) 0.013(2) C30 0.051(3) 0.031(2) 0.0150(18) 0.0031(17) 0.0066(19) 0.015(2) C31 0.044(3) 0.031(2) 0.0181(19) 0.0059(17) 0.0123(19) 0.002(2) C32 0.031(2) 0.026(2) 0.0190(18) 0.0003(16) 0.0113(17) -0.0014(18) C33 0.0175(17) 0.0214(18) 0.0170(16) -0.0044(14) 0.0107(14) -0.0036(15) C34 0.027(2) 0.0208(19) 0.0229(19) 0.0006(15) 0.0094(16) -0.0025(17) C35 0.033(2) 0.026(2) 0.030(2) -0.0025(18) 0.0147(19) -0.0126(19) C36 0.021(2) 0.034(2) 0.031(2) -0.0064(18) 0.0113(17) -0.0111(18) C37 0.0184(19) 0.029(2) 0.034(2) 0.0002(18) 0.0112(17) -0.0008(17) C38 0.0209(19) 0.0206(19) 0.0248(19) -0.0010(15) 0.0122(16) -0.0023(15) C39 0.0183(18) 0.0150(17) 0.0185(17) 0.0031(13) 0.0073(14) 0.0019(14) C40 0.021(2) 0.022(2) 0.034(2) -0.0039(17) 0.0052(18) 0.0007(16) C41 0.019(2) 0.031(3) 0.063(3) -0.006(2) 0.006(2) 0.0072(19) C42 0.027(2) 0.019(2) 0.062(3) -0.003(2) 0.021(2) 0.0058(18) C43 0.031(2) 0.0153(18) 0.033(2) 0.0016(16) 0.0162(19) -0.0013(17) C44 0.0201(18) 0.0164(17) 0.0185(17) 0.0028(14) 0.0064(14) -0.0006(14) C45 0.0133(17) 0.0171(18) 0.0184(17) -0.0019(13) 0.0017(13) -0.0002(13) C46 0.0186(19) 0.0214(19) 0.0198(18) -0.0010(15) 0.0042(15) -0.0016(15) C47 0.019(2) 0.023(2) 0.031(2) -0.0017(17) 0.0050(17) -0.0048(16) C48 0.028(2) 0.032(2) 0.028(2) -0.0113(18) 0.0015(18) -0.0115(19) C49 0.036(3) 0.039(3) 0.0178(19) -0.0114(18) 0.0050(18) -0.013(2) C50 0.026(2) 0.026(2) 0.0152(17) -0.0009(15) 0.0030(15) -0.0034(16) C51 0.0209(19) 0.0161(17) 0.0138(16) -0.0006(13) 0.0061(14) -0.0019(14) C52 0.030(2) 0.025(2) 0.025(2) 0.0100(17) 0.0098(17) 0.0058(18) C53 0.053(3) 0.029(2) 0.027(2) 0.0141(19) 0.021(2) 0.006(2) C54 0.041(3) 0.026(2) 0.027(2) 0.0002(17) 0.019(2) -0.007(2) C55 0.029(2) 0.032(2) 0.026(2) -0.0033(18) 0.0144(18) -0.0040(18) C56 0.023(2) 0.023(2) 0.0208(18) 0.0021(15) 0.0082(16) -0.0005(16) C57 0.0206(19) 0.0186(19) 0.0253(19) 0.0046(15) 0.0033(16) -0.0030(15) C58 0.030(2) 0.025(2) 0.029(2) 0.0037(18) 0.0090(18) -0.0018(18) C59 0.032(3) 0.035(3) 0.050(3) 0.016(2) 0.017(2) -0.001(2) C60 0.030(3) 0.028(2) 0.053(3) 0.014(2) 0.005(2) -0.010(2) C61 0.037(3) 0.025(2) 0.039(3) 0.001(2) 0.000(2) -0.009(2) C62 0.035(3) 0.022(2) 0.029(2) 0.0004(17) 0.0088(19) -0.0013(19) C63 0.110(7) 0.144(8) 0.107(7) -0.022(6) 0.017(6) -0.016(6) C64 0.066(4) 0.054(4) 0.065(4) -0.008(3) 0.035(4) -0.015(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.054801(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pt1 . P2 . 2.2445(9) yes Pt1 . P3 . 2.3240(9) yes Pt1 . P4 . 2.3573(9) yes Pt1 . P5 . 2.3018(9) yes Pt1 . H1 . 1.468 no Cl1 . C63 . 1.799(13) yes Cl2 . C63 . 1.737(12) yes Cl3 . C64 . 1.741(7) yes Cl4 . C64 . 1.738(7) yes P1 . F10 . 1.572(8) yes P1 . F20 . 1.536(11) yes P1 . F30 . 1.583(7) yes P1 . F40 . 1.578(8) yes P1 . F50 . 1.583(9) yes P1 . F60 . 1.593(13) yes P1 . F11 . 1.582(11) yes P1 . F21 . 1.602(15) yes P1 . F31 . 1.624(13) yes P1 . F41 . 1.553(14) yes P1 . F51 . 1.554(11) yes P1 . F61 . 1.612(11) yes P2 . O1 . 1.625(3) yes P2 . N1 . 1.671(3) yes P2 . N2 . 1.654(3) yes P3 . C26 . 1.835(4) yes P3 . C27 . 1.822(4) yes P3 . C33 . 1.824(4) yes P4 . C39 . 1.831(4) yes P4 . C45 . 1.832(4) yes P4 . C51 . 1.826(4) yes P5 . C1 . 1.823(4) yes P5 . C7 . 1.822(4) yes P5 . C13 . 1.826(4) yes O1 . C57 . 1.402(5) yes N1 . C18 . 1.421(5) yes N1 . C19 . 1.474(5) yes N2 . C20 . 1.472(5) yes N2 . C21 . 1.431(5) yes C1 . C2 . 1.402(5) yes C1 . C6 . 1.398(5) yes C2 . C3 . 1.379(5) yes C2 . H21 . 0.933 no C3 . C4 . 1.389(6) yes C3 . H31 . 0.923 no C4 . C5 . 1.382(6) yes C4 . H41 . 0.926 no C5 . C6 . 1.386(5) yes C5 . H51 . 0.929 no C6 . H61 . 0.927 no C7 . C8 . 1.385(5) yes C7 . C12 . 1.399(5) yes C8 . C9 . 1.394(6) yes C8 . H81 . 0.940 no C9 . C10 . 1.388(7) yes C9 . H91 . 0.933 no C10 . C11 . 1.384(6) yes C10 . H101 . 0.935 no C11 . C12 . 1.387(5) yes C11 . H111 . 0.941 no C12 . H121 . 0.932 no C13 . C14 . 1.409(5) yes C13 . C18 . 1.410(5) yes C14 . C15 . 1.380(6) yes C14 . H141 . 0.941 no C15 . C16 . 1.384(6) yes C15 . H151 . 0.928 no C16 . C17 . 1.386(6) yes C16 . H161 . 0.916 no C17 . C18 . 1.394(5) yes C17 . H171 . 0.928 no C19 . C20 . 1.521(6) yes C19 . H191 . 0.974 no C19 . H192 . 0.983 no C20 . H201 . 0.967 no C20 . H202 . 0.962 no C21 . C22 . 1.390(5) yes C21 . C26 . 1.407(5) yes C22 . C23 . 1.392(6) yes C22 . H221 . 0.935 no C23 . C24 . 1.383(6) yes C23 . H231 . 0.930 no C24 . C25 . 1.385(6) yes C24 . H241 . 0.924 no C25 . C26 . 1.398(5) yes C25 . H251 . 0.937 no C27 . C28 . 1.384(6) yes C27 . C32 . 1.404(5) yes C28 . C29 . 1.395(6) yes C28 . H281 . 0.927 no C29 . C30 . 1.381(7) yes C29 . H291 . 0.931 no C30 . C31 . 1.378(7) yes C30 . H301 . 0.928 no C31 . C32 . 1.383(6) yes C31 . H311 . 0.939 no C32 . H321 . 0.937 no C33 . C34 . 1.404(6) yes C33 . C38 . 1.387(6) yes C34 . C35 . 1.383(6) yes C34 . H341 . 0.932 no C35 . C36 . 1.396(7) yes C35 . H351 . 0.931 no C36 . C37 . 1.392(6) yes C36 . H361 . 0.942 no C37 . C38 . 1.384(6) yes C37 . H371 . 0.927 no C38 . H381 . 0.939 no C39 . C40 . 1.388(6) yes C39 . C44 . 1.391(5) yes C40 . C41 . 1.396(6) yes C40 . H401 . 0.929 no C41 . C42 . 1.383(7) yes C41 . H411 . 0.933 no C42 . C43 . 1.380(7) yes C42 . H421 . 0.920 no C43 . C44 . 1.393(6) yes C43 . H431 . 0.922 no C44 . H441 . 0.928 no C45 . C46 . 1.394(5) yes C45 . C50 . 1.389(5) yes C46 . C47 . 1.388(6) yes C46 . H461 . 0.930 no C47 . C48 . 1.380(6) yes C47 . H471 . 0.929 no C48 . C49 . 1.378(7) yes C48 . H481 . 0.929 no C49 . C50 . 1.395(6) yes C49 . H491 . 0.933 no C50 . H501 . 0.931 no C51 . C52 . 1.384(5) yes C51 . C56 . 1.396(6) yes C52 . C53 . 1.386(6) yes C52 . H521 . 0.924 no C53 . C54 . 1.375(7) yes C53 . H531 . 0.932 no C54 . C55 . 1.373(7) yes C54 . H541 . 0.926 no C55 . C56 . 1.391(6) yes C55 . H551 . 0.932 no C56 . H561 . 0.930 no C57 . C58 . 1.379(6) yes C57 . C62 . 1.378(6) yes C58 . C59 . 1.376(7) yes C58 . H581 . 0.929 no C59 . C60 . 1.403(8) yes C59 . H591 . 0.935 no C60 . C61 . 1.366(8) yes C60 . H601 . 0.941 no C61 . C62 . 1.384(7) yes C61 . H611 . 0.932 no C62 . H621 . 0.934 no C63 . H631 . 1.003 no C63 . H632 . 1.002 no C64 . H641 . 0.976 no C64 . H642 . 0.970 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag P2 . Pt1 . P3 . 90.29(3) yes P2 . Pt1 . P4 . 101.62(3) yes P3 . Pt1 . P4 . 111.77(3) yes P2 . Pt1 . P5 . 89.89(3) yes P3 . Pt1 . P5 . 126.32(3) yes P4 . Pt1 . P5 . 120.68(3) yes P2 . Pt1 . H1 . 168.0 no P3 . Pt1 . H1 . 86.9 no P4 . Pt1 . H1 . 90.2 no P5 . Pt1 . H1 . 82.4 no F10 . P1 . F20 . 90.9(5) yes F10 . P1 . F30 . 89.3(4) yes F20 . P1 . F30 . 89.2(5) yes F10 . P1 . F40 . 89.6(4) yes F20 . P1 . F40 . 179.5(5) yes F30 . P1 . F40 . 90.8(4) yes F10 . P1 . F50 . 88.9(4) yes F20 . P1 . F50 . 93.5(6) yes F30 . P1 . F50 . 176.9(4) yes F40 . P1 . F50 . 86.6(4) yes F10 . P1 . F60 . 179.1(6) yes F20 . P1 . F60 . 90.0(6) yes F30 . P1 . F60 . 90.9(5) yes F40 . P1 . F60 . 89.6(6) yes F50 . P1 . F60 . 90.8(6) yes F11 . P1 . F21 . 82.4(7) yes F11 . P1 . F31 . 81.9(6) yes F21 . P1 . F31 . 89.1(7) yes F11 . P1 . F41 . 94.5(7) yes F21 . P1 . F41 . 176.7(7) yes F31 . P1 . F41 . 89.4(7) yes F11 . P1 . F51 . 94.7(6) yes F21 . P1 . F51 . 90.7(7) yes F31 . P1 . F51 . 176.6(6) yes F41 . P1 . F51 . 90.7(7) yes F11 . P1 . F61 . 173.6(6) yes F21 . P1 . F61 . 91.4(6) yes F31 . P1 . F61 . 96.3(6) yes F41 . P1 . F61 . 91.7(7) yes F51 . P1 . F61 . 87.1(6) yes Pt1 . P2 . O1 . 112.37(11) yes Pt1 . P2 . N1 . 115.35(12) yes O1 . P2 . N1 . 108.90(16) yes Pt1 . P2 . N2 . 117.26(12) yes O1 . P2 . N2 . 108.59(16) yes N1 . P2 . N2 . 92.62(16) yes Pt1 . P3 . C26 . 114.67(12) yes Pt1 . P3 . C27 . 119.09(13) yes C26 . P3 . C27 . 99.18(17) yes Pt1 . P3 . C33 . 108.99(12) yes C26 . P3 . C33 . 107.70(18) yes C27 . P3 . C33 . 106.28(18) yes Pt1 . P4 . C39 . 115.32(13) yes Pt1 . P4 . C45 . 113.66(13) yes C39 . P4 . C45 . 102.93(18) yes Pt1 . P4 . C51 . 115.69(13) yes C39 . P4 . C51 . 104.07(17) yes C45 . P4 . C51 . 103.62(18) yes Pt1 . P5 . C1 . 116.12(12) yes Pt1 . P5 . C7 . 115.31(12) yes C1 . P5 . C7 . 101.15(17) yes Pt1 . P5 . C13 . 113.55(12) yes C1 . P5 . C13 . 104.72(17) yes C7 . P5 . C13 . 104.45(17) yes P2 . O1 . C57 . 125.2(3) yes P2 . N1 . C18 . 119.6(3) yes P2 . N1 . C19 . 111.9(3) yes C18 . N1 . C19 . 121.3(3) yes P2 . N2 . C20 . 114.9(3) yes P2 . N2 . C21 . 124.2(3) yes C20 . N2 . C21 . 120.9(3) yes P5 . C1 . C2 . 121.3(3) yes P5 . C1 . C6 . 119.8(3) yes C2 . C1 . C6 . 118.9(3) yes C1 . C2 . C3 . 120.2(4) yes C1 . C2 . H21 . 120.3 no C3 . C2 . H21 . 119.5 no C2 . C3 . C4 . 120.6(4) yes C2 . C3 . H31 . 118.6 no C4 . C3 . H31 . 120.8 no C3 . C4 . C5 . 119.6(4) yes C3 . C4 . H41 . 120.2 no C5 . C4 . H41 . 120.1 no C4 . C5 . C6 . 120.5(4) yes C4 . C5 . H51 . 119.8 no C6 . C5 . H51 . 119.7 no C1 . C6 . C5 . 120.2(4) yes C1 . C6 . H61 . 119.5 no C5 . C6 . H61 . 120.3 no P5 . C7 . C8 . 123.5(3) yes P5 . C7 . C12 . 117.6(3) yes C8 . C7 . C12 . 118.9(4) yes C7 . C8 . C9 . 120.8(4) yes C7 . C8 . H81 . 119.2 no C9 . C8 . H81 . 120.0 no C8 . C9 . C10 . 119.8(4) yes C8 . C9 . H91 . 119.4 no C10 . C9 . H91 . 120.8 no C9 . C10 . C11 . 119.8(4) yes C9 . C10 . H101 . 119.8 no C11 . C10 . H101 . 120.4 no C10 . C11 . C12 . 120.3(4) yes C10 . C11 . H111 . 120.3 no C12 . C11 . H111 . 119.3 no C7 . C12 . C11 . 120.3(4) yes C7 . C12 . H121 . 119.8 no C11 . C12 . H121 . 119.9 no P5 . C13 . C14 . 120.5(3) yes P5 . C13 . C18 . 121.1(3) yes C14 . C13 . C18 . 118.3(3) yes C13 . C14 . C15 . 120.9(4) yes C13 . C14 . H141 . 119.6 no C15 . C14 . H141 . 119.5 no C14 . C15 . C16 . 120.1(4) yes C14 . C15 . H151 . 120.1 no C16 . C15 . H151 . 119.8 no C15 . C16 . C17 . 120.3(4) yes C15 . C16 . H161 . 120.1 no C17 . C16 . H161 . 119.6 no C16 . C17 . C18 . 120.3(4) yes C16 . C17 . H171 . 119.6 no C18 . C17 . H171 . 120.2 no N1 . C18 . C13 . 120.2(3) yes N1 . C18 . C17 . 119.9(4) yes C13 . C18 . C17 . 119.9(4) yes N1 . C19 . C20 . 105.3(3) yes N1 . C19 . H191 . 109.4 no C20 . C19 . H191 . 111.0 no N1 . C19 . H192 . 110.1 no C20 . C19 . H192 . 110.8 no H191 . C19 . H192 . 110.0 no C19 . C20 . N2 . 106.3(3) yes C19 . C20 . H201 . 111.0 no N2 . C20 . H201 . 109.2 no C19 . C20 . H202 . 111.1 no N2 . C20 . H202 . 110.2 no H201 . C20 . H202 . 108.9 no N2 . C21 . C22 . 117.9(3) yes N2 . C21 . C26 . 122.4(3) yes C22 . C21 . C26 . 119.7(4) yes C21 . C22 . C23 . 120.9(4) yes C21 . C22 . H221 . 119.4 no C23 . C22 . H221 . 119.7 no C22 . C23 . C24 . 119.6(4) yes C22 . C23 . H231 . 119.9 no C24 . C23 . H231 . 120.5 no C23 . C24 . C25 . 120.0(4) yes C23 . C24 . H241 . 120.8 no C25 . C24 . H241 . 119.3 no C24 . C25 . C26 . 121.3(4) yes C24 . C25 . H251 . 118.9 no C26 . C25 . H251 . 119.8 no P3 . C26 . C21 . 121.0(3) yes P3 . C26 . C25 . 120.4(3) yes C21 . C26 . C25 . 118.5(3) yes P3 . C27 . C28 . 118.2(3) yes P3 . C27 . C32 . 122.5(3) yes C28 . C27 . C32 . 119.0(4) yes C27 . C28 . C29 . 120.7(4) yes C27 . C28 . H281 . 120.1 no C29 . C28 . H281 . 119.2 no C28 . C29 . C30 . 119.8(5) yes C28 . C29 . H291 . 119.9 no C30 . C29 . H291 . 120.4 no C29 . C30 . C31 . 120.0(4) yes C29 . C30 . H301 . 120.4 no C31 . C30 . H301 . 119.6 no C30 . C31 . C32 . 120.8(4) yes C30 . C31 . H311 . 119.3 no C32 . C31 . H311 . 120.0 no C27 . C32 . C31 . 119.8(4) yes C27 . C32 . H321 . 120.0 no C31 . C32 . H321 . 120.2 no P3 . C33 . C34 . 118.0(3) yes P3 . C33 . C38 . 121.7(3) yes C34 . C33 . C38 . 118.8(4) yes C33 . C34 . C35 . 120.4(4) yes C33 . C34 . H341 . 120.0 no C35 . C34 . H341 . 119.6 no C34 . C35 . C36 . 120.4(4) yes C34 . C35 . H351 . 119.2 no C36 . C35 . H351 . 120.5 no C35 . C36 . C37 . 119.2(4) yes C35 . C36 . H361 . 120.4 no C37 . C36 . H361 . 120.4 no C36 . C37 . C38 . 120.4(4) yes C36 . C37 . H371 . 119.9 no C38 . C37 . H371 . 119.7 no C33 . C38 . C37 . 120.9(4) yes C33 . C38 . H381 . 119.1 no C37 . C38 . H381 . 120.0 no P4 . C39 . C40 . 122.2(3) yes P4 . C39 . C44 . 118.8(3) yes C40 . C39 . C44 . 118.9(4) yes C39 . C40 . C41 . 120.3(4) yes C39 . C40 . H401 . 119.5 no C41 . C40 . H401 . 120.2 no C40 . C41 . C42 . 120.2(5) yes C40 . C41 . H411 . 120.2 no C42 . C41 . H411 . 119.6 no C41 . C42 . C43 . 120.0(4) yes C41 . C42 . H421 . 119.9 no C43 . C42 . H421 . 120.1 no C42 . C43 . C44 . 119.8(4) yes C42 . C43 . H431 . 119.4 no C44 . C43 . H431 . 120.9 no C43 . C44 . C39 . 120.8(4) yes C43 . C44 . H441 . 120.3 no C39 . C44 . H441 . 118.8 no P4 . C45 . C46 . 118.6(3) yes P4 . C45 . C50 . 122.2(3) yes C46 . C45 . C50 . 119.2(4) yes C45 . C46 . C47 . 120.3(4) yes C45 . C46 . H461 . 120.1 no C47 . C46 . H461 . 119.6 no C46 . C47 . C48 . 120.2(4) yes C46 . C47 . H471 . 120.0 no C48 . C47 . H471 . 119.7 no C47 . C48 . C49 . 119.9(4) yes C47 . C48 . H481 . 120.2 no C49 . C48 . H481 . 120.0 no C48 . C49 . C50 . 120.5(4) yes C48 . C49 . H491 . 119.8 no C50 . C49 . H491 . 119.8 no C49 . C50 . C45 . 119.9(4) yes C49 . C50 . H501 . 120.1 no C45 . C50 . H501 . 120.0 no P4 . C51 . C52 . 122.6(3) yes P4 . C51 . C56 . 118.8(3) yes C52 . C51 . C56 . 118.7(4) yes C51 . C52 . C53 . 120.5(4) yes C51 . C52 . H521 . 120.0 no C53 . C52 . H521 . 119.6 no C52 . C53 . C54 . 120.4(4) yes C52 . C53 . H531 . 119.7 no C54 . C53 . H531 . 119.8 no C53 . C54 . C55 . 120.0(4) yes C53 . C54 . H541 . 119.8 no C55 . C54 . H541 . 120.2 no C54 . C55 . C56 . 120.0(4) yes C54 . C55 . H551 . 120.4 no C56 . C55 . H551 . 119.5 no C51 . C56 . C55 . 120.4(4) yes C51 . C56 . H561 . 119.8 no C55 . C56 . H561 . 119.8 no O1 . C57 . C58 . 117.5(4) yes O1 . C57 . C62 . 120.9(4) yes C58 . C57 . C62 . 121.6(4) yes C57 . C58 . C59 . 119.7(5) yes C57 . C58 . H581 . 120.0 no C59 . C58 . H581 . 120.2 no C58 . C59 . C60 . 119.1(5) yes C58 . C59 . H591 . 119.4 no C60 . C59 . H591 . 121.5 no C59 . C60 . C61 . 120.2(5) yes C59 . C60 . H601 . 120.3 no C61 . C60 . H601 . 119.4 no C60 . C61 . C62 . 120.9(5) yes C60 . C61 . H611 . 119.3 no C62 . C61 . H611 . 119.8 no C61 . C62 . C57 . 118.4(5) yes C61 . C62 . H621 . 120.9 no C57 . C62 . H621 . 120.7 no Cl1 . C63 . Cl2 . 112.4(7) yes Cl1 . C63 . H631 . 109.1 no Cl2 . C63 . H631 . 108.1 no Cl1 . C63 . H632 . 108.7 no Cl2 . C63 . H632 . 108.7 no H631 . C63 . H632 . 109.8 no Cl3 . C64 . Cl4 . 108.6(4) yes Cl3 . C64 . H641 . 111.5 no Cl4 . C64 . H641 . 111.4 no Cl3 . C64 . H642 . 107.6 no Cl4 . C64 . H642 . 107.9 no H641 . C64 . H642 . 109.7 no _iucr_refine_instruction_details_constraints ; # # Punched on 05/10/11 at 09:09:15 # #LIST 12 BLOCK CONT SCALE CONT PT ( 1 ,X'S,U'S) UNTIL P ( 5 ) CONT F ( 10 ,X'S,U[ISO]) UNTIL F ( 61 ) CONT O ( 1 ,X'S,U'S) UNTIL C ( 64 ) SUMFIX PART(1001,OCC) AND PART(1002,OCC) RIDE PT ( 1,X'S) H ( 1,X'S) RIDE C ( 2,X'S) H ( 21,X'S) RIDE C ( 3,X'S) H ( 31,X'S) RIDE C ( 4,X'S) H ( 41,X'S) RIDE C ( 5,X'S) H ( 51,X'S) RIDE C ( 6,X'S) H ( 61,X'S) RIDE C ( 8,X'S) H ( 81,X'S) RIDE C ( 9,X'S) H ( 91,X'S) RIDE C ( 10,X'S) H ( 101,X'S) RIDE C ( 11,X'S) H ( 111,X'S) RIDE C ( 12,X'S) H ( 121,X'S) RIDE C ( 14,X'S) H ( 141,X'S) RIDE C ( 15,X'S) H ( 151,X'S) RIDE C ( 16,X'S) H ( 161,X'S) RIDE C ( 17,X'S) H ( 171,X'S) RIDE C ( 19,X'S) H ( 191,X'S) H ( 192,X'S) RIDE C ( 20,X'S) H ( 201,X'S) H ( 202,X'S) RIDE C ( 22,X'S) H ( 221,X'S) RIDE C ( 23,X'S) H ( 231,X'S) RIDE C ( 24,X'S) H ( 241,X'S) RIDE C ( 25,X'S) H ( 251,X'S) RIDE C ( 28,X'S) H ( 281,X'S) RIDE C ( 29,X'S) H ( 291,X'S) RIDE C ( 30,X'S) H ( 301,X'S) RIDE C ( 31,X'S) H ( 311,X'S) RIDE C ( 32,X'S) H ( 321,X'S) RIDE C ( 34,X'S) H ( 341,X'S) RIDE C ( 35,X'S) H ( 351,X'S) RIDE C ( 36,X'S) H ( 361,X'S) RIDE C ( 37,X'S) H ( 371,X'S) RIDE C ( 38,X'S) H ( 381,X'S) RIDE C ( 40,X'S) H ( 401,X'S) RIDE C ( 41,X'S) H ( 411,X'S) RIDE C ( 42,X'S) H ( 421,X'S) RIDE C ( 43,X'S) H ( 431,X'S) RIDE C ( 44,X'S) H ( 441,X'S) RIDE C ( 46,X'S) H ( 461,X'S) RIDE C ( 47,X'S) H ( 471,X'S) RIDE C ( 48,X'S) H ( 481,X'S) RIDE C ( 49,X'S) H ( 491,X'S) RIDE C ( 50,X'S) H ( 501,X'S) RIDE C ( 52,X'S) H ( 521,X'S) RIDE C ( 53,X'S) H ( 531,X'S) RIDE C ( 54,X'S) H ( 541,X'S) RIDE C ( 55,X'S) H ( 551,X'S) RIDE C ( 56,X'S) H ( 561,X'S) RIDE C ( 58,X'S) H ( 581,X'S) RIDE C ( 59,X'S) H ( 591,X'S) RIDE C ( 60,X'S) H ( 601,X'S) RIDE C ( 61,X'S) H ( 611,X'S) RIDE C ( 62,X'S) H ( 621,X'S) RIDE C ( 63,X'S) H ( 631,X'S) H ( 632,X'S) RIDE C ( 64,X'S) H ( 641,X'S) H ( 642,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 05/10/11 at 09:09:15 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) U(IJ)'S 0.0, 0.010000 = CL(1) TO C(63) END ; #=== data_6PF6 _database_code_depnum_ccdc_archive 'CCDC 869436' #TrackingRef '- combined_bf.cif' _audit_creation_date 12-02-16 _audit_creation_method CRYSTALS_ver_14.40 _oxford_structure_analysis_title 'bfpan_740_0m in P2(1)/n' _chemical_name_systematic ? _chemical_melting_point ? _vrf_PLAT112_6PF6 ; PROBLEM: ADDSYM Detects Additional (Pseudo) Symm. Elem... n RESPONSE: There are two molecules of each platinum complex & anion in the asymmetric unit; the second molecule has a numbering scheme 100 greater than the first molecule. The two molecules are nearly related by the n-glide operation; however, it is apparent that the condition is inexact, as 25% of the data for which the condition I(h0l), h+l odd absent applies, has an I/sigma(I) value greater than 3.0. Such an occurrence could also arise from twinning. However, ROTAX, TwinRotMat, and a plot of Fo vs. Fc revealed no evidence for twinning. Finally, it is important to point out that CheckCIF ignores disordered atoms in its assessment of missed symmetry. Here, it is the disordered atoms that validate the choice of P21. For example, the occupancies of the disordered central P atoms are 94/6 in one molecule and 52/48 in the other. ; _vrf_PLAT111_6PF6 ; PROBLEM: ADDSYM Detects (Pseudo) Centre of Symmetry ..... 100 PerFi RESPONSE: There are two molecules of each platinum complex & anion in the asymmetric unit; the second molecule has a numbering scheme 100 greater than the first molecule. The two molecules are nearly related by the n-glide operation; however, it is apparent that the condition is inexact, as 25% of the data for which the condition I(h0l), h+l odd absent applies, has an I/sigma(I) value greater than 3.0. For this Alert, the punch line is that if we have no n glide, we have no 1-bar either. All this could also arise from twinning. However, ROTAX, TwinRotMat, and a plot of Fo vs. Fc revealed no evidence for twinning. Finally, it is important to point out that CheckCIF ignores disordered atoms in its assessment of missed symmetry. Here, it is the disordered atoms that validate the choice of P21. For example, the occupancies of the disordered central P atoms are 94/6 in one molecule and 52/48 in the other. ; _vrf_PLAT113_6PF6 ; PROBLEM: ADDSYM Suggests Possible Pseudo/New Space-group. P21/c RESPONSE: CheckCIF is in fact referring to the transformed cell, after acknowledging that the data fits P21/n fairly well. There are two molecules of each platinum complex & anion in the asymmetric unit; the second molecule has a numbering scheme 100 greater than the first molecule. The two molecules are nearly related by the n-glide operation; however, it is apparent that the condition is inexact, as 25% of the data for which the condition I(h0l), h+l odd absent applies, has an I/sigma(I) value greater than 3.0. For this Alert, the punch line is that if we have no n glide, we have no 1-bar either. Then we do not have P21/n, then we do not have P21/c. All this could also arise from twinning. However, ROTAX, TwinRotMat, and a plot of Fo vs. Fc revealed no evidence for twinning. Finally, it is important to point out that CheckCIF ignores disordered atoms in its assessment of missed symmetry. Here, it is the disordered atoms that validate the choice of P21. For example, the occupancies of the disordered central P atoms are 94/6 in one molecule and 52/48 in the other. ; _cell_length_a 12.1189(4) _cell_length_b 13.4744(5) _cell_length_c 22.8621(9) _cell_angle_alpha 90 _cell_angle_beta 98.743(2) _cell_angle_gamma 90 _cell_volume 3689.9(2) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21 1 ' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y+1/2,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Pt -1.7033 8.3905 27.0059 1.5129 17.7639 8.8117 15.7131 0.4246 5.7837 38.6103 11.6883 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C38 H32 Cl1 F6 N2 P4 Pt1 # Dc = 1.77 Fooo = 1932.00 Mu = 41.11 M = 1970.22 # Found Formula = C38 H32 Cl1 F6.00 N2 P4 Pt1 # Dc = 1.77 FOOO = 1932.00 Mu = 41.11 M = 1970.22 _chemical_formula_sum 'C38 H32 Cl1 F6.00 N2 P4 Pt1' _chemical_formula_moiety 'C38 H32 Cl N2 P3 Pt, F6 P' _chemical_compound_source ? _chemical_formula_weight 985.11 _cell_measurement_reflns_used 9915 _cell_measurement_theta_min 2 _cell_measurement_theta_max 29 _cell_measurement_temperature 120 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_min 0.060 _exptl_crystal_size_mid 0.110 _exptl_crystal_size_max 0.550 _exptl_crystal_density_diffrn 1.773 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1932 _exptl_absorpt_coefficient_mu 4.111 # Sheldrick geometric approximatio 0.64 0.78 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Analytical Absorption (De Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_min 0.64 _exptl_absorpt_correction_T_max 0.78 _diffrn_measurement_device_type 'Bruker Kappa Apex2' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 120 _diffrn_reflns_number 21159 _reflns_number_total 21159 _diffrn_reflns_av_R_equivalents 0.044 # Number of reflections without Friedels Law is 21159 # Number of reflections with Friedels Law is 11176 # Theoretical number of reflections is about 10807 _diffrn_reflns_theta_min 1.700 _diffrn_reflns_theta_max 30.046 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.046 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 32 _reflns_limit_h_min -17 _reflns_limit_h_max 16 _reflns_limit_k_min -18 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 32 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -2.13 _refine_diff_density_max 2.16 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 21159 _refine_ls_number_restraints 7 _refine_ls_number_parameters 952 _oxford_refine_ls_R_factor_ref 0.0552 _refine_ls_wR_factor_ref 0.0835 _refine_ls_goodness_of_fit_ref 0.9786 _refine_ls_shift/su_max 0.0061564 _refine_ls_shift/su_mean 0.0001530 # The values computed with all filters except I/sigma _oxford_reflns_number_all 21159 _refine_ls_R_factor_all 0.0552 _refine_ls_wR_factor_all 0.0835 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 17543 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_gt 0.0794 _refine_ls_abs_structure_Flack 0.500(7) _refine_ls_abs_structure_details 'Flack (1983), 9983 Friedel-pairs' # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration ad _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr #undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 6.59P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Bruker Analytical X-ray Systems, Inc., 2006. Apex2, Version 2 User Manual, M86-E01078, Madison, WI. De Meulenaer, J. & Tompa, H. (1965). Acta Cryst. 19, 1014. Flack, H. D. (1983). Acta Cryst. A39, 876-881. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Pt1 Pt -0.008098(19) 0.19951(10) 0.567069(10) 0.0170 1.0000 Uani . . . . . . Pt11 Pt 0.49966(2) 0.30558(10) 0.929336(11) 0.0223 1.0000 Uani . . . . . . Cl1 Cl -0.05926(17) 0.3599(2) 0.53223(11) 0.0335 1.0000 Uani . . . . . . Cl11 Cl 0.5644(2) 0.1601(2) 0.97594(13) 0.0530 1.0000 Uani . . . . . . P1 P 0.13568(14) 0.1955(3) 0.51263(8) 0.0188 1.0000 Uani . . . . . . P2 P 0.02130(17) 0.04393(19) 0.58669(10) 0.0175 0.940(5) Uani . U P . . . P3 P 0.064(2) 0.080(3) 0.6248(14) 0.0162 0.060(5) Uani . U P . . . P4 P -0.12394(14) 0.2109(2) 0.63758(8) 0.0180 1.0000 Uani . . . . . . P5 P 0.0318(2) 0.8021(3) 0.84664(12) 0.0491 1.0000 Uani . . . . . . P101 P 0.35689(15) 0.3088(3) 0.98560(8) 0.0208 1.0000 Uani . . . . . . P102 P 0.4217(3) 0.4280(3) 0.87313(15) 0.0165 0.524(6) Uani . . P . . . P103 P 0.4752(4) 0.4613(4) 0.9135(2) 0.0218 0.476(6) Uani . . P . . . P104 P 0.61749(15) 0.2935(2) 0.85972(9) 0.0201 1.0000 Uani . . . . . . P105 P 0.4605(2) 0.7035(3) 0.65536(12) 0.0489 1.0000 Uani . . . . . . F1 F -0.0816(6) 0.8192(7) 0.8035(4) 0.0985 1.0000 Uani . . . . . . F2 F -0.0085(7) 0.8775(7) 0.8954(4) 0.043(2) 0.615(10) Uiso . . P 1 2 . F3 F -0.0113(7) 0.7136(8) 0.8763(4) 0.058(3) 0.615(10) Uiso . . P 1 2 . F4 F 0.1004(9) 0.7266(9) 0.8044(5) 0.085(4) 0.615(10) Uiso . . P 1 2 . F5 F 0.0818(10) 0.8933(10) 0.8185(5) 0.075(3) 0.615(10) Uiso . . P 1 2 . F6 F 0.1478(5) 0.7864(7) 0.8901(3) 0.0795 1.0000 Uani . . . . . . F21 F 0.0382(13) 0.9108(12) 0.8591(8) 0.066(5) 0.385(10) Uiso . . P 1 1 . F22 F -0.0288(16) 0.776(2) 0.8984(9) 0.107(7) 0.385(10) Uiso . . P 1 1 . F23 F 0.0247(8) 0.6869(8) 0.8257(5) 0.035(3) 0.385(10) Uiso . . P 1 1 . F24 F 0.082(2) 0.818(2) 0.7860(12) 0.133(9) 0.385(10) Uiso . . P 1 1 . F101 F 0.5775(6) 0.6921(8) 0.6950(3) 0.1025 1.0000 Uani . . . . . . F102 F 0.4402(9) 0.8005(9) 0.6872(5) 0.067(3) 0.549(10) Uiso . . P 1 3 . F103 F 0.3855(9) 0.6326(9) 0.6915(5) 0.067(3) 0.549(10) Uiso . . P 1 3 . F104 F 0.4826(7) 0.6115(7) 0.6187(4) 0.041(2) 0.549(10) Uiso . . P 1 3 . F105 F 0.5239(8) 0.7792(9) 0.6082(5) 0.055(3) 0.549(10) Uiso . . P 1 3 . F106 F 0.3423(5) 0.7174(6) 0.6148(3) 0.0718 1.0000 Uani . . . . . . F121 F 0.4201(16) 0.7248(17) 0.7175(9) 0.114(7) 0.451(10) Uiso . . P 1 4 . F122 F 0.4442(10) 0.5853(10) 0.6686(6) 0.056(3) 0.451(10) Uiso . . P 1 4 . F123 F 0.5127(11) 0.6635(13) 0.5991(6) 0.075(5) 0.451(10) Uiso . . P 1 4 . F124 F 0.4939(8) 0.8103(8) 0.6468(5) 0.045(3) 0.451(10) Uiso . . P 1 4 . N1 N 0.1492(5) -0.0004(5) 0.5981(3) 0.0207 1.0000 Uani . . . . . . N2 N -0.0152(6) -0.0017(6) 0.6490(3) 0.0225 1.0000 Uani . . . . . . N101 N 0.3443(5) 0.5077(6) 0.9028(3) 0.0255 1.0000 Uani . . . . . . N102 N 0.5077(6) 0.5115(6) 0.8500(3) 0.0247 1.0000 Uani . . . . . . C1 C 0.2001(6) 0.3176(8) 0.5156(3) 0.0240 1.0000 Uani . . . . . . C2 C 0.2294(6) 0.3660(7) 0.4668(4) 0.0239 1.0000 Uani . . . . . . C3 C 0.2769(6) 0.4602(8) 0.4738(4) 0.0280 1.0000 Uani . . . . . . C4 C 0.2938(7) 0.5057(8) 0.5280(5) 0.0360 1.0000 Uani . . . . . . C5 C 0.2648(7) 0.4584(8) 0.5786(4) 0.0327 1.0000 Uani . . . . . . C6 C 0.2181(7) 0.3647(8) 0.5729(5) 0.0288 1.0000 Uani . . . . . . C7 C 0.0905(6) 0.1635(6) 0.4357(3) 0.0204 1.0000 Uani . . . . . . C8 C -0.0221(7) 0.1615(7) 0.4150(4) 0.0269 1.0000 Uani . . . . . . C9 C -0.0592(9) 0.1394(7) 0.3559(4) 0.0375 1.0000 Uani . . . . . . C10 C 0.0174(10) 0.1220(8) 0.3173(4) 0.0457 1.0000 Uani . . . . . . C11 C 0.1303(10) 0.1242(8) 0.3376(4) 0.0403 1.0000 Uani . . . . . . C12 C 0.1676(8) 0.1406(9) 0.3974(4) 0.0357 1.0000 Uani . . . . . . C13 C 0.2513(6) 0.1170(6) 0.5407(3) 0.0169 1.0000 Uani . . . . . . C14 C 0.3576(6) 0.1427(7) 0.5262(4) 0.0256 1.0000 Uani . . . . . . C15 C 0.4494(6) 0.0831(7) 0.5418(4) 0.0261 1.0000 Uani . . . . . . C16 C 0.4435(7) 0.0033(8) 0.5735(4) 0.0313 1.0000 Uani . . . . . . C17 C 0.3423(6) -0.0270(7) 0.5903(4) 0.0226 1.0000 Uani . . . . . . C18 C 0.2452(6) 0.0297(7) 0.5741(4) 0.0180 1.0000 Uani . . . . . . C19 C 0.1611(8) -0.0834(8) 0.6415(5) 0.0425 1.0000 Uani . . . . . . C20 C 0.0412(7) -0.0973(7) 0.6588(4) 0.0314 1.0000 Uani . . . . . . C21 C -0.1257(7) 0.0055(8) 0.6621(4) 0.0249 1.0000 Uani . . . . . . C22 C -0.1770(7) -0.0791(7) 0.6828(4) 0.0243 1.0000 Uani . . . . . . C23 C -0.2842(7) -0.0745(7) 0.6958(4) 0.0234 1.0000 Uani . . . . . . C24 C -0.3420(6) 0.0137(7) 0.6924(4) 0.0232 1.0000 Uani . . . . . . C25 C -0.2901(7) 0.0974(7) 0.6739(4) 0.0227 1.0000 Uani . . . . . . C26 C -0.1830(6) 0.0961(6) 0.6601(3) 0.0166 1.0000 Uani . . . . . . C27 C -0.0378(6) 0.2590(6) 0.7026(3) 0.0186 1.0000 Uani . . . . . . C28 C -0.0242(7) 0.2076(10) 0.7566(3) 0.0314 1.0000 Uani . . . . . . C29 C 0.0433(8) 0.2423(8) 0.8057(4) 0.0417 1.0000 Uani . . . . . . C30 C 0.1043(10) 0.3293(9) 0.8001(4) 0.0531 1.0000 Uani . . . . . . C31 C 0.0932(7) 0.3805(8) 0.7478(5) 0.0373 1.0000 Uani . . . . . . C32 C 0.0225(7) 0.3439(8) 0.6988(4) 0.0287 1.0000 Uani . . . . . . C33 C -0.2410(5) 0.2932(7) 0.6179(3) 0.0190 1.0000 Uani . . . . . . C34 C -0.2624(7) 0.3727(8) 0.6547(4) 0.0270 1.0000 Uani . . . . . . C35 C -0.3523(7) 0.4342(7) 0.6367(5) 0.0372 1.0000 Uani . . . . . . C36 C -0.4209(7) 0.4181(8) 0.5837(5) 0.0357 1.0000 Uani . . . . . . C37 C -0.4005(7) 0.3404(7) 0.5480(4) 0.0373 1.0000 Uani . . . . . . C38 C -0.3080(6) 0.2777(7) 0.5631(4) 0.0279 1.0000 Uani . . . . . . C101 C 0.4012(7) 0.3437(7) 1.0619(4) 0.0301 1.0000 Uani . . . . . . C102 C 0.5151(9) 0.3508(8) 1.0830(5) 0.0401 1.0000 Uani . . . . . . C103 C 0.5526(10) 0.3692(10) 1.1423(5) 0.0544 1.0000 Uani . . . . . . C104 C 0.4752(10) 0.3821(8) 1.1804(4) 0.0435 1.0000 Uani . . . . . . C105 C 0.3655(11) 0.3798(10) 1.1573(5) 0.0563 1.0000 Uani . . . . . . C106 C 0.3271(9) 0.3566(9) 1.1002(4) 0.0401 1.0000 Uani . . . . . . C107 C 0.2963(5) 0.1854(7) 0.9810(3) 0.0190 1.0000 Uani . . . . . . C108 C 0.2738(7) 0.1347(8) 1.0305(4) 0.0307 1.0000 Uani . . . . . . C109 C 0.2324(7) 0.0382(8) 1.0238(4) 0.0369 1.0000 Uani . . . . . . C110 C 0.2116(7) -0.0062(8) 0.9703(5) 0.0322 1.0000 Uani . . . . . . C111 C 0.2285(7) 0.0479(8) 0.9205(5) 0.0368 1.0000 Uani . . . . . . C112 C 0.2702(8) 0.1429(9) 0.9278(4) 0.0317 1.0000 Uani . . . . . . C113 C 0.2391(7) 0.3909(7) 0.9584(4) 0.0267 1.0000 Uani . . . . . . C114 C 0.1396(8) 0.3626(9) 0.9747(4) 0.0390 1.0000 Uani . . . . . . C115 C 0.0416(8) 0.4161(8) 0.9594(4) 0.0366 1.0000 Uani . . . . . . C116 C 0.0512(7) 0.5080(8) 0.9280(4) 0.0292 1.0000 Uani . . . . . . C117 C 0.1480(7) 0.5336(8) 0.9101(4) 0.0337 1.0000 Uani . . . . . . C118 C 0.2461(7) 0.4766(7) 0.9236(4) 0.0255 1.0000 Uani . . . . . . C119 C 0.3397(6) 0.5949(9) 0.8630(5) 0.0432 1.0000 Uani . . . . . . C120 C 0.4528(8) 0.6130(8) 0.8497(6) 0.0464 1.0000 Uani . . . . . . C121 C 0.6150(7) 0.5007(6) 0.8340(4) 0.0193 1.0000 Uani . . . . . . C122 C 0.6680(7) 0.5870(8) 0.8178(4) 0.0259 1.0000 Uani . . . . . . C123 C 0.7735(8) 0.5820(9) 0.8046(4) 0.0335 1.0000 Uani . . . . . . C124 C 0.8320(7) 0.4941(8) 0.8070(4) 0.0296 1.0000 Uani . . . . . . C125 C 0.7831(7) 0.4070(8) 0.8229(4) 0.0266 1.0000 Uani . . . . . . C126 C 0.6731(6) 0.4107(7) 0.8379(3) 0.0226 1.0000 Uani . . . . . . C127 C 0.7346(6) 0.2121(9) 0.8796(4) 0.0273 1.0000 Uani . . . . . . C128 C 0.7577(7) 0.1348(8) 0.8439(4) 0.0258 1.0000 Uani . . . . . . C129 C 0.8491(7) 0.0741(8) 0.8629(4) 0.0352 1.0000 Uani . . . . . . C130 C 0.9156(7) 0.0918(9) 0.9168(5) 0.0417 1.0000 Uani . . . . . . C131 C 0.8920(6) 0.1702(8) 0.9524(4) 0.0341 1.0000 Uani . . . . . . C132 C 0.8033(6) 0.2285(7) 0.9324(4) 0.0289 1.0000 Uani . . . . . . C133 C 0.5289(7) 0.2441(7) 0.7948(4) 0.0283 1.0000 Uani . . . . . . C134 C 0.5193(7) 0.2929(9) 0.7411(4) 0.0318 1.0000 Uani . . . . . . C135 C 0.4416(8) 0.2572(9) 0.6941(4) 0.0423 1.0000 Uani . . . . . . C136 C 0.3811(8) 0.1751(8) 0.6995(4) 0.0437 1.0000 Uani . . . . . . C137 C 0.3928(9) 0.1244(8) 0.7535(5) 0.0465 1.0000 Uani . . . . . . C138 C 0.4672(8) 0.1565(7) 0.8011(5) 0.0354 1.0000 Uani . . . . . . H21 H 0.2173 0.3350 0.4297 0.0289 1.0000 Uiso R . . . . . H31 H 0.2977 0.4921 0.4407 0.0331 1.0000 Uiso R . . . . . H41 H 0.3251 0.5693 0.5319 0.0426 1.0000 Uiso R . . . . . H51 H 0.2756 0.4903 0.6157 0.0392 1.0000 Uiso R . . . . . H61 H 0.1999 0.3316 0.6059 0.0350 1.0000 Uiso R . . . . . H81 H -0.0738 0.1776 0.4392 0.0318 1.0000 Uiso R . . . . . H91 H -0.1359 0.1352 0.3421 0.0446 1.0000 Uiso R . . . . . H101 H -0.0076 0.1102 0.2777 0.0533 1.0000 Uiso R . . . . . H111 H 0.1813 0.1152 0.3116 0.0489 1.0000 Uiso R . . . . . H121 H 0.2427 0.1356 0.4122 0.0427 1.0000 Uiso R . . . . . H141 H 0.3660 0.2015 0.5058 0.0309 1.0000 Uiso R . . . . . H151 H 0.5157 0.1002 0.5295 0.0319 1.0000 Uiso R . . . . . H161 H 0.5070 -0.0344 0.5852 0.0381 1.0000 Uiso R . . . . . H171 H 0.3391 -0.0841 0.6122 0.0269 1.0000 Uiso R . . . . . H191 H 0.1855 -0.1428 0.6234 0.0512 1.0000 Uiso R . . . . . H192 H 0.2156 -0.0653 0.6755 0.0509 1.0000 Uiso R . . . . . H201 H 0.0002 -0.1490 0.6358 0.0377 1.0000 Uiso R . . . . . H202 H 0.0499 -0.1129 0.7005 0.0381 1.0000 Uiso R . . . . . H221 H -0.1377 -0.1385 0.6872 0.0288 1.0000 Uiso R . . . . . H231 H -0.3184 -0.1322 0.7068 0.0280 1.0000 Uiso R . . . . . H241 H -0.4144 0.0170 0.7021 0.0277 1.0000 Uiso R . . . . . H251 H -0.3289 0.1573 0.6704 0.0269 1.0000 Uiso R . . . . . H281 H -0.0606 0.1476 0.7592 0.0379 1.0000 Uiso R . . . . . H291 H 0.0467 0.2097 0.8408 0.0500 1.0000 Uiso R . . . . . H301 H 0.1551 0.3521 0.8326 0.0649 1.0000 Uiso R . . . . . H311 H 0.1330 0.4389 0.7447 0.0451 1.0000 Uiso R . . . . . H321 H 0.0163 0.3778 0.6630 0.0338 1.0000 Uiso R . . . . . H341 H -0.2160 0.3839 0.6900 0.0323 1.0000 Uiso R . . . . . H351 H -0.3665 0.4873 0.6605 0.0440 1.0000 Uiso R . . . . . H361 H -0.4818 0.4592 0.5716 0.0429 1.0000 Uiso R . . . . . H371 H -0.4484 0.3291 0.5130 0.0434 1.0000 Uiso R . . . . . H381 H -0.2918 0.2285 0.5378 0.0342 1.0000 Uiso R . . . . . H1021 H 0.5674 0.3423 1.0572 0.0479 1.0000 Uiso R . . . . . H1031 H 0.6294 0.3733 1.1563 0.0648 1.0000 Uiso R . . . . . H1041 H 0.4983 0.3912 1.2205 0.0525 1.0000 Uiso R . . . . . H1061 H 0.2509 0.3491 1.0870 0.0478 1.0000 Uiso R . . . . . H1081 H 0.2870 0.1644 1.0680 0.0370 1.0000 Uiso R . . . . . H1091 H 0.2186 0.0032 1.0575 0.0454 1.0000 Uiso R . . . . . H1101 H 0.1869 -0.0717 0.9661 0.0387 1.0000 Uiso R . . . . . H1111 H 0.2116 0.0207 0.8824 0.0443 1.0000 Uiso R . . . . . H1121 H 0.2839 0.1795 0.8951 0.0378 1.0000 Uiso R . . . . . H1141 H 0.1374 0.3048 0.9970 0.0471 1.0000 Uiso R . . . . . H1151 H -0.0259 0.3944 0.9697 0.0440 1.0000 Uiso R . . . . . H1161 H -0.0108 0.5494 0.9193 0.0351 1.0000 Uiso R . . . . . H1171 H 0.1504 0.5904 0.8881 0.0400 1.0000 Uiso R . . . . . H1191 H 0.2887 0.5813 0.8272 0.0518 1.0000 Uiso R . . . . . H1192 H 0.3142 0.6521 0.8827 0.0520 1.0000 Uiso R . . . . . H1201 H 0.4493 0.6421 0.8108 0.0564 1.0000 Uiso R . . . . . H1202 H 0.4945 0.6554 0.8794 0.0561 1.0000 Uiso R . . . . . H1221 H 0.6315 0.6475 0.8164 0.0307 1.0000 Uiso R . . . . . H1231 H 0.8067 0.6397 0.7931 0.0400 1.0000 Uiso R . . . . . H1241 H 0.9046 0.4923 0.7986 0.0349 1.0000 Uiso R . . . . . H1251 H 0.8226 0.3473 0.8244 0.0318 1.0000 Uiso R . . . . . H1281 H 0.7135 0.1235 0.8082 0.0305 1.0000 Uiso R . . . . . H1291 H 0.8660 0.0214 0.8396 0.0432 1.0000 Uiso R . . . . . H1301 H 0.9762 0.0512 0.9293 0.0502 1.0000 Uiso R . . . . . H1311 H 0.9359 0.1825 0.9887 0.0404 1.0000 Uiso R . . . . . H1321 H 0.7872 0.2822 0.9548 0.0343 1.0000 Uiso R . . . . . H1341 H 0.5613 0.3481 0.7363 0.0380 1.0000 Uiso R . . . . . H1351 H 0.4336 0.2907 0.6586 0.0512 1.0000 Uiso R . . . . . H1361 H 0.3306 0.1523 0.6675 0.0518 1.0000 Uiso R . . . . . H1371 H 0.3493 0.0684 0.7570 0.0552 1.0000 Uiso R . . . . . H1381 H 0.4763 0.1221 0.8366 0.0427 1.0000 Uiso R . . . . . H1051 H 0.3135 0.3950 1.1821 0.0671 1.0000 Uiso 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 0.01934(11) 0.01398(15) 0.01886(12) 0.00289(12) 0.00655(9) 0.00211(12) Pt11 0.02796(14) 0.01483(17) 0.02653(15) 0.00233(13) 0.01193(12) 0.00150(12) Cl1 0.0336(9) 0.0206(8) 0.0506(11) 0.0154(8) 0.0202(8) 0.0091(7) Cl11 0.0487(12) 0.0473(15) 0.0704(15) 0.0432(13) 0.0322(11) 0.0239(10) P1 0.0209(7) 0.0181(11) 0.0186(8) 0.0030(12) 0.0069(6) 0.0022(11) P2 0.0203(9) 0.0122(12) 0.0203(10) -0.0006(9) 0.0042(9) 0.0007(9) P3 0.019(3) 0.012(3) 0.019(3) -0.001(3) 0.005(3) 0.002(3) P4 0.0189(7) 0.0167(14) 0.0191(8) -0.0011(10) 0.0049(6) 0.0024(9) P5 0.0624(14) 0.0294(16) 0.0507(14) -0.0030(17) -0.0065(12) 0.0013(17) P101 0.0256(8) 0.0177(11) 0.0211(8) -0.0009(12) 0.0097(7) -0.0006(11) P102 0.0205(15) 0.0121(13) 0.0171(14) 0.0012(10) 0.0032(11) 0.0004(11) P103 0.030(2) 0.017(3) 0.020(2) 0.002(2) 0.0113(19) 0.0004(19) P104 0.0244(8) 0.0151(14) 0.0222(9) 0.0029(10) 0.0083(7) 0.0016(9) P105 0.0661(14) 0.0221(14) 0.0525(14) -0.0083(17) -0.0101(12) 0.0046(17) F1 0.109(5) 0.046(5) 0.113(6) 0.014(5) -0.072(5) -0.004(5) F6 0.063(4) 0.055(6) 0.107(5) -0.019(5) -0.027(3) 0.019(4) F101 0.119(5) 0.051(5) 0.110(6) 0.032(6) -0.072(5) -0.021(6) F106 0.051(3) 0.039(5) 0.119(5) -0.015(4) -0.007(3) 0.012(3) N1 0.027(3) 0.015(4) 0.021(3) 0.006(3) 0.007(2) -0.001(3) N2 0.033(3) 0.011(3) 0.025(3) 0.005(3) 0.010(3) 0.003(3) N101 0.024(3) 0.017(4) 0.036(4) -0.001(3) 0.006(3) 0.007(3) N102 0.025(3) 0.019(4) 0.032(4) 0.005(3) 0.008(3) 0.001(3) C1 0.023(3) 0.029(6) 0.021(3) -0.008(4) 0.006(3) -0.001(4) C2 0.027(4) 0.022(4) 0.024(4) 0.012(3) 0.010(3) -0.003(3) C3 0.021(3) 0.030(5) 0.032(4) 0.008(4) 0.000(3) 0.002(3) C4 0.018(3) 0.026(5) 0.061(6) 0.004(5) -0.002(4) 0.003(3) C5 0.032(4) 0.027(6) 0.039(5) -0.010(4) 0.005(4) -0.007(4) C6 0.029(4) 0.028(5) 0.034(5) -0.005(4) 0.019(3) -0.008(3) C7 0.036(4) 0.015(4) 0.012(3) -0.004(3) 0.010(3) 0.002(3) C8 0.029(4) 0.022(4) 0.028(4) 0.000(4) 0.001(3) -0.009(3) C9 0.052(5) 0.021(5) 0.039(5) -0.005(4) 0.003(4) -0.008(4) C10 0.082(8) 0.029(7) 0.021(4) -0.003(4) -0.009(5) 0.008(5) C11 0.069(7) 0.039(7) 0.018(4) 0.003(4) 0.024(4) 0.014(5) C12 0.042(4) 0.044(6) 0.023(4) -0.002(4) 0.009(4) 0.013(4) C13 0.016(3) 0.019(5) 0.016(3) 0.004(3) 0.007(3) 0.001(3) C14 0.033(4) 0.014(4) 0.034(4) 0.001(4) 0.017(3) 0.006(3) C15 0.015(3) 0.024(5) 0.042(4) -0.005(4) 0.011(3) 0.005(3) C16 0.026(4) 0.030(5) 0.037(5) -0.008(4) 0.003(3) 0.008(4) C17 0.022(3) 0.018(4) 0.029(4) 0.005(3) 0.007(3) -0.003(3) C18 0.018(3) 0.016(4) 0.022(4) -0.010(3) 0.008(3) 0.002(3) C19 0.053(5) 0.019(5) 0.056(6) 0.020(4) 0.010(5) -0.002(4) C20 0.040(4) 0.012(3) 0.048(4) 0.016(3) 0.025(3) 0.012(3) C21 0.022(3) 0.032(5) 0.022(4) -0.004(4) 0.006(3) 0.008(3) C22 0.036(4) 0.014(4) 0.021(4) -0.001(3) 0.001(3) 0.005(3) C23 0.029(4) 0.016(4) 0.027(4) 0.002(3) 0.011(3) -0.014(3) C24 0.024(3) 0.027(5) 0.021(4) 0.007(3) 0.010(3) -0.002(3) C25 0.026(4) 0.018(5) 0.023(4) 0.001(4) 0.002(3) 0.005(3) C26 0.020(3) 0.009(4) 0.022(4) 0.002(3) 0.005(3) 0.003(3) C27 0.019(3) 0.014(4) 0.024(4) -0.005(3) 0.005(3) 0.002(3) C28 0.039(4) 0.025(5) 0.031(4) 0.004(5) 0.006(3) 0.003(5) C29 0.059(5) 0.041(6) 0.025(4) 0.000(4) 0.007(4) 0.000(4) C30 0.078(7) 0.038(8) 0.036(5) -0.019(5) -0.015(5) 0.000(5) C31 0.034(4) 0.023(5) 0.053(6) -0.006(4) 0.001(4) -0.006(3) C32 0.033(4) 0.034(6) 0.019(3) 0.000(3) 0.004(3) 0.001(3) C33 0.019(3) 0.014(5) 0.025(3) 0.000(4) 0.009(3) 0.004(3) C34 0.029(4) 0.023(5) 0.031(4) 0.004(4) 0.013(4) 0.002(4) C35 0.032(4) 0.016(5) 0.066(7) 0.012(5) 0.015(4) 0.009(4) C36 0.029(4) 0.022(5) 0.059(6) 0.014(5) 0.020(4) 0.006(4) C37 0.024(4) 0.028(5) 0.056(5) 0.015(4) -0.005(4) -0.001(3) C38 0.024(3) 0.028(6) 0.032(4) 0.008(4) 0.003(3) -0.001(3) C101 0.036(4) 0.019(5) 0.036(4) 0.007(4) 0.009(4) -0.002(3) C102 0.050(5) 0.035(6) 0.035(5) -0.007(5) 0.006(4) -0.007(4) C103 0.069(7) 0.049(7) 0.037(6) 0.002(5) -0.019(6) -0.028(6) C104 0.084(8) 0.019(6) 0.031(5) -0.010(4) 0.019(5) 0.006(5) C105 0.075(8) 0.055(9) 0.036(6) -0.017(5) 0.001(5) 0.035(6) C106 0.058(5) 0.033(5) 0.033(4) 0.001(4) 0.017(4) 0.014(4) C107 0.020(3) 0.011(5) 0.027(3) 0.008(3) 0.010(3) 0.002(3) C108 0.021(4) 0.032(5) 0.037(5) -0.004(4) -0.001(3) 0.005(3) C109 0.041(4) 0.030(5) 0.038(5) 0.019(4) -0.001(4) -0.016(4) C110 0.031(4) 0.018(5) 0.047(5) 0.005(4) 0.003(4) -0.005(3) C111 0.034(4) 0.033(6) 0.048(6) -0.010(5) 0.019(4) -0.001(4) C112 0.041(5) 0.030(5) 0.026(4) -0.002(4) 0.012(4) -0.004(4) C113 0.028(4) 0.023(5) 0.028(4) -0.009(4) 0.003(3) 0.008(3) C114 0.038(5) 0.040(6) 0.039(5) 0.005(5) 0.005(4) -0.001(5) C115 0.038(4) 0.033(6) 0.040(5) 0.003(4) 0.008(4) -0.007(4) C116 0.026(4) 0.025(5) 0.038(5) -0.006(4) 0.008(3) 0.005(3) C117 0.038(4) 0.029(6) 0.034(5) -0.005(4) 0.004(4) 0.016(4) C118 0.038(4) 0.015(5) 0.023(4) 0.001(3) 0.002(3) 0.001(4) C119 0.021(4) 0.040(6) 0.073(7) 0.024(5) 0.023(4) 0.015(4) C120 0.037(4) 0.023(5) 0.084(7) 0.016(5) 0.025(5) 0.012(4) C121 0.030(4) 0.012(4) 0.015(3) 0.005(3) 0.002(3) -0.005(3) C122 0.032(4) 0.024(5) 0.024(4) 0.004(4) 0.011(3) -0.007(4) C123 0.043(5) 0.036(6) 0.023(4) 0.002(4) 0.009(4) -0.004(4) C124 0.029(4) 0.034(6) 0.028(4) -0.006(4) 0.011(3) -0.008(4) C125 0.029(4) 0.030(5) 0.024(4) -0.001(4) 0.010(3) -0.006(4) C126 0.030(4) 0.025(5) 0.014(3) 0.002(3) 0.008(3) -0.007(3) C127 0.030(4) 0.026(6) 0.029(4) 0.010(4) 0.011(3) -0.005(4) C128 0.028(4) 0.019(5) 0.031(5) 0.004(4) 0.008(4) 0.007(3) C129 0.044(5) 0.029(6) 0.036(5) 0.003(4) 0.017(4) 0.012(4) C130 0.023(4) 0.040(7) 0.061(6) 0.023(6) 0.002(4) 0.004(4) C131 0.026(3) 0.046(7) 0.032(4) 0.011(4) 0.008(3) -0.002(3) C132 0.032(4) 0.024(5) 0.031(4) -0.008(3) 0.004(3) -0.004(3) C133 0.031(4) 0.026(5) 0.028(4) -0.005(4) 0.004(4) 0.004(3) C134 0.037(4) 0.031(6) 0.027(4) -0.001(4) 0.002(3) -0.001(4) C135 0.042(5) 0.049(7) 0.031(4) 0.005(4) -0.008(4) 0.003(4) C136 0.049(5) 0.034(7) 0.043(5) -0.008(4) -0.011(4) -0.002(4) C137 0.057(6) 0.035(7) 0.041(5) -0.007(4) -0.014(5) -0.010(4) C138 0.045(5) 0.013(4) 0.046(5) -0.004(4) 0.000(4) -0.008(4) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.074091(6) loop_ _oxford_twin_element_scale_factors 0.500(7) 0.500(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pt1 . Cl1 . 2.354(2) yes Pt1 . P1 . 2.2906(19) yes Pt1 . P2 . 2.162(2) yes Pt1 . P3 . 2.18(3) yes Pt1 . P4 . 2.298(2) yes Pt11 . Cl11 . 2.310(2) yes Pt11 . P101 . 2.308(2) yes Pt11 . P102 . 2.212(4) yes Pt11 . P103 . 2.142(5) yes Pt11 . P104 . 2.300(2) yes P1 . C1 . 1.819(11) yes P1 . C7 . 1.812(7) yes P1 . C13 . 1.794(8) yes P2 . N1 . 1.644(7) yes P2 . N2 . 1.672(8) yes P3 . N1 . 1.67(4) yes P3 . N2 . 1.62(4) yes P4 . C26 . 1.813(9) yes P4 . C27 . 1.802(7) yes P4 . C33 . 1.803(8) yes P5 . F1 . 1.582(6) yes P5 . F6 . 1.607(6) yes P5 . F21 . 1.491(16) yes P5 . F22 . 1.53(2) yes P5 . F23 . 1.623(12) yes P5 . F24 . 1.61(3) yes P5 . F1 . 1.582(6) yes P5 . F2 . 1.637(9) yes P5 . F3 . 1.505(11) yes P5 . F4 . 1.703(12) yes P5 . F5 . 1.553(12) yes P5 . F6 . 1.607(6) yes P101 . C101 . 1.808(9) yes P101 . C107 . 1.815(10) yes P101 . C113 . 1.838(9) yes P102 . N101 . 1.640(8) yes P102 . N102 . 1.674(9) yes P103 . N101 . 1.688(8) yes P103 . N102 . 1.701(9) yes P104 . C126 . 1.816(10) yes P104 . C127 . 1.797(10) yes P104 . C133 . 1.821(8) yes P105 . F101 . 1.569(6) yes P105 . F102 . 1.535(12) yes P105 . F103 . 1.628(12) yes P105 . F104 . 1.543(9) yes P105 . F105 . 1.745(12) yes P105 . F106 . 1.595(6) yes P105 . F101 . 1.569(6) yes P105 . F106 . 1.595(6) yes P105 . F121 . 1.60(2) yes P105 . F122 . 1.639(14) yes P105 . F123 . 1.611(15) yes P105 . F124 . 1.516(12) yes N1 . C18 . 1.419(11) yes N1 . C19 . 1.489(11) yes N2 . C20 . 1.460(11) yes N2 . C21 . 1.420(11) yes N101 . C118 . 1.409(12) yes N101 . C119 . 1.482(13) yes N102 . C120 . 1.521(13) yes N102 . C121 . 1.409(11) yes C1 . C2 . 1.383(12) yes C1 . C6 . 1.443(13) yes C2 . C3 . 1.393(13) yes C2 . H21 . 0.937 no C3 . C4 . 1.370(14) yes C3 . H31 . 0.937 no C4 . C5 . 1.411(15) yes C4 . H41 . 0.936 no C5 . C6 . 1.382(14) yes C5 . H51 . 0.943 no C6 . H61 . 0.929 no C7 . C8 . 1.375(10) yes C7 . C12 . 1.410(12) yes C8 . C9 . 1.389(12) yes C8 . H81 . 0.924 no C9 . C10 . 1.395(16) yes C9 . H91 . 0.937 no C10 . C11 . 1.377(15) yes C10 . H101 . 0.923 no C11 . C12 . 1.391(13) yes C11 . H111 . 0.928 no C12 . H121 . 0.924 no C13 . C14 . 1.422(11) yes C13 . C18 . 1.410(12) yes C14 . C15 . 1.375(11) yes C14 . H141 . 0.933 no C15 . C16 . 1.304(14) yes C15 . H151 . 0.920 no C16 . C17 . 1.402(12) yes C16 . H161 . 0.927 no C17 . C18 . 1.404(11) yes C17 . H171 . 0.921 no C19 . C20 . 1.573(13) yes C19 . H191 . 0.969 no C19 . H192 . 0.970 no C20 . H201 . 0.964 no C20 . H202 . 0.967 no C21 . C22 . 1.414(14) yes C21 . C26 . 1.402(13) yes C22 . C23 . 1.377(12) yes C22 . H221 . 0.929 no C23 . C24 . 1.376(14) yes C23 . H231 . 0.933 no C24 . C25 . 1.388(13) yes C24 . H241 . 0.938 no C25 . C26 . 1.381(10) yes C25 . H251 . 0.931 no C27 . C28 . 1.404(12) yes C27 . C32 . 1.367(13) yes C28 . C29 . 1.367(12) yes C28 . H281 . 0.928 no C29 . C30 . 1.402(16) yes C29 . H291 . 0.910 no C30 . C31 . 1.370(15) yes C30 . H301 . 0.941 no C31 . C32 . 1.393(12) yes C31 . H311 . 0.931 no C32 . H321 . 0.928 no C33 . C34 . 1.410(13) yes C33 . C38 . 1.400(10) yes C34 . C35 . 1.381(12) yes C34 . H341 . 0.923 no C35 . C36 . 1.380(13) yes C35 . H351 . 0.930 no C36 . C37 . 1.373(14) yes C36 . H361 . 0.930 no C37 . C38 . 1.404(11) yes C37 . H371 . 0.926 no C38 . H381 . 0.920 no C101 . C102 . 1.394(12) yes C101 . C106 . 1.358(14) yes C102 . C103 . 1.386(14) yes C102 . H1021 . 0.937 no C103 . C104 . 1.384(17) yes C103 . H1031 . 0.938 no C104 . C105 . 1.355(16) yes C104 . H1041 . 0.925 no C105 . C106 . 1.352(14) yes C105 . H1051 . 0.933 no C106 . H1061 . 0.933 no C107 . C108 . 1.384(13) yes C107 . C112 . 1.338(12) yes C108 . C109 . 1.393(14) yes C108 . H1081 . 0.938 no C109 . C110 . 1.352(14) yes C109 . H1091 . 0.940 no C110 . C111 . 1.393(14) yes C110 . H1101 . 0.933 no C111 . C112 . 1.377(15) yes C111 . H1111 . 0.938 no C112 . H1121 . 0.931 no C113 . C114 . 1.370(13) yes C113 . C118 . 1.413(14) yes C114 . C115 . 1.388(14) yes C114 . H1141 . 0.933 no C115 . C116 . 1.444(14) yes C115 . H1151 . 0.933 no C116 . C117 . 1.345(13) yes C116 . H1161 . 0.933 no C117 . C118 . 1.410(12) yes C117 . H1171 . 0.919 no C119 . C120 . 1.469(12) yes C119 . H1191 . 0.964 no C119 . H1192 . 0.968 no C120 . H1201 . 0.968 no C120 . H1202 . 0.968 no C121 . C122 . 1.405(12) yes C121 . C126 . 1.399(13) yes C122 . C123 . 1.360(12) yes C122 . H1221 . 0.925 no C123 . C124 . 1.376(15) yes C123 . H1231 . 0.931 no C124 . C125 . 1.388(14) yes C124 . H1241 . 0.929 no C125 . C126 . 1.427(11) yes C125 . H1251 . 0.933 no C127 . C128 . 1.379(15) yes C127 . C132 . 1.376(10) yes C128 . C129 . 1.393(12) yes C128 . H1281 . 0.917 no C129 . C130 . 1.386(13) yes C129 . H1291 . 0.931 no C130 . C131 . 1.390(15) yes C130 . H1301 . 0.925 no C131 . C132 . 1.353(12) yes C131 . H1311 . 0.930 no C132 . H1321 . 0.925 no C133 . C134 . 1.381(13) yes C133 . C138 . 1.417(13) yes C134 . C135 . 1.402(12) yes C134 . H1341 . 0.918 no C135 . C136 . 1.344(15) yes C135 . H1351 . 0.921 no C136 . C137 . 1.400(15) yes C136 . H1361 . 0.931 no C137 . C138 . 1.373(12) yes C137 . H1371 . 0.931 no C138 . H1381 . 0.927 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 . Pt1 . P1 . 91.21(10) yes Cl1 . Pt1 . P2 . 170.83(8) yes P1 . Pt1 . P2 . 88.55(11) yes Cl1 . Pt1 . P3 . 160.6(9) yes P1 . Pt1 . P3 . 92.3(9) yes Cl1 . Pt1 . P4 . 91.04(10) yes P1 . Pt1 . P4 . 168.22(6) yes P2 . Pt1 . P4 . 91.06(10) yes P3 . Pt1 . P4 . 81.8(9) yes Cl11 . Pt11 . P101 . 89.42(10) yes Cl11 . Pt11 . P102 . 170.16(13) yes P101 . Pt11 . P102 . 91.11(12) yes Cl11 . Pt11 . P103 . 159.63(15) yes P101 . Pt11 . P103 . 88.84(16) yes P102 . Pt11 . P103 . 30.21(15) yes Cl11 . Pt11 . P104 . 93.21(10) yes P101 . Pt11 . P104 . 169.72(7) yes P102 . Pt11 . P104 . 84.61(12) yes P103 . Pt11 . P104 . 92.09(15) yes Pt1 . P1 . C1 . 108.4(3) yes Pt1 . P1 . C7 . 113.0(3) yes C1 . P1 . C7 . 108.4(4) yes Pt1 . P1 . C13 . 115.9(3) yes C1 . P1 . C13 . 102.3(4) yes C7 . P1 . C13 . 108.2(4) yes Pt1 . P2 . N1 . 120.4(3) yes Pt1 . P2 . N2 . 118.5(3) yes N1 . P2 . N2 . 95.5(3) yes Pt1 . P3 . N1 . 118.2(17) yes Pt1 . P3 . N2 . 120.3(15) yes N1 . P3 . N2 . 96.3(20) yes Pt1 . P4 . C26 . 116.9(3) yes Pt1 . P4 . C27 . 105.3(3) yes C26 . P4 . C27 . 106.1(4) yes Pt1 . P4 . C33 . 114.1(3) yes C26 . P4 . C33 . 105.4(4) yes C27 . P4 . C33 . 108.7(4) yes F1 . P5 . F6 . 179.1(6) yes F1 . P5 . F21 . 89.5(7) yes F6 . P5 . F21 . 89.7(7) yes F1 . P5 . F22 . 92.5(8) yes F6 . P5 . F22 . 88.2(8) yes F21 . P5 . F22 . 95.7(12) yes F1 . P5 . F23 . 87.3(5) yes F6 . P5 . F23 . 93.4(5) yes F21 . P5 . F23 . 173.9(9) yes F22 . P5 . F23 . 89.7(11) yes F1 . P5 . F24 . 81.4(9) yes F6 . P5 . F24 . 98.0(9) yes F21 . P5 . F24 . 91.1(13) yes F22 . P5 . F24 . 170.9(14) yes F23 . P5 . F24 . 83.3(12) yes F1 . P5 . F2 . 90.8(5) yes F1 . P5 . F3 . 93.9(5) yes F2 . P5 . F3 . 91.4(6) yes F1 . P5 . F4 . 100.7(5) yes F2 . P5 . F4 . 168.1(5) yes F3 . P5 . F4 . 90.8(6) yes F1 . P5 . F5 . 89.0(6) yes F2 . P5 . F5 . 88.1(6) yes F3 . P5 . F5 . 177.0(5) yes F4 . P5 . F5 . 89.0(7) yes F1 . P5 . F6 . 179.1(6) yes F2 . P5 . F6 . 89.1(4) yes F3 . P5 . F6 . 87.0(5) yes F4 . P5 . F6 . 79.4(5) yes F5 . P5 . F6 . 90.0(5) yes Pt11 . P101 . C101 . 113.9(3) yes Pt11 . P101 . C107 . 106.3(3) yes C101 . P101 . C107 . 110.6(4) yes Pt11 . P101 . C113 . 115.6(3) yes C101 . P101 . C113 . 105.8(4) yes C107 . P101 . C113 . 104.2(4) yes Pt11 . P102 . N101 . 117.9(3) yes Pt11 . P102 . N102 . 117.0(3) yes N101 . P102 . N102 . 96.5(4) yes Pt11 . P103 . N101 . 119.3(4) yes Pt11 . P103 . N102 . 119.3(4) yes N101 . P103 . N102 . 93.7(4) yes Pt11 . P104 . C126 . 115.1(3) yes Pt11 . P104 . C127 . 114.7(3) yes C126 . P104 . C127 . 106.8(4) yes Pt11 . P104 . C133 . 103.8(3) yes C126 . P104 . C133 . 106.9(4) yes C127 . P104 . C133 . 109.2(5) yes F101 . P105 . F102 . 90.3(6) yes F101 . P105 . F103 . 100.1(5) yes F102 . P105 . F103 . 96.7(7) yes F101 . P105 . F104 . 91.1(6) yes F102 . P105 . F104 . 175.0(7) yes F103 . P105 . F104 . 87.8(6) yes F101 . P105 . F105 . 88.3(5) yes F102 . P105 . F105 . 85.0(6) yes F103 . P105 . F105 . 171.4(5) yes F104 . P105 . F105 . 90.3(6) yes F101 . P105 . F106 . 178.8(6) yes F102 . P105 . F106 . 88.9(5) yes F103 . P105 . F106 . 80.9(5) yes F104 . P105 . F106 . 89.6(4) yes F105 . P105 . F106 . 90.7(5) yes F101 . P105 . F106 . 178.8(6) yes F101 . P105 . F121 . 82.9(8) yes F106 . P105 . F121 . 97.2(8) yes F101 . P105 . F122 . 85.5(6) yes F106 . P105 . F122 . 95.7(5) yes F121 . P105 . F122 . 87.0(10) yes F101 . P105 . F123 . 89.9(6) yes F106 . P105 . F123 . 90.1(6) yes F121 . P105 . F123 . 168.9(10) yes F122 . P105 . F123 . 84.0(8) yes F101 . P105 . F124 . 86.2(5) yes F106 . P105 . F124 . 92.7(5) yes F121 . P105 . F124 . 93.9(9) yes F122 . P105 . F124 . 171.4(6) yes F123 . P105 . F124 . 94.0(8) yes P3 . N1 . C18 . 122.6(13) yes P2 . N1 . C18 . 130.1(6) yes P3 . N1 . C19 . 104.4(13) yes P2 . N1 . C19 . 111.9(6) yes C18 . N1 . C19 . 118.1(7) yes P2 . N2 . C20 . 106.1(6) yes P3 . N2 . C20 . 111.5(13) yes P2 . N2 . C21 . 122.3(6) yes P3 . N2 . C21 . 131.0(13) yes C20 . N2 . C21 . 117.5(8) yes P103 . N101 . C118 . 131.6(6) yes P102 . N101 . C118 . 120.6(7) yes P103 . N101 . C119 . 109.2(6) yes P102 . N101 . C119 . 103.6(6) yes C118 . N101 . C119 . 119.2(6) yes P103 . N102 . C120 . 101.7(7) yes P102 . N102 . C120 . 108.2(6) yes P103 . N102 . C121 . 121.5(6) yes P102 . N102 . C121 . 131.0(6) yes C120 . N102 . C121 . 120.8(8) yes P1 . C1 . C2 . 123.9(7) yes P1 . C1 . C6 . 115.8(7) yes C2 . C1 . C6 . 120.2(10) yes C1 . C2 . C3 . 119.3(9) yes C1 . C2 . H21 . 119.7 no C3 . C2 . H21 . 120.9 no C2 . C3 . C4 . 120.9(9) yes C2 . C3 . H31 . 118.9 no C4 . C3 . H31 . 120.2 no C3 . C4 . C5 . 121.2(10) yes C3 . C4 . H41 . 120.0 no C5 . C4 . H41 . 118.9 no C4 . C5 . C6 . 119.1(9) yes C4 . C5 . H51 . 120.9 no C6 . C5 . H51 . 120.0 no C1 . C6 . C5 . 119.3(10) yes C1 . C6 . H61 . 120.3 no C5 . C6 . H61 . 120.4 no P1 . C7 . C8 . 118.5(6) yes P1 . C7 . C12 . 121.6(6) yes C8 . C7 . C12 . 119.9(7) yes C7 . C8 . C9 . 119.9(9) yes C7 . C8 . H81 . 121.1 no C9 . C8 . H81 . 118.9 no C8 . C9 . C10 . 120.1(9) yes C8 . C9 . H91 . 120.0 no C10 . C9 . H91 . 119.9 no C9 . C10 . C11 . 120.4(9) yes C9 . C10 . H101 . 119.9 no C11 . C10 . H101 . 119.7 no C10 . C11 . C12 . 119.5(10) yes C10 . C11 . H111 . 120.4 no C12 . C11 . H111 . 120.1 no C7 . C12 . C11 . 119.9(9) yes C7 . C12 . H121 . 119.8 no C11 . C12 . H121 . 120.2 no P1 . C13 . C14 . 117.3(6) yes P1 . C13 . C18 . 125.7(6) yes C14 . C13 . C18 . 116.9(7) yes C13 . C14 . C15 . 121.6(8) yes C13 . C14 . H141 . 119.7 no C15 . C14 . H141 . 118.8 no C14 . C15 . C16 . 121.0(8) yes C14 . C15 . H151 . 118.9 no C16 . C15 . H151 . 120.1 no C15 . C16 . C17 . 121.1(8) yes C15 . C16 . H161 . 120.0 no C17 . C16 . H161 . 118.9 no C16 . C17 . C18 . 120.1(8) yes C16 . C17 . H171 . 120.2 no C18 . C17 . H171 . 119.7 no N1 . C18 . C13 . 124.1(7) yes N1 . C18 . C17 . 116.4(8) yes C13 . C18 . C17 . 119.2(7) yes N1 . C19 . C20 . 104.9(7) yes N1 . C19 . H191 . 109.9 no C20 . C19 . H191 . 111.3 no N1 . C19 . H192 . 109.3 no C20 . C19 . H192 . 111.8 no H191 . C19 . H192 . 109.6 no C19 . C20 . N2 . 106.6(7) yes C19 . C20 . H201 . 111.6 no N2 . C20 . H201 . 111.4 no C19 . C20 . H202 . 107.9 no N2 . C20 . H202 . 108.8 no H201 . C20 . H202 . 110.5 no N2 . C21 . C22 . 119.6(8) yes N2 . C21 . C26 . 122.1(9) yes C22 . C21 . C26 . 118.1(8) yes C21 . C22 . C23 . 120.9(9) yes C21 . C22 . H221 . 119.0 no C23 . C22 . H221 . 120.1 no C22 . C23 . C24 . 121.0(8) yes C22 . C23 . H231 . 119.5 no C24 . C23 . H231 . 119.5 no C23 . C24 . C25 . 118.0(8) yes C23 . C24 . H241 . 121.0 no C25 . C24 . H241 . 121.1 no C24 . C25 . C26 . 123.0(9) yes C24 . C25 . H251 . 118.9 no C26 . C25 . H251 . 118.1 no P4 . C26 . C21 . 122.5(6) yes P4 . C26 . C25 . 118.6(7) yes C21 . C26 . C25 . 118.8(8) yes P4 . C27 . C28 . 121.6(7) yes P4 . C27 . C32 . 119.8(7) yes C28 . C27 . C32 . 118.5(8) yes C27 . C28 . C29 . 122.0(11) yes C27 . C28 . H281 . 119.6 no C29 . C28 . H281 . 118.4 no C28 . C29 . C30 . 117.9(10) yes C28 . C29 . H291 . 120.0 no C30 . C29 . H291 . 122.0 no C29 . C30 . C31 . 121.2(8) yes C29 . C30 . H301 . 119.4 no C31 . C30 . H301 . 119.3 no C30 . C31 . C32 . 119.4(9) yes C30 . C31 . H311 . 120.6 no C32 . C31 . H311 . 120.0 no C31 . C32 . C27 . 120.9(9) yes C31 . C32 . H321 . 119.5 no C27 . C32 . H321 . 119.6 no P4 . C33 . C34 . 121.8(5) yes P4 . C33 . C38 . 117.3(7) yes C34 . C33 . C38 . 120.8(8) yes C33 . C34 . C35 . 119.2(8) yes C33 . C34 . H341 . 120.2 no C35 . C34 . H341 . 120.6 no C34 . C35 . C36 . 120.6(10) yes C34 . C35 . H351 . 119.8 no C36 . C35 . H351 . 119.6 no C35 . C36 . C37 . 120.3(8) yes C35 . C36 . H361 . 120.8 no C37 . C36 . H361 . 118.9 no C36 . C37 . C38 . 121.4(8) yes C36 . C37 . H371 . 119.5 no C38 . C37 . H371 . 119.1 no C37 . C38 . C33 . 117.6(9) yes C37 . C38 . H381 . 121.1 no C33 . C38 . H381 . 121.2 no P101 . C101 . C102 . 119.0(8) yes P101 . C101 . C106 . 121.8(7) yes C102 . C101 . C106 . 119.0(9) yes C101 . C102 . C103 . 120.7(11) yes C101 . C102 . H1021 . 120.2 no C103 . C102 . H1021 . 119.0 no C102 . C103 . C104 . 119.0(10) yes C102 . C103 . H1031 . 120.3 no C104 . C103 . H1031 . 120.7 no C103 . C104 . C105 . 118.0(9) yes C103 . C104 . H1041 . 120.6 no C105 . C104 . H1041 . 121.3 no C104 . C105 . C106 . 123.7(12) yes C104 . C105 . H1051 . 118.0 no C106 . C105 . H1051 . 118.2 no C101 . C106 . C105 . 119.1(11) yes C101 . C106 . H1061 . 119.7 no C105 . C106 . H1061 . 121.1 no P101 . C107 . C108 . 122.2(7) yes P101 . C107 . C112 . 118.8(7) yes C108 . C107 . C112 . 119.0(9) yes C107 . C108 . C109 . 118.9(9) yes C107 . C108 . H1081 . 120.7 no C109 . C108 . H1081 . 120.5 no C108 . C109 . C110 . 121.8(9) yes C108 . C109 . H1091 . 119.0 no C110 . C109 . H1091 . 119.2 no C109 . C110 . C111 . 118.6(9) yes C109 . C110 . H1101 . 121.7 no C111 . C110 . H1101 . 119.8 no C110 . C111 . C112 . 119.0(10) yes C110 . C111 . H1111 . 121.0 no C112 . C111 . H1111 . 120.0 no C111 . C112 . C107 . 122.6(10) yes C111 . C112 . H1121 . 120.2 no C107 . C112 . H1121 . 117.2 no P101 . C113 . C114 . 114.3(8) yes P101 . C113 . C118 . 124.9(7) yes C114 . C113 . C118 . 120.8(8) yes C113 . C114 . C115 . 122.7(10) yes C113 . C114 . H1141 . 118.7 no C115 . C114 . H1141 . 118.5 no C114 . C115 . C116 . 116.2(9) yes C114 . C115 . H1151 . 121.5 no C116 . C115 . H1151 . 122.3 no C115 . C116 . C117 . 120.7(9) yes C115 . C116 . H1161 . 119.8 no C117 . C116 . H1161 . 119.5 no C116 . C117 . C118 . 122.7(10) yes C116 . C117 . H1171 . 118.8 no C118 . C117 . H1171 . 118.5 no C113 . C118 . C117 . 116.5(9) yes C113 . C118 . N101 . 124.0(8) yes C117 . C118 . N101 . 119.5(8) yes N101 . C119 . C120 . 108.0(7) yes N101 . C119 . H1191 . 109.3 no C120 . C119 . H1191 . 110.8 no N101 . C119 . H1192 . 109.3 no C120 . C119 . H1192 . 109.8 no H1191 . C119 . H1192 . 109.7 no N102 . C120 . C119 . 105.8(9) yes N102 . C120 . H1201 . 109.0 no C119 . C120 . H1201 . 110.3 no N102 . C120 . H1202 . 110.3 no C119 . C120 . H1202 . 110.9 no H1201 . C120 . H1202 . 110.4 no N102 . C121 . C122 . 117.4(8) yes N102 . C121 . C126 . 123.3(8) yes C122 . C121 . C126 . 119.2(8) yes C121 . C122 . C123 . 120.0(10) yes C121 . C122 . H1221 . 120.1 no C123 . C122 . H1221 . 119.8 no C122 . C123 . C124 . 122.0(10) yes C122 . C123 . H1231 . 118.8 no C124 . C123 . H1231 . 119.2 no C123 . C124 . C125 . 120.0(9) yes C123 . C124 . H1241 . 120.8 no C125 . C124 . H1241 . 119.1 no C124 . C125 . C126 . 119.0(10) yes C124 . C125 . H1251 . 120.1 no C126 . C125 . H1251 . 120.9 no P104 . C126 . C125 . 115.8(7) yes P104 . C126 . C121 . 124.5(6) yes C125 . C126 . C121 . 119.7(9) yes P104 . C127 . C128 . 122.3(6) yes P104 . C127 . C132 . 118.2(8) yes C128 . C127 . C132 . 119.5(8) yes C127 . C128 . C129 . 118.7(8) yes C127 . C128 . H1281 . 120.6 no C129 . C128 . H1281 . 120.7 no C128 . C129 . C130 . 120.3(10) yes C128 . C129 . H1291 . 120.2 no C130 . C129 . H1291 . 119.5 no C129 . C130 . C131 . 120.5(8) yes C129 . C130 . H1301 . 120.0 no C131 . C130 . H1301 . 119.5 no C130 . C131 . C132 . 117.8(8) yes C130 . C131 . H1311 . 121.1 no C132 . C131 . H1311 . 121.0 no C127 . C132 . C131 . 123.1(9) yes C127 . C132 . H1321 . 117.5 no C131 . C132 . H1321 . 119.4 no P104 . C133 . C134 . 120.7(8) yes P104 . C133 . C138 . 118.4(7) yes C134 . C133 . C138 . 120.8(9) yes C133 . C134 . C135 . 118.4(10) yes C133 . C134 . H1341 . 121.2 no C135 . C134 . H1341 . 120.4 no C134 . C135 . C136 . 121.6(10) yes C134 . C135 . H1351 . 118.5 no C136 . C135 . H1351 . 119.9 no C135 . C136 . C137 . 120.0(9) yes C135 . C136 . H1361 . 120.1 no C137 . C136 . H1361 . 119.9 no C136 . C137 . C138 . 120.8(10) yes C136 . C137 . H1371 . 119.2 no C138 . C137 . H1371 . 119.9 no C133 . C138 . C137 . 118.3(10) yes C133 . C138 . H1381 . 120.8 no C137 . C138 . H1381 . 120.9 no _iucr_refine_instruction_details_constraints ; # # Punched on 16/02/12 at 14:12:10 # #LIST 12 BLOCK CONT SCALE CONT PT ( 1 ,X'S,U'S) UNTIL F ( 1 ) CONT F ( 2 ,X'S,U[ISO]) UNTIL F ( 5 ) CONT F ( 6 ,X'S,U'S) CONT F ( 21 ,X'S,U[ISO]) UNTIL F ( 24 ) CONT F ( 101 ,X'S,U'S) CONT F ( 102 ,X'S,U[ISO]) UNTIL F ( 105 ) CONT F ( 106 ,X'S,U'S) CONT F ( 121 ,X'S,U[ISO]) UNTIL F ( 124 ) CONT N ( 1 ,X'S,U'S) UNTIL C ( 138 ) SUMFIX P(2,OCC) AND P(3,OCC) SUMFIX P(102,OCC) AND P(103,OCC) SUMFIX PART(1001,OCC) AND PART(1002,OCC) SUMFIX PART(1003,OCC) AND PART(1004,OCC) SUMFIX ELEMENT SCALES RIDE C ( 2,X'S) H ( 21,X'S) RIDE C ( 3,X'S) H ( 31,X'S) RIDE C ( 4,X'S) H ( 41,X'S) RIDE C ( 5,X'S) H ( 51,X'S) RIDE C ( 6,X'S) H ( 61,X'S) RIDE C ( 8,X'S) H ( 81,X'S) RIDE C ( 9,X'S) H ( 91,X'S) RIDE C ( 10,X'S) H ( 101,X'S) RIDE C ( 11,X'S) H ( 111,X'S) RIDE C ( 12,X'S) H ( 121,X'S) RIDE C ( 14,X'S) H ( 141,X'S) RIDE C ( 15,X'S) H ( 151,X'S) RIDE C ( 16,X'S) H ( 161,X'S) RIDE C ( 17,X'S) H ( 171,X'S) RIDE C ( 19,X'S) H ( 191,X'S) H ( 192,X'S) RIDE C ( 20,X'S) H ( 201,X'S) H ( 202,X'S) RIDE C ( 22,X'S) H ( 221,X'S) RIDE C ( 23,X'S) H ( 231,X'S) RIDE C ( 24,X'S) H ( 241,X'S) RIDE C ( 25,X'S) H ( 251,X'S) RIDE C ( 28,X'S) H ( 281,X'S) RIDE C ( 29,X'S) H ( 291,X'S) RIDE C ( 30,X'S) H ( 301,X'S) RIDE C ( 31,X'S) H ( 311,X'S) RIDE C ( 32,X'S) H ( 321,X'S) RIDE C ( 34,X'S) H ( 341,X'S) RIDE C ( 35,X'S) H ( 351,X'S) RIDE C ( 36,X'S) H ( 361,X'S) RIDE C ( 37,X'S) H ( 371,X'S) RIDE C ( 38,X'S) H ( 381,X'S) RIDE C ( 102,X'S) H (1021,X'S) RIDE C ( 103,X'S) H (1031,X'S) RIDE C ( 104,X'S) H (1041,X'S) RIDE C ( 105,X'S) H (1051,X'S) RIDE C ( 106,X'S) H (1061,X'S) RIDE C ( 108,X'S) H (1081,X'S) RIDE C ( 109,X'S) H (1091,X'S) RIDE C ( 110,X'S) H (1101,X'S) RIDE C ( 111,X'S) H (1111,X'S) RIDE C ( 112,X'S) H (1121,X'S) RIDE C ( 114,X'S) H (1141,X'S) RIDE C ( 115,X'S) H (1151,X'S) RIDE C ( 116,X'S) H (1161,X'S) RIDE C ( 117,X'S) H (1171,X'S) RIDE C ( 119,X'S) H (1191,X'S) H (1192,X'S) RIDE C ( 120,X'S) H (1201,X'S) H (1202,X'S) RIDE C ( 122,X'S) H (1221,X'S) RIDE C ( 123,X'S) H (1231,X'S) RIDE C ( 124,X'S) H (1241,X'S) RIDE C ( 125,X'S) H (1251,X'S) RIDE C ( 128,X'S) H (1281,X'S) RIDE C ( 129,X'S) H (1291,X'S) RIDE C ( 130,X'S) H (1301,X'S) RIDE C ( 131,X'S) H (1311,X'S) RIDE C ( 132,X'S) H (1321,X'S) RIDE C ( 134,X'S) H (1341,X'S) RIDE C ( 135,X'S) H (1351,X'S) RIDE C ( 136,X'S) H (1361,X'S) RIDE C ( 137,X'S) H (1371,X'S) RIDE C ( 138,X'S) H (1381,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 16/02/12 at 14:12:10 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) A-U(IJ)'S 0.0, 0.0030000 = P(2) TO P(3) END ; #=== data_7 _database_code_depnum_ccdc_archive 'CCDC 869437' #TrackingRef '- combined_bf.cif' _audit_creation_date 11-11-11 _audit_creation_method CRYSTALS_ver_14.30 _vrf_PLAT410_7 ; PROBLEM: Short Intra H...H Contact H171 .. H192 .. 1.88 Ang. RESPONSE: This warning arises owing to unresolved disorder of the methylene carbon atoms. Location and placement of H atoms is thus subject to minor errors. Additional comment appears in the experimental section. ; _oxford_structure_analysis_title 'bfpan_6169_0m in C2/c' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 25.0443(7) _cell_length_b 15.9342(5) _cell_length_c 9.6935(3) _cell_angle_alpha 90 _cell_angle_beta 110.393(1) _cell_angle_gamma 90 _cell_volume 3625.85(19) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1 ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,y+1/2,z -x+1/2,-y+1/2,-z -x,y,-z+1/2 x,-y,z+1/2 -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Pt -1.7033 8.3905 27.0059 1.5129 17.7639 8.8117 15.7131 0.4246 5.7837 38.6103 11.6883 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C38 H33 N2 O1 P3 Pt1 # Dc = 1.51 Fooo = 1620.00 Mu = 40.33 M = 410.85 # Found Formula = C38 H32 N2 O1 P3 Pt1 # Dc = 1.50 FOOO = 1620.00 Mu = 40.33 M = 410.35 _chemical_formula_sum 'C38 H32 N2 O1 P3 Pt1' _chemical_formula_moiety 'C38 H32 N2 O1 P3 Pt1' _chemical_compound_source ? _chemical_formula_weight 820.70 _cell_measurement_reflns_used 9905 _cell_measurement_theta_min 2 _cell_measurement_theta_max 29 _cell_measurement_temperature 120 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_min 0.130 _exptl_crystal_size_mid 0.210 _exptl_crystal_size_max 0.270 _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1620 _exptl_absorpt_coefficient_mu 4.033 # Sheldrick geometric approximatio 0.43 0.59 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Analytical Absorption (De Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_min 0.43 _exptl_absorpt_correction_T_max 0.59 _diffrn_measurement_device_type 'Bruker Kappa Apex2' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 120 _diffrn_reflns_number 5303 _reflns_number_total 5303 _diffrn_reflns_av_R_equivalents 0.032 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 5303 # Theoretical number of reflections is about 10620 _diffrn_reflns_theta_min 1.545 _diffrn_reflns_theta_max 30.046 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.046 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _reflns_limit_h_min -35 _reflns_limit_h_max 33 _reflns_limit_k_min 0 _reflns_limit_k_max 22 _reflns_limit_l_min 0 _reflns_limit_l_max 13 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -1.71 _refine_diff_density_max 2.01 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>0.0\s(I) _refine_ls_number_reflns 5303 _refine_ls_number_restraints 0 _refine_ls_number_parameters 231 _oxford_refine_ls_R_factor_ref 0.0348 _refine_ls_wR_factor_ref 0.0605 _refine_ls_goodness_of_fit_ref 0.9968 _refine_ls_shift/su_max 0.0014223 _refine_ls_shift/su_mean 0.0000334 # The values computed with all filters except I/sigma _oxford_reflns_number_all 5303 _refine_ls_R_factor_all 0.0348 _refine_ls_wR_factor_all 0.0605 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4020 _refine_ls_R_factor_gt 0.0242 _refine_ls_wR_factor_gt 0.0550 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.02P)^2^ +12.81P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Bruker Analytical X-ray Systems, Inc., 2006. Apex2, Version 2 User Manual, M86-E01078, Madison, WI. De Meulenaer, J. & Tompa, H. (1965). Acta Cryst. 19, 1014. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Pt1 Pt 0.5000 0.752629(10) 0.2500 0.0232 1.0000 Uani S T . . . . P1 P 0.59610(3) 0.75528(5) 0.34678(7) 0.0261 1.0000 Uani . . . . . . P2 P 0.48900(6) 0.86751(9) 0.36769(17) 0.0260 0.5000 Uani . . . 1 1 . O1 O 0.47583(18) 0.9488(3) 0.2878(5) 0.0334 0.5000 Uani . . . . . . N1 N 0.5453(2) 0.8797(3) 0.5310(5) 0.0291 0.5000 Uani . . . 1 1 . N2 N 0.4443(2) 0.8491(3) 0.4632(5) 0.0296 0.5000 Uani . . . 1 1 . C1 C 0.62865(13) 0.6682(2) 0.4692(3) 0.0343 1.0000 Uani . . . . . . C2 C 0.60921(17) 0.5876(3) 0.4252(4) 0.0512 1.0000 Uani . . . . . . C3 C 0.63376(19) 0.5200(3) 0.5142(5) 0.0628 1.0000 Uani . . . . . . C4 C 0.67610(19) 0.5331(3) 0.6497(5) 0.0605 1.0000 Uani . . . . . . C5 C 0.69511(18) 0.6126(3) 0.6927(4) 0.0566 1.0000 Uani . . . . . . C6 C 0.67212(16) 0.6806(3) 0.6024(4) 0.0453 1.0000 Uani . . . . . . C7 C 0.62754(12) 0.75207(19) 0.2039(3) 0.0289 1.0000 Uani . . . . . . C8 C 0.67512(14) 0.7022(2) 0.2221(4) 0.0360 1.0000 Uani . . . . . . C9 C 0.69954(16) 0.6980(2) 0.1139(4) 0.0461 1.0000 Uani . . . . . . C10 C 0.67720(17) 0.7441(3) -0.0108(4) 0.0516 1.0000 Uani . . . . . . C11 C 0.63097(17) 0.7957(3) -0.0304(4) 0.0492 1.0000 Uani . . . . . . C12 C 0.60411(14) 0.7996(2) 0.0744(4) 0.0378 1.0000 Uani . . . . . . C13 C 0.62620(12) 0.8489(2) 0.4514(3) 0.0316 1.0000 Uani . . . . . . C14 C 0.67785(12) 0.8812(2) 0.4505(3) 0.0324 1.0000 Uani . . . . . . C15 C 0.70204(16) 0.9510(2) 0.5316(4) 0.0461 1.0000 Uani . . . . . . C16 C 0.67446(19) 0.9891(3) 0.6166(4) 0.0571 1.0000 Uani . . . . . . C17 C 0.62415(17) 0.9584(3) 0.6200(4) 0.0598 1.0000 Uani . . . . . . C18 C 0.59868(14) 0.8901(3) 0.5370(4) 0.0485 1.0000 Uani . . . . . . C19 C 0.5212(3) 0.9318(4) 0.6233(7) 0.0351 0.5000 Uani . . . . . . C20 C 0.4652(3) 0.8894(4) 0.6098(7) 0.0370 0.5000 Uani . . . 1 1 . H21 H 0.5778 0.5776 0.3350 0.0609 1.0000 Uiso R . . . . . H31 H 0.6217 0.4657 0.4855 0.0755 1.0000 Uiso R . . . . . H41 H 0.6917 0.4874 0.7104 0.0729 1.0000 Uiso R . . . . . H51 H 0.7233 0.6214 0.7813 0.0682 1.0000 Uiso R . . . . . H61 H 0.6856 0.7337 0.6302 0.0540 1.0000 Uiso R . . . . . H81 H 0.6910 0.6714 0.3091 0.0427 1.0000 Uiso R . . . . . H91 H 0.7307 0.6641 0.1277 0.0551 1.0000 Uiso R . . . . . H101 H 0.6931 0.7410 -0.0842 0.0618 1.0000 Uiso R . . . . . H111 H 0.6171 0.8288 -0.1137 0.0586 1.0000 Uiso R . . . . . H141 H 0.6965 0.8553 0.3959 0.0387 1.0000 Uiso R . . . . . H151 H 0.7353 0.9714 0.5277 0.0551 1.0000 Uiso R . . . . . H161 H 0.6898 1.0367 0.6718 0.0694 1.0000 Uiso R . . . . . H171 H 0.6070 0.9833 0.6804 0.0718 1.0000 Uiso R . . . . . H191 H 0.5146 0.9891 0.5804 0.0417 0.5000 Uiso R . . . . . H192 H 0.5470 0.9343 0.7263 0.0419 0.5000 Uiso R . . . . . H201 H 0.4383 0.9314 0.6216 0.0441 0.5000 Uiso R . . 1 1 . H202 H 0.4718 0.8462 0.6851 0.0440 0.5000 Uiso R . . 1 1 . H121 H 0.5709 0.8327 0.0580 0.0451 0.5000 Uiso R . . 1 1 . H181 H 0.5626 0.8711 0.5362 0.0575 0.5000 Uiso R . . 1 1 . 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 0.02035(7) 0.02384(7) 0.02465(7) 0.0000 0.00682(5) 0.0000 P1 0.0212(3) 0.0336(4) 0.0235(3) -0.0012(3) 0.0079(2) 0.0032(3) P2 0.0222(6) 0.0278(7) 0.0283(7) -0.0023(5) 0.0092(6) 0.0019(5) O1 0.031(2) 0.032(2) 0.038(2) 0.0032(18) 0.0134(19) 0.0014(17) N1 0.021(2) 0.043(3) 0.025(2) -0.009(2) 0.0097(19) -0.003(2) N2 0.027(2) 0.035(3) 0.029(2) -0.008(2) 0.013(2) -0.004(2) C1 0.0301(16) 0.0452(18) 0.0303(16) 0.0065(13) 0.0139(13) 0.0092(13) C2 0.043(2) 0.052(2) 0.050(2) 0.0130(18) 0.0060(17) 0.0022(17) C3 0.056(3) 0.049(2) 0.077(3) 0.017(2) 0.015(2) 0.011(2) C4 0.061(3) 0.070(3) 0.052(2) 0.026(2) 0.022(2) 0.032(2) C5 0.057(2) 0.070(3) 0.0341(19) 0.0075(18) 0.0052(17) 0.031(2) C6 0.046(2) 0.055(2) 0.0315(16) 0.0035(15) 0.0093(15) 0.0181(17) C7 0.0292(12) 0.0325(13) 0.0265(12) -0.0010(13) 0.0119(10) 0.0027(13) C8 0.0353(16) 0.0380(16) 0.0389(17) -0.0034(13) 0.0181(14) 0.0060(13) C9 0.048(2) 0.048(2) 0.054(2) -0.0056(17) 0.0320(18) 0.0067(16) C10 0.057(2) 0.066(2) 0.0447(19) -0.010(2) 0.0345(18) -0.001(2) C11 0.052(2) 0.067(3) 0.0320(17) 0.0059(17) 0.0191(17) 0.0025(19) C12 0.0344(17) 0.0455(18) 0.0352(16) 0.0071(14) 0.0142(14) 0.0061(14) C13 0.0208(13) 0.0438(17) 0.0258(14) -0.0081(12) 0.0027(11) 0.0032(12) C14 0.0234(14) 0.0383(16) 0.0334(15) -0.0049(12) 0.0073(12) 0.0015(12) C15 0.0387(19) 0.049(2) 0.0430(19) -0.0079(16) 0.0052(15) -0.0082(16) C16 0.059(3) 0.049(2) 0.046(2) -0.0202(18) -0.0025(19) 0.0058(19) C17 0.042(2) 0.085(3) 0.042(2) -0.027(2) 0.0013(17) 0.026(2) C18 0.0201(14) 0.086(3) 0.0365(18) -0.0240(18) 0.0063(13) 0.0045(16) C19 0.034(3) 0.039(3) 0.035(3) -0.011(3) 0.017(3) -0.003(3) C20 0.039(3) 0.039(3) 0.036(3) -0.009(3) 0.018(3) -0.005(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.046447(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pt1 . P1 5_655 2.2586(7) yes Pt1 . P2 5_655 2.2242(14) yes Pt1 . P1 . 2.2586(7) yes Pt1 . P2 . 2.2242(14) yes P1 . C1 . 1.823(3) yes P1 . C7 . 1.817(3) yes P1 . C13 . 1.814(3) yes P2 . P2 5_655 2.527(3) yes P2 . O1 . 1.485(4) yes P2 . N1 . 1.725(5) yes P2 . N2 . 1.709(5) yes O1 . O1 5_655 1.619(8) yes N1 . C18 . 1.329(5) yes N1 . C19 . 1.492(7) yes N2 . C12 5_655 1.384(6) yes N2 . C20 . 1.479(8) yes C1 . C2 . 1.386(5) yes C1 . C6 . 1.383(5) yes C2 . C3 . 1.385(5) yes C2 . H21 . 0.964 no C3 . C4 . 1.387(6) yes C3 . H31 . 0.926 no C4 . C5 . 1.366(6) yes C4 . H41 . 0.933 no C5 . C6 . 1.385(5) yes C5 . H51 . 0.913 no C6 . H61 . 0.916 no C7 . C8 . 1.392(4) yes C7 . C12 . 1.407(4) yes C8 . C9 . 1.388(4) yes C8 . H81 . 0.936 no C9 . C10 . 1.357(5) yes C9 . H91 . 0.920 no C10 . C11 . 1.378(6) yes C10 . H101 . 0.931 no C11 . C12 . 1.402(5) yes C11 . H111 . 0.925 no C12 . H121 . 0.950 no C13 . C14 . 1.394(4) yes C13 . C18 . 1.412(4) yes C14 . C15 . 1.375(4) yes C14 . H141 . 0.917 no C15 . C16 . 1.387(5) yes C15 . H151 . 0.908 no C16 . C17 . 1.362(6) yes C16 . H161 . 0.930 no C17 . C18 . 1.372(5) yes C17 . H171 . 0.927 no C18 . H181 . 0.950 no C19 . C20 . 1.521(9) yes C19 . H191 . 0.993 no C19 . H192 . 0.982 no C20 . H201 . 0.985 no C20 . H202 . 0.974 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag P1 5_655 Pt1 . P2 5_655 94.36(4) yes P1 5_655 Pt1 . P1 . 177.86(4) yes P2 5_655 Pt1 . P1 . 83.86(4) yes P1 5_655 Pt1 . P2 . 83.86(4) yes P2 5_655 Pt1 . P2 . 69.23(8) yes P1 . Pt1 . P2 . 94.36(4) yes Pt1 . P1 . C1 . 115.22(11) yes Pt1 . P1 . C7 . 111.40(9) yes C1 . P1 . C7 . 105.10(14) yes Pt1 . P1 . C13 . 115.01(10) yes C1 . P1 . C13 . 104.95(15) yes C7 . P1 . C13 . 104.07(14) yes P2 5_655 P2 . Pt1 . 55.38(4) yes P2 5_655 P2 . O1 . 66.91(17) yes Pt1 . P2 . O1 . 119.64(18) yes P2 5_655 P2 . N1 . 117.61(18) yes Pt1 . P2 . N1 . 110.86(18) yes O1 . P2 . N1 . 110.0(3) yes P2 5_655 P2 . N2 . 151.57(19) yes Pt1 . P2 . N2 . 111.02(18) yes O1 . P2 . N2 . 111.3(2) yes N1 . P2 . N2 . 90.1(2) yes O1 5_655 O1 . P2 . 99.8(2) yes P2 . N1 . C18 . 122.8(4) yes P2 . N1 . C19 . 104.0(4) yes C18 . N1 . C19 . 121.0(4) yes C12 5_655 N2 . P2 . 129.3(4) yes C12 5_655 N2 . C20 . 119.1(4) yes P2 . N2 . C20 . 111.5(4) yes P1 . C1 . C2 . 118.4(3) yes P1 . C1 . C6 . 121.8(3) yes C2 . C1 . C6 . 119.8(3) yes C1 . C2 . C3 . 119.8(4) yes C1 . C2 . H21 . 121.4 no C3 . C2 . H21 . 118.7 no C2 . C3 . C4 . 120.0(4) yes C2 . C3 . H31 . 120.8 no C4 . C3 . H31 . 119.2 no C3 . C4 . C5 . 119.9(4) yes C3 . C4 . H41 . 119.6 no C5 . C4 . H41 . 120.5 no C4 . C5 . C6 . 120.6(4) yes C4 . C5 . H51 . 120.1 no C6 . C5 . H51 . 119.3 no C5 . C6 . C1 . 119.8(4) yes C5 . C6 . H61 . 120.4 no C1 . C6 . H61 . 119.7 no P1 . C7 . C8 . 119.9(2) yes P1 . C7 . C12 . 120.5(2) yes C8 . C7 . C12 . 119.6(3) yes C7 . C8 . C9 . 120.9(3) yes C7 . C8 . H81 . 119.4 no C9 . C8 . H81 . 119.7 no C8 . C9 . C10 . 119.6(3) yes C8 . C9 . H91 . 119.5 no C10 . C9 . H91 . 120.8 no C9 . C10 . C11 . 120.7(3) yes C9 . C10 . H101 . 120.0 no C11 . C10 . H101 . 119.3 no C10 . C11 . C12 . 121.3(3) yes C10 . C11 . H111 . 120.1 no C12 . C11 . H111 . 118.6 no C7 . C12 . C11 . 117.8(3) yes C7 . C12 . N2 5_655 126.6(3) yes C11 . C12 . N2 5_655 115.6(3) yes C7 . C12 . H121 . 121.1 no C11 . C12 . H121 . 121.1 no P1 . C13 . C14 . 120.4(2) yes P1 . C13 . C18 . 121.2(3) yes C14 . C13 . C18 . 118.4(3) yes C13 . C14 . C15 . 121.3(3) yes C13 . C14 . H141 . 119.9 no C15 . C14 . H141 . 118.8 no C14 . C15 . C16 . 118.9(4) yes C14 . C15 . H151 . 119.7 no C16 . C15 . H151 . 121.4 no C15 . C16 . C17 . 120.9(4) yes C15 . C16 . H161 . 120.6 no C17 . C16 . H161 . 118.5 no C16 . C17 . C18 . 121.0(3) yes C16 . C17 . H171 . 119.8 no C18 . C17 . H171 . 119.1 no C13 . C18 . C17 . 119.4(3) yes C13 . C18 . N1 . 127.3(4) yes C17 . C18 . N1 . 112.3(4) yes C13 . C18 . H181 . 120.3 no C17 . C18 . H181 . 120.3 no N1 . C19 . C20 . 104.7(5) yes N1 . C19 . H191 . 107.7 no C20 . C19 . H191 . 111.0 no N1 . C19 . H192 . 112.0 no C20 . C19 . H192 . 111.4 no H191 . C19 . H192 . 110.0 no C19 . C20 . N2 . 106.5(5) yes C19 . C20 . H201 . 109.6 no N2 . C20 . H201 . 112.2 no C19 . C20 . H202 . 109.8 no N2 . C20 . H202 . 109.0 no H201 . C20 . H202 . 109.7 no _iucr_refine_instruction_details_constraints ; # # Punched on 11/11/11 at 11:19:10 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 2,X'S) H ( 21,X'S) RIDE C ( 3,X'S) H ( 31,X'S) RIDE C ( 4,X'S) H ( 41,X'S) RIDE C ( 5,X'S) H ( 51,X'S) RIDE C ( 6,X'S) H ( 61,X'S) RIDE C ( 8,X'S) H ( 81,X'S) RIDE C ( 9,X'S) H ( 91,X'S) RIDE C ( 10,X'S) H ( 101,X'S) RIDE C ( 11,X'S) H ( 111,X'S) RIDE C ( 12,X'S) H ( 121,X'S) RIDE C ( 14,X'S) H ( 141,X'S) RIDE C ( 15,X'S) H ( 151,X'S) RIDE C ( 16,X'S) H ( 161,X'S) RIDE C ( 17,X'S) H ( 171,X'S) RIDE C ( 18,X'S) H ( 181,X'S) RIDE C ( 19,X'S) H ( 191,X'S) H ( 192,X'S) RIDE C ( 20,X'S) H ( 201,X'S) H ( 202,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 11/11/11 at 11:19:10 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 -0.019 276 87 ' ' 2 0.500 0.500 0.047 276 87 ' ' _platon_squeeze_details ; During the structure solution, electron density difference maps revealed that there were considerable disordered solvent molecules, which could not be successfully modeled. >From history, the remaining solvate was likely ether or THF in a volume of 553.9 \%A3 per unit cell (15.3%). It appeared that the cavity areas contained about four ether and/or THF molecules, located near the centers of symmetry at (0, 0, 0) and ( 1/2, 1/2 , 0 ). Modeling with or without restraints was unsuccessful, as was step by step acquisition of peaks using successive electron density difference maps. Thus, the structure factors were modified using the PLATON SQUEEZE technique, in order to produce a ?solvate-free? structure factor set. PLATON reported a total electron density of 174 e- per unit cell, likely representing four THF or ether molecules, consistent with our earlier observations. Use of the SQUEEZE technique resulted in a decrease of ca. 1.7 % in R. ; #===END