Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_CRYSTALS_cif_1 _database_code_CSD 162979 _journal_coden_Cambridge 182 _audit_creation_date 01-21-03 _audit_creation_method CRYSTALS_ver_12-03-99 # 1. SUBMISSION DETAILS _publ_contact_letter ; ; _publ_contact_author_name 'Lowe, Gordon' _publ_contact_author_address ; The Dyson Perrins Laboratory, Department of Chemistry, Oxford University, South Parks Road, Oxford OX1 3QY ; _publ_contact_author_phone ' 01865 275 649 ' _publ_contact_author_fax ' 01865 275 674 ' _publ_contact_author_email ' gordon.lowe@chem.ox.ac.uk ' #============================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_coden_ASTM ? _journal_name_full 'Chemical Communications' _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; The X-ray structure of N,S-bis-[4'-chloro-2,2',2"-terpyridine platinum (II)] 2-mercaptoimidazole tris-fluorophosphate and tris-[2,2':6',2"-terpyridine platinum (II)] sulfonium perchlorate ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address _publ_author_footnote 'Lowe, Gordon' ; The Dyson Perrins Laboratory, Department of Chemistry, Oxford University, South Parks Road, Oxford OX1 3QY ; ; ? #footnote for author 1 ; 'Ross, Steven. A.' ; The Dyson Perrins Laboratory, Department of Chemistry, Oxford University, South Parks Road, Oxford OX1 3QY ; ; ? # footnote 2 ; 'Probert, Michael. R.' ; Chemical Crystallography, Department of Chemistry, Oxford University, 9 Parks Road, Oxford OX1 3PD ; ; ? # footnote 2 ; 'Cowley, Andrew. R.' ; Chemical Crystallography, Department of Chemistry, Oxford University, 9 Parks Road, Oxford OX1 3PD ; ; ? # footnote 2 ; #============================================================================== # 4. TEXT _publ_section_abstract #Text of the abstract ; ? ; _publ_section_comment #Text of the paper ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions #Captions to figures ; ? ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen for refinement keywords. ; H atoms placed geometrically after each cycle ; _publ_section_exptl_prep ; ? ; #========================================================================== _chemical_name_systematic # IUPAC name, in full ; tris-[2,2':6'2''-terpyridine platinum(II)] sulphonium perchlorate bisacetone solvate ; _chemical_melting_point 'not measured' # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment noref #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et all 200 ; _computing_publication_material ; CRYSTALS (Watkin et all 200 ; _computing_molecular_graphics ; CAMERON (Watkin et al 1996) ; #============================================================= _cell_length_a 15.2505(3) _cell_angle_alpha 90 _cell_length_b 24.4126(5) _cell_angle_beta 90.0327(15) _cell_length_c 17.3087(3) _cell_angle_gamma 90 _cell_volume 6444.1 _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'C 1 2/c 1 ' 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 ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'Pt ' -2.3520 8.3880 27.0059 1.5129 17.7639 8.8117 15.7131 0.4246 5.7837 38.6103 11.6883 'International_Tables_Vol_IV_Table_2.2B' 'S ' 0.1100 0.1240 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C28.50 H28.50 Cl2 N4.50 O10 Pt1.50 S0.50 ' _chemical_formula_moiety ' C28.50 H28.50 Cl2 N4.50 O10 Pt1.50 S0.50 ' _chemical_compound_source ; synthesis as described ; _chemical_formula_weight 973.63 _cell_measurement_reflns_used 6217 _cell_measurement_theta_min 3 _cell_measurement_theta_max 27 _cell_measurement_temperature 190 _cell_formula_units_Z 8 _exptl_crystal_description ' block ' _exptl_crystal_colour ' red ' _exptl_crystal_size_min 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_max 0.50 _exptl_crystal_density_diffrn 2.007 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 3736.066 _exptl_absorpt_coefficient_mu 6.776 _diffrn_measurement_device_type ; Enraf Nonius Kappa CCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; COLLECT (Nonius BV, 1997) ; _computing_data_reduction ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.045 _exptl_absorpt_correction_T_max 0.064 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 190 _diffrn_reflns_number 20122 _reflns_number_total 6940 _diffrn_reflns_av_R_equivalents 0.031 # Number of reflections with Friedels Law is 6940 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 7702 _diffrn_measured_fraction_theta_max 0.901 _reflns_number_gt 6004 _diffrn_reflns_theta_min 4.74 _diffrn_reflns_theta_max 27.90 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _reflns_limit_h_min -20 _reflns_limit_h_max 20 _reflns_limit_k_min 0 _reflns_limit_k_max 32 _reflns_limit_l_min 0 _reflns_limit_l_max 22 _refine_diff_density_min -1.78 _refine_diff_density_max 0.97 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 6004 _refine_ls_number_parameters 422 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0306 _refine_ls_goodness_of_fit_ref 1.0934 _refine_ls_shift/su_max 0.038416 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 5 parameters, Carruthers & Watkin , 1979, 12.3 -2.17 10.4 2.72 1.01 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 COLLECT Software, Nonius BV 1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Watkin, D.J., Prout, C.K., Carruthers, J.R., Betteridge, P.W. & Cooper R.I. (2001) CRYSTALS Issue 11. Chemical Crystallography Laboratory, OXFORD, UK. 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 loop_ _atom_site_label _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 Pt1 -0.381193(7) 0.107775(5) -0.292317(7) 0.0212 1.0000 Uani Pt2 -0.5000 -0.035139(6) -0.2500 0.0212 1.0000 Uani Cl1 -0.34336(7) 0.12587(4) -0.55336(5) 0.0379 1.0000 Uani Cl2 -0.16626(6) 0.17791(4) -0.09500(6) 0.0443 1.0000 Uani S1 -0.50840(13) 0.05910(6) -0.2691(1) 0.0261 0.5000 Uani O1 -0.3505(5) 0.10158(18) -0.4788(3) 0.1035 1.0000 Uani O2 -0.2532(3) 0.14070(17) -0.5638(4) 0.0935 1.0000 Uani O3 -0.3976(2) 0.17338(13) -0.5567(2) 0.0559 1.0000 Uani O4 -0.3683(3) 0.08612(17) -0.6086(2) 0.0630 1.0000 Uani O5 -0.2423(3) 0.1622(2) -0.1339(3) 0.0830 1.0000 Uani O6 -0.1567(4) 0.1448(3) -0.0275(4) 0.1175 1.0000 Uani O7 -0.0907(2) 0.17218(16) -0.1440(3) 0.0670 1.0000 Uani O8 -0.1725(4) 0.2328(2) -0.0684(3) 0.0902 1.0000 Uani N1 -0.28420(18) 0.05971(12) -0.24816(16) 0.0272 1.0000 Uani N2 -0.27921(18) 0.15019(11) -0.32652(16) 0.0263 1.0000 Uani N3 -0.44337(19) 0.17017(11) -0.34922(16) 0.0280 1.0000 Uani N4 -0.44347(18) -0.04903(11) -0.35473(18) 0.0291 1.0000 Uani N5 -0.5000 -0.11518(14) -0.2500 0.0268 1.0000 Uani C1 -0.2914(3) 0.01483(16) -0.2045(2) 0.0365 1.0000 Uani C2 -0.2182(3) -0.01426(19) -0.1783(3) 0.0474 1.0000 Uani C3 -0.1362(3) 0.0055(2) -0.1961(3) 0.0559 1.0000 Uani C4 -0.1283(3) 0.0527(2) -0.2387(3) 0.0479 1.0000 Uani C5 -0.2024(2) 0.07963(15) -0.2651(2) 0.0321 1.0000 Uani C6 -0.1994(2) 0.12982(15) -0.3106(2) 0.0319 1.0000 Uani C7 -0.1255(3) 0.15768(17) -0.3376(2) 0.0392 1.0000 Uani C8 -0.1381(3) 0.20581(18) -0.3778(2) 0.0408 1.0000 Uani C9 -0.2220(3) 0.22649(16) -0.3919(2) 0.0394 1.0000 Uani C10 -0.2932(2) 0.19649(14) -0.36555(19) 0.0289 1.0000 Uani C11 -0.3866(2) 0.20889(13) -0.3771(2) 0.0294 1.0000 Uani C12 -0.4160(3) 0.25488(16) -0.4158(2) 0.0399 1.0000 Uani C13 -0.5055(3) 0.26047(17) -0.4299(3) 0.0448 1.0000 Uani C14 -0.5625(3) 0.22052(17) -0.4047(2) 0.0399 1.0000 Uani C15 -0.5289(2) 0.17595(15) -0.3638(2) 0.0328 1.0000 Uani C16 -0.4209(2) -0.01251(14) -0.4097(2) 0.0342 1.0000 Uani C17 -0.3831(3) -0.02840(17) -0.4790(2) 0.0415 1.0000 Uani C18 -0.3655(3) -0.08335(19) -0.4920(2) 0.0453 1.0000 Uani C19 -0.3904(3) -0.12157(16) -0.4362(2) 0.0388 1.0000 Uani C20 -0.4301(2) -0.10369(14) -0.3694(2) 0.0324 1.0000 Uani C21 -0.4628(2) -0.14113(13) -0.3096(2) 0.0299 1.0000 Uani C22 -0.4611(3) -0.19812(14) -0.3103(2) 0.0379 1.0000 Uani C23 -0.5000 -0.22598(19) -0.2500 0.0397 1.0000 Uani O9 0.0355(3) 0.03043(15) -0.10502(19) 0.0779 1.0000 Uani C24 0.0798(2) 0.04080(14) -0.0487(2) 0.0528 1.0000 Uani C25 0.1612(3) 0.0099(2) -0.0324(3) 0.0853 1.0000 Uani C26 0.0552(3) 0.08438(18) 0.0062(3) 0.0660 1.0000 Uani O10 -0.4230(12) 0.3115(6) -0.2515(6) 0.161(5) 0.46(1) Uiso C27 -0.365(1) 0.3346(5) -0.2153(5) 0.096(3) 0.46(1) Uiso C28 -0.2739(12) 0.3147(8) -0.2186(9) 0.142(3) 0.46(1) Uiso C29 -0.3823(17) 0.3833(6) -0.1668(7) 0.142(3) 0.46(1) Uiso O11 -0.248(1) 0.4075(6) -0.1927(4) 0.161(5) 0.54(1) Uiso C30 -0.3045(9) 0.3723(5) -0.1964(3) 0.096(3) 0.54(1) Uiso C31 -0.2855(15) 0.3168(6) -0.2254(4) 0.142(3) 0.54(1) Uiso C32 -0.396(1) 0.3835(9) -0.1717(4) 0.142(3) 0.54(1) Uiso H11 -0.3512 0.0016 -0.1900 0.0437 1.0000 Uiso H21 -0.2253 -0.0486 -0.1473 0.0569 1.0000 Uiso H31 -0.0826 -0.0144 -0.1781 0.0671 1.0000 Uiso H41 -0.0689 0.0677 -0.2507 0.0575 1.0000 Uiso H71 -0.0652 0.1431 -0.3280 0.0471 1.0000 Uiso H81 -0.0859 0.2264 -0.3973 0.0490 1.0000 Uiso H91 -0.2305 0.2618 -0.4202 0.0473 1.0000 Uiso H121 -0.3738 0.2836 -0.4335 0.0479 1.0000 Uiso H131 -0.5282 0.2933 -0.4581 0.0538 1.0000 Uiso H141 -0.6268 0.2234 -0.4155 0.0479 1.0000 Uiso H151 -0.5704 0.1473 -0.3447 0.0394 1.0000 Uiso H161 -0.4317 0.0273 -0.4002 0.0410 1.0000 Uiso H171 -0.3687 -0.0005 -0.5193 0.0498 1.0000 Uiso H181 -0.3355 -0.0954 -0.5405 0.0544 1.0000 Uiso H191 -0.3795 -0.1615 -0.4447 0.0465 1.0000 Uiso H221 -0.4323 -0.2184 -0.3535 0.0455 1.0000 Uiso H231 -0.5000 -0.2669 -0.2500 0.0477 1.0000 Uiso H251 0.1886 0.0242 0.0161 0.1023 1.0000 Uiso H252 0.2031 0.0145 -0.0764 0.1023 1.0000 Uiso H253 0.1470 -0.0298 -0.0259 0.1023 1.0000 Uiso H261 0.0999 0.0865 0.0484 0.0792 1.0000 Uiso H262 0.0525 0.1203 -0.0216 0.0792 1.0000 Uiso H263 -0.0035 0.0759 0.0289 0.0792 1.0000 Uiso H281 -0.2358 0.3385 -0.1857 0.1707 0.4626 Uiso H282 -0.2527 0.3158 -0.2732 0.1707 0.4626 Uiso H283 -0.2715 0.2761 -0.1991 0.1707 0.4626 Uiso H291 -0.3264 0.3959 -0.1423 0.1707 0.4626 Uiso H292 -0.4068 0.4133 -0.1998 0.1707 0.4626 Uiso H293 -0.4256 0.3735 -0.1257 0.1707 0.4626 Uiso H311 -0.3402 0.2942 -0.2239 0.1707 0.5374 Uiso H312 -0.2639 0.3192 -0.2799 0.1707 0.5374 Uiso H313 -0.2396 0.2994 -0.1923 0.1707 0.5374 Uiso H321 -0.4321 0.3498 -0.1791 0.1707 0.5374 Uiso H322 -0.4204 0.4140 -0.2035 0.1707 0.5374 Uiso H323 -0.3961 0.3942 -0.1160 0.1707 0.5374 Uiso 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 0.01738(7) 0.01851(7) 0.02783(8) -0.00197(4) 0.00408(5) -0.00476(4) Pt2 0.01479(8) 0.01373(8) 0.0351(1) 0.0000 0.00034(6) 0.0000 Cl1 0.0446(5) 0.0298(4) 0.0392(4) -0.0010(3) -0.0007(4) -0.0036(3) Cl2 0.0326(4) 0.0453(5) 0.0551(5) 0.0049(4) 0.0016(4) -0.0065(4) S1 0.0183(8) 0.0166(5) 0.0436(12) -0.0003(5) 0.0088(9) -0.0001(5) O1 0.209(7) 0.050(2) 0.051(2) 0.0071(17) 0.017(3) -0.002(3) O2 0.0338(19) 0.055(2) 0.192(6) 0.011(3) -0.029(3) -0.0048(15) O3 0.0471(18) 0.0363(15) 0.084(2) -0.0003(15) 0.0040(16) 0.0016(13) O4 0.050(2) 0.071(2) 0.067(2) -0.0307(19) -0.0117(16) 0.0058(17) O5 0.042(2) 0.118(4) 0.090(3) -0.043(3) -0.0041(19) -0.006(2) O6 0.090(4) 0.142(6) 0.120(4) 0.081(4) -0.005(3) -0.010(4) O7 0.0410(19) 0.058(2) 0.102(3) 0.0008(19) 0.0186(18) -0.0035(15) O8 0.101(4) 0.078(3) 0.092(3) -0.032(2) 0.033(3) -0.027(3) N1 0.0220(12) 0.0302(13) 0.0296(13) -0.002(1) 0.0002(11) -0.004(1) N2 0.0225(13) 0.0289(13) 0.0275(13) 0.002(1) 0.001(1) -0.008(1) N3 0.0291(14) 0.0241(13) 0.0310(13) -0.000(1) 0.0007(11) -0.005(1) N4 0.0225(13) 0.0214(12) 0.0433(16) 0.0033(11) -0.0028(11) -0.0012(9) N5 0.031(2) 0.0121(15) 0.037(2) 0.0000 -0.0057(16) 0.0000 C1 0.0337(18) 0.0364(18) 0.0393(18) 0.0053(14) -0.0034(15) -0.0056(14) C2 0.038(2) 0.048(2) 0.056(2) 0.0164(19) -0.0139(18) -0.0065(17) C3 0.036(2) 0.056(3) 0.075(3) 0.018(2) -0.019(2) -0.0049(19) C4 0.0257(18) 0.054(2) 0.064(3) 0.010(2) -0.0105(18) -0.0076(16) C5 0.0193(14) 0.0353(16) 0.0418(18) -0.0012(14) -0.0008(13) -0.0085(12) C6 0.0197(14) 0.0399(18) 0.0361(17) -0.0017(14) 0.0000(13) -0.0089(13) C7 0.0264(17) 0.045(2) 0.046(2) 0.0025(16) 0.0021(15) -0.0121(15) C8 0.0307(19) 0.045(2) 0.046(2) 0.0032(16) 0.0043(16) -0.0150(15) C9 0.042(2) 0.0337(17) 0.0427(19) 0.0066(15) 0.0015(16) -0.0123(15) C10 0.0287(16) 0.0285(15) 0.0295(15) -0.0023(12) 0.0002(13) -0.0071(12) C11 0.0272(16) 0.0279(15) 0.0330(16) -0.0001(12) 0.0009(13) -0.0058(12) C12 0.043(2) 0.0317(17) 0.0454(19) 0.0097(16) 0.0023(16) -0.0029(16) C13 0.047(2) 0.038(2) 0.050(2) 0.0100(16) -0.0010(18) 0.0041(16) C14 0.035(2) 0.041(2) 0.043(2) 0.0031(16) -0.0042(16) 0.0034(15) C15 0.0268(16) 0.0360(17) 0.0356(16) 0.0007(14) 0.0015(13) 0.0005(13) C16 0.0315(18) 0.0290(16) 0.0421(19) -0.0003(14) -0.0011(15) -0.0042(13) C17 0.042(2) 0.042(2) 0.0407(19) 0.0054(16) 0.0051(16) -0.0083(16) C18 0.048(2) 0.048(2) 0.041(2) -0.0086(17) 0.0069(18) -0.0065(18) C19 0.045(2) 0.0328(17) 0.0387(19) -0.0076(14) 0.0056(16) -0.0004(15) C20 0.0296(17) 0.0233(14) 0.0441(19) -0.0040(13) -0.0047(15) 0.0004(12) C21 0.0288(16) 0.0234(14) 0.0375(17) -0.0023(12) -0.0050(13) 0.0044(12) C22 0.053(2) 0.0217(15) 0.0387(18) -0.0059(13) -0.0056(16) 0.0064(14) C23 0.050(3) 0.018(2) 0.051(3) 0.0000 -0.013(3) 0.0000 O9 0.067(3) 0.093(3) 0.074(3) -0.010(2) -0.023(2) -0.007(2) C24 0.038(2) 0.054(3) 0.066(3) 0.008(2) -0.009(2) -0.0083(18) C25 0.061(4) 0.093(5) 0.103(5) -0.022(4) -0.030(3) 0.016(3) C26 0.059(3) 0.068(3) 0.072(3) 0.003(3) -0.005(3) -0.009(3) _refine_ls_extinction_method 'None' 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 . S1 . 2.3102(19) yes Pt1 . S1 5_454 2.3195(19) yes Pt1 . N1 . 2.037(3) yes Pt1 . N2 . 1.960(3) yes Pt1 . N3 . 2.047(3) yes Pt2 . S1 . 2.3279(14) yes Pt2 . S1 5_454 2.3279(14) yes Pt2 . N4 . 2.036(3) yes Pt2 . N4 5_454 2.036(3) yes Pt2 . N5 . 1.954(3) yes Cl1 . O1 . 1.425(4) yes Cl1 . O2 . 1.433(4) yes Cl1 . O3 . 1.426(3) yes Cl1 . O4 . 1.414(3) yes Cl2 . O5 . 1.394(4) yes Cl2 . O6 . 1.428(5) yes Cl2 . O7 . 1.438(4) yes Cl2 . O8 . 1.421(5) yes S1 . S1 5_454 0.710(3) yes N1 . C1 . 1.336(5) yes N1 . C5 . 1.370(4) yes N2 . C6 . 1.343(5) yes N2 . C10 . 1.334(4) yes N3 . C11 . 1.370(4) yes N3 . C15 . 1.337(5) yes N4 . C16 . 1.349(5) yes N4 . C20 . 1.374(4) yes N5 . C21 . 1.336(4) yes N5 . C21 5_454 1.336(4) yes C1 . C2 . 1.398(6) yes C1 . H11 . 1.000(4) no C2 . C3 . 1.375(7) yes C2 . H21 . 1.000(4) no C3 . C4 . 1.373(7) yes C3 . H31 . 1.000(5) no C4 . C5 . 1.385(5) yes C4 . H41 . 1.000(4) no C5 . C6 . 1.458(5) yes C6 . C7 . 1.396(5) yes C7 . C8 . 1.379(6) yes C7 . H71 . 1.000(4) no C8 . C9 . 1.398(6) yes C8 . H81 . 1.000(4) no C9 . C10 . 1.386(5) yes C9 . H91 . 1.000(4) no C10 . C11 . 1.470(5) yes C11 . C12 . 1.383(5) yes C12 . C13 . 1.393(6) yes C12 . H121 . 1.000(4) no C13 . C14 . 1.378(6) yes C13 . H131 . 1.000(4) no C14 . C15 . 1.395(5) yes C14 . H141 . 1.000(4) no C15 . H151 . 1.000(4) no C16 . C17 . 1.386(6) yes C16 . H161 . 1.000(4) no C17 . C18 . 1.386(6) yes C17 . H171 . 1.000(4) no C18 . C19 . 1.396(6) yes C18 . H181 . 1.000(4) no C19 . C20 . 1.377(6) yes C19 . H191 . 1.000(4) no C20 . C21 . 1.469(5) yes C21 . C22 . 1.392(5) yes C22 . C23 . 1.380(5) yes C22 . H221 . 1.000(4) no C23 . H231 . 1.000(5) no O9 . C24 . 1.213(5) yes C24 . C25 . 1.479(6) yes C24 . C26 . 1.475(6) yes C25 . H251 . 1.000(6) no C25 . H252 . 1.000(4) no C25 . H253 . 1.000(4) no C26 . H261 . 1.000(6) no C26 . H262 . 1.000(4) no C26 . H263 . 1.000(4) no O10 . C27 . 1.226(9) yes C27 . C28 . 1.47(1) yes C27 . C29 . 1.48(1) yes C27 . C30 . 1.34(2) yes C27 . C31 . 1.30(3) yes C27 . C32 . 1.49(3) yes C27 . H311 . 1.065(13) no C27 . H321 . 1.261(14) no C28 . C30 . 1.53(3) yes C28 . C31 . 0.22(3) yes C28 . H281 . 1.00(2) no C28 . H282 . 1.000(13) no C28 . H283 . 1.000(13) no C28 . H311 . 1.13(2) no C28 . H312 . 1.077(13) no C28 . H313 . 0.787(14) no C29 . C30 . 1.32(3) yes C29 . C32 . 0.22(3) yes C29 . H291 . 1.00(3) no C29 . H292 . 1.000(14) no C29 . H293 . 1.000(14) no C29 . H321 . 1.14(2) no C29 . H322 . 1.142(17) no C29 . H323 . 0.944(14) no O11 . C30 . 1.223(9) yes C30 . C31 . 1.47(1) yes C30 . C32 . 1.48(1) yes C30 . H291 . 1.149(11) no C31 . H281 . 1.153(17) no C31 . H282 . 0.967(16) no C31 . H283 . 1.113(12) no C31 . H311 . 1.00(2) no C31 . H312 . 1.000(12) no C31 . H313 . 1.000(12) no C32 . H291 . 1.211(16) no C32 . H292 . 0.891(14) no C32 . H293 . 0.950(11) no C32 . H321 . 1.00(2) no C32 . H322 . 1.000(12) no C32 . H323 . 1.000(12) no H282 . H312 . 0.222 no H283 . H313 . 0.757 no H292 . H322 . 0.219 no H293 . H323 . 0.695 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 S1 . Pt1 . S1 5_454 17.64(7) yes S1 . Pt1 . N1 . 104.38(9) yes S1 5_454 Pt1 . N1 . 93.44(9) yes S1 . Pt1 . N2 . 172.14(9) yes S1 5_454 Pt1 . N2 . 170.18(9) yes N1 . Pt1 . N2 . 80.88(11) yes S1 . Pt1 . N3 . 94.45(9) yes S1 5_454 Pt1 . N3 . 105.41(9) yes N1 . Pt1 . N3 . 161.02(11) yes N2 . Pt1 . N3 . 80.15(12) yes S1 . Pt2 . S1 5_454 17.54(7) yes S1 . Pt2 . N4 . 93.51(9) yes S1 5_454 Pt2 . N4 . 105.54(9) yes S1 . Pt2 . N4 5_454 105.54(9) yes S1 5_454 Pt2 . N4 5_454 93.51(9) yes N4 . Pt2 . N4 5_454 160.83(15) yes S1 . Pt2 . N5 . 171.23(4) yes S1 5_454 Pt2 . N5 . 171.23(4) yes N4 . Pt2 . N5 . 80.42(7) yes N4 5_454 Pt2 . N5 . 80.42(7) yes O1 . Cl1 . O2 . 107.0(4) yes O1 . Cl1 . O3 . 109.3(3) yes O2 . Cl1 . O3 . 110.3(2) yes O1 . Cl1 . O4 . 107.8(3) yes O2 . Cl1 . O4 . 110.3(3) yes O3 . Cl1 . O4 . 112.0(2) yes O5 . Cl2 . O6 . 108.9(4) yes O5 . Cl2 . O7 . 110.8(3) yes O6 . Cl2 . O7 . 110.2(3) yes O5 . Cl2 . O8 . 111.1(3) yes O6 . Cl2 . O8 . 106.0(4) yes O7 . Cl2 . O8 . 109.7(3) yes Pt1 . S1 . Pt1 5_454 115.22(6) yes Pt1 . S1 . Pt2 . 119.14(8) yes Pt1 5_454 S1 . Pt2 . 118.75(8) yes Pt1 . S1 . S1 5_454 81.9(3) yes Pt1 5_454 S1 . S1 5_454 80.4(3) yes Pt2 . S1 . S1 5_454 81.23(4) yes Pt1 . N1 . C1 . 128.7(2) yes Pt1 . N1 . C5 . 112.1(2) yes C1 . N1 . C5 . 119.2(3) yes Pt1 . N2 . C6 . 117.5(2) yes Pt1 . N2 . C10 . 118.3(2) yes C6 . N2 . C10 . 124.2(3) yes Pt1 . N3 . C11 . 112.9(2) yes Pt1 . N3 . C15 . 128.4(2) yes C11 . N3 . C15 . 118.6(3) yes Pt2 . N4 . C16 . 128.8(2) yes Pt2 . N4 . C20 . 112.9(2) yes C16 . N4 . C20 . 118.3(3) yes Pt2 . N5 . C21 . 118.30(19) yes Pt2 . N5 . C21 5_454 118.30(19) yes C21 . N5 . C21 5_454 123.4(4) yes N1 . C1 . C2 . 122.3(4) yes N1 . C1 . H11 . 118.8(4) no C2 . C1 . H11 . 118.8(4) no C1 . C2 . C3 . 118.3(4) yes C1 . C2 . H21 . 120.8(4) no C3 . C2 . H21 . 120.8(4) no C2 . C3 . C4 . 119.6(4) yes C2 . C3 . H31 . 120.2(5) no C4 . C3 . H31 . 120.2(5) no C3 . C4 . C5 . 120.3(4) yes C3 . C4 . H41 . 119.9(4) no C5 . C4 . H41 . 119.9(4) no N1 . C5 . C4 . 120.2(3) yes N1 . C5 . C6 . 116.3(3) yes C4 . C5 . C6 . 123.5(3) yes N2 . C6 . C5 . 113.1(3) yes N2 . C6 . C7 . 118.9(4) yes C5 . C6 . C7 . 128.0(3) yes C6 . C7 . C8 . 118.2(4) yes C6 . C7 . H71 . 120.9(4) no C8 . C7 . H71 . 120.9(4) no C7 . C8 . C9 . 121.5(3) yes C7 . C8 . H81 . 119.2(4) no C9 . C8 . H81 . 119.2(4) no C8 . C9 . C10 . 117.9(3) yes C8 . C9 . H91 . 121.0(4) no C10 . C9 . H91 . 121.0(4) no N2 . C10 . C9 . 119.3(3) yes N2 . C10 . C11 . 113.4(3) yes C9 . C10 . C11 . 127.2(3) yes N3 . C11 . C10 . 115.0(3) yes N3 . C11 . C12 . 121.7(3) yes C10 . C11 . C12 . 123.2(3) yes C11 . C12 . C13 . 118.8(3) yes C11 . C12 . H121 . 120.6(4) no C13 . C12 . H121 . 120.6(4) no C12 . C13 . C14 . 119.6(4) yes C12 . C13 . H131 . 120.2(4) no C14 . C13 . H131 . 120.2(4) no C13 . C14 . C15 . 118.8(4) yes C13 . C14 . H141 . 120.6(4) no C15 . C14 . H141 . 120.6(4) no N3 . C15 . C14 . 122.4(3) yes N3 . C15 . H151 . 118.8(3) no C14 . C15 . H151 . 118.8(3) no N4 . C16 . C17 . 122.1(3) yes N4 . C16 . H161 . 118.9(4) no C17 . C16 . H161 . 118.9(4) no C16 . C17 . C18 . 119.5(4) yes C16 . C17 . H171 . 120.3(4) no C18 . C17 . H171 . 120.3(4) no C17 . C18 . C19 . 118.8(4) yes C17 . C18 . H181 . 120.6(4) no C19 . C18 . H181 . 120.6(4) no C18 . C19 . C20 . 119.3(4) yes C18 . C19 . H191 . 120.4(4) no C20 . C19 . H191 . 120.4(4) no N4 . C20 . C19 . 121.9(3) yes N4 . C20 . C21 . 115.1(3) yes C19 . C20 . C21 . 123.0(3) yes N5 . C21 . C20 . 113.2(3) yes N5 . C21 . C22 . 119.3(3) yes C20 . C21 . C22 . 127.5(3) yes C21 . C22 . C23 . 118.5(4) yes C21 . C22 . H221 . 120.7(4) no C23 . C22 . H221 . 120.7(3) no C22 . C23 . C22 5_454 120.9(4) yes C22 . C23 . H231 . 119.5(2) no C22 5_454 C23 . H231 . 119.5(2) no O9 . C24 . C25 . 121.0(4) yes O9 . C24 . C26 . 121.7(4) yes C25 . C24 . C26 . 117.3(4) yes C24 . C25 . H251 . 109.5(5) no C24 . C25 . H252 . 109.5(4) no H251 . C25 . H252 . 109.5(4) no C24 . C25 . H253 . 109.5(3) no H251 . C25 . H253 . 109.5(4) no H252 . C25 . H253 . 109.5(6) no C24 . C26 . H261 . 109.5(5) no C24 . C26 . H262 . 109.5(4) no H261 . C26 . H262 . 109.5(4) no C24 . C26 . H263 . 109.5(4) no H261 . C26 . H263 . 109.5(4) no H262 . C26 . H263 . 109.5(6) no O10 . C27 . C28 . 120.7(8) yes O10 . C27 . C29 . 121.9(8) yes C28 . C27 . C29 . 117.4(8) yes O10 . C27 . C30 . 159.7(4) yes C28 . C27 . C30 . 65.9(13) yes C29 . C27 . C30 . 55.6(12) yes O10 . C27 . C31 . 116.9(14) yes C28 . C27 . C31 . 5.6(8) yes C29 . C27 . C31 . 121.1(14) yes C30 . C27 . C31 . 68.0(12) yes O10 . C27 . C32 . 113.4(13) yes C28 . C27 . C32 . 125.8(13) yes C29 . C27 . C32 . 8.5(13) yes C30 . C27 . C32 . 62.9(11) yes C31 . C27 . C32 . 129.4(17) yes O10 . C27 . H311 . 75.9(11) no C28 . C27 . H311 . 50.0(10) no C29 . C27 . H311 . 152.5(8) no C30 . C27 . H311 . 115.4(14) no C31 . C27 . H311 . 48.9(10) no O10 . C27 . H321 . 78.3(10) no C28 . C27 . H321 . 152.4(8) no C29 . C27 . H321 . 48.2(10) no C30 . C27 . H321 . 103.6(12) no C31 . C27 . H321 . 158.0(9) no C32 . C27 . H311 . 157.6(6) no C32 . C27 . H321 . 41.6(8) no H311 . C27 . H321 . 128.9(7) no C27 . C28 . C30 . 53.0(10) yes C27 . C28 . C31 . 35.1(66) yes C30 . C28 . C31 . 70.8(82) yes C27 . C28 . H281 . 109.5(16) no C30 . C28 . H281 . 60.1(12) no C31 . C28 . H281 . 129.7(90) no C27 . C28 . H282 . 109.5(11) no C30 . C28 . H282 . 108.1(8) no C31 . C28 . H282 . 75.2(59) no H281 . C28 . H282 . 109.5(13) no C27 . C28 . H283 . 109.5(11) no C30 . C28 . H283 . 142.3(13) no C31 . C28 . H283 . 115.8(84) no H281 . C28 . H283 . 109.5(13) no H282 . C28 . H283 . 109.5(22) no C27 . C28 . H311 . 46.1(8) no C30 . C28 . H311 . 98.8(14) no C31 . C28 . H311 . 48.7(67) no H281 . C28 . H311 . 145.3(17) no H282 . C28 . H311 . 103.1(19) no C27 . C28 . H312 . 98.0(10) no C30 . C28 . H312 . 101.3(8) no C31 . C28 . H312 . 63.8(58) no H281 . C28 . H312 . 114.7(12) no H282 . C28 . H312 . 11.50(15) no C27 . C28 . H313 . 139.6(11) no C30 . C28 . H313 . 119.6(24) no C31 . C28 . H313 . 164.0(83) no H281 . C28 . H313 . 63.9(15) no H282 . C28 . H313 . 110.1(19) no H283 . C28 . H311 . 69.2(11) no H283 . C28 . H312 . 115.0(22) no H311 . C28 . H312 . 95.3(17) no H283 . C28 . H313 . 48.3(7) no H311 . C28 . H313 . 115.5(12) no H312 . C28 . H313 . 121.5(20) no C27 . C29 . C30 . 56.8(11) yes C27 . C29 . C32 . 88.2(81) yes C30 . C29 . C32 . 133.4(60) yes C27 . C29 . H291 . 109.5(16) no C30 . C29 . H291 . 57.4(13) no C32 . C29 . H291 . 160.4(87) no C27 . C29 . H292 . 109.5(11) no C30 . C29 . H292 . 105.3(8) no C32 . C29 . H292 . 54.7(54) no H291 . C29 . H292 . 109.5(14) no C27 . C29 . H293 . 109.5(11) no C30 . C29 . H293 . 145.2(15) no C32 . C29 . H293 . 70.6(41) no H291 . C29 . H293 . 109.5(14) no H292 . C29 . H293 . 109.5(22) no C27 . C29 . H321 . 55.8(8) no C30 . C29 . H321 . 112.5(16) no C32 . C29 . H321 . 47.7(72) no H291 . C29 . H321 . 150.5(14) no H292 . C29 . H321 . 99.9(21) no C27 . C29 . H322 . 107.8(11) no C30 . C29 . H322 . 112.1(5) no C32 . C29 . H322 . 45.8(55) no H291 . C29 . H322 . 117.8(12) no H292 . C29 . H322 . 9.0(3) no C27 . C29 . H323 . 142.8(6) no C30 . C29 . H323 . 128.3(24) no C32 . C29 . H323 . 98.2(65) no H291 . C29 . H323 . 73.0(14) no H292 . C29 . H323 . 104.0(17) no H293 . C29 . H321 . 61.3(11) no H293 . C29 . H322 . 102.5(21) no H321 . C29 . H322 . 91.6(18) no H293 . C29 . H323 . 41.8(5) no H321 . C29 . H323 . 103.1(14) no H322 . C29 . H323 . 102.7(17) no C27 . C30 . C28 . 61.1(10) yes C27 . C30 . C29 . 67.6(12) yes C28 . C30 . C29 . 124.0(15) yes C27 . C30 . O11 . 168.8(6) yes C28 . C30 . O11 . 116.3(13) yes C29 . C30 . O11 . 118.3(14) yes C27 . C30 . C31 . 54.6(12) yes C28 . C30 . C31 . 8.1(10) yes C29 . C30 . C31 . 119.8(14) yes O11 . C30 . C31 . 121.6(8) yes C27 . C30 . C32 . 63.5(13) yes C28 . C30 . C32 . 121.9(12) yes C29 . C30 . C32 . 6.2(10) yes O11 . C30 . C32 . 121.4(8) yes C31 . C30 . C32 . 117.0(7) yes C27 . C30 . H291 . 110.1(12) no C28 . C30 . H291 . 139.0(5) no C29 . C30 . H291 . 47.2(10) no O11 . C30 . H291 . 79.1(9) no C31 . C30 . H291 . 142.9(6) no C32 . C30 . H291 . 53.0(8) no C27 . C31 . C28 . 139.4(71) yes C27 . C31 . C30 . 57.4(11) yes C28 . C31 . C30 . 101.2(87) yes C27 . C31 . H281 . 112.2(15) no C28 . C31 . H281 . 41.9(81) no C30 . C31 . H281 . 60.3(7) no C27 . C31 . H282 . 127.4(8) no C28 . C31 . H282 . 92.2(70) no C30 . C31 . H282 . 114.6(12) no H281 . C31 . H282 . 100.4(20) no C27 . C31 . H283 . 115.0(17) no C28 . C31 . H283 . 54.0(69) no C30 . C31 . H283 . 135.9(6) no H281 . C31 . H283 . 92.2(7) no H282 . C31 . H283 . 103.2(15) no C27 . C31 . H311 . 53.4(12) no C28 . C31 . H311 . 121.8(66) no C30 . C31 . H311 . 109.5(15) no H281 . C31 . H311 . 141.8(11) no H282 . C31 . H311 . 116.2(13) no C27 . C31 . H312 . 114.6(9) no C28 . C31 . H312 . 104.8(71) no C30 . C31 . H312 . 109.5(10) no H281 . C31 . H312 . 108.6(20) no H282 . C31 . H312 . 12.81(15) no C27 . C31 . H313 . 135.9(12) no C28 . C31 . H313 . 12.5(63) no C30 . C31 . H313 . 109.5(10) no H281 . C31 . H313 . 52.6(7) no H282 . C31 . H313 . 96.7(18) no H283 . C31 . H311 . 69.9(11) no H283 . C31 . H312 . 112.0(15) no H311 . C31 . H312 . 109.5(12) no H283 . C31 . H313 . 41.5(4) no H311 . C31 . H313 . 109.5(12) no H312 . C31 . H313 . 109.5(20) no C27 . C32 . C29 . 83.2(80) yes C27 . C32 . C30 . 53.6(10) yes C29 . C32 . C30 . 40.4(55) yes C27 . C32 . H291 . 97.8(13) no C29 . C32 . H291 . 16.1(73) no C30 . C32 . H291 . 49.3(6) no C27 . C32 . H292 . 116.0(9) no C29 . C32 . H292 . 113.6(66) no C30 . C32 . H292 . 99.9(11) no H291 . C32 . H292 . 100.9(19) no C27 . C32 . H293 . 111.9(17) no C29 . C32 . H293 . 96.7(28) no C30 . C32 . H293 . 130.2(8) no H291 . C32 . H293 . 97.5(7) no H292 . C32 . H293 . 125.1(20) no C27 . C32 . H321 . 56.9(12) no C29 . C32 . H321 . 122.9(77) no C30 . C32 . H321 . 109.5(15) no H291 . C32 . H321 . 138.0(14) no H292 . C32 . H321 . 119.8(12) no C27 . C32 . H322 . 116.0(9) no C29 . C32 . H322 . 125.1(68) no C30 . C32 . H322 . 109.5(10) no H291 . C32 . H322 . 111.9(19) no H292 . C32 . H322 . 11.52(15) no C27 . C32 . H323 . 134.5(12) no C29 . C32 . H323 . 69.1(55) no C30 . C32 . H323 . 109.5(10) no H291 . C32 . H323 . 62.3(8) no H292 . C32 . H323 . 108.1(22) no H293 . C32 . H321 . 68.3(12) no H293 . C32 . H322 . 118.1(17) no H321 . C32 . H322 . 109.5(12) no H293 . C32 . H323 . 41.7(4) no H321 . C32 . H323 . 109.5(12) no H322 . C32 . H323 . 109.5(20) no C28 . H281 . C31 . 8.4(13) no C28 . H282 . C31 . 12.7(15) no C28 . H282 . H312 . 104.5(10) no C31 . H282 . H312 . 92.0(9) no C28 . H283 . C31 . 10.2(18) no C28 . H283 . H313 . 51.0(12) no C31 . H283 . H313 . 61.2(10) no C29 . H291 . C30 . 75.4(12) no C29 . H291 . C32 . 3.5(16) no C30 . H291 . C32 . 77.7(8) no C29 . H292 . C32 . 11.7(20) no C29 . H292 . H322 . 125.7(13) no C32 . H292 . H322 . 114.1(11) no C29 . H293 . C32 . 12.7(17) no C29 . H293 . H323 . 64.8(12) no C32 . H293 . H323 . 73.0(13) no C27 . H311 . C28 . 83.9(11) no C27 . H311 . C31 . 77.6(12) no C28 . H311 . C31 . 9.5(7) no C28 . H312 . C31 . 11.4(16) no C28 . H312 . H282 . 64.0(9) no C31 . H312 . H282 . 75.2(10) no C28 . H313 . C31 . 3.5(20) no C28 . H313 . H283 . 80.7(15) no C31 . H313 . H283 . 77.3(11) no C27 . H321 . C29 . 76.0(10) no C27 . H321 . C32 . 81.5(12) no C29 . H321 . C32 . 9.4(14) no C29 . H322 . C32 . 9.1(18) no C29 . H322 . H292 . 45.3(11) no C32 . H322 . H292 . 54.4(11) no C29 . H323 . C32 . 12.7(20) no C29 . H323 . H293 . 73.4(12) no C32 . H323 . H293 . 65.3(12) no data_CRYSTALS_cif_2 _database_code_CSD 162980 _audit_creation_date 01-22-03 _audit_creation_method CRYSTALS_ver_12-03-99 # # 1. SUBMISSION DETAILS _publ_contact_letter ; ; _publ_contact_author_name 'Lowe, Gordon' _publ_contact_author_address ; The Dyson Perrins Laboratory, Department of Chemistry, Oxford University, South Parks Road, Oxford OX1 3QY ; _publ_contact_author_phone ' 01865 275 649 ' _publ_contact_author_fax ' 01865 275 674 ' _publ_contact_author_email ' gordon.lowe@chem.ox.ac.uk ' #============================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_coden_ASTM ? _journal_name_full 'Chemical Communications' _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; The X-ray structure of N,S-bis-[4'-chloro-2,2',2"-terpyridine platinum (II)] 2-mercaptoimidazole tris-fluorophosphate and tris-[2,2':6',2"-terpyridine platinum (II)] sulfonium perchlorate ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address _publ_author_footnote 'Lowe, Gordon' ; The Dyson Perrins Laboratory, Department of Chemistry, Oxford University, South Parks Road, Oxford OX1 3QY ; ; ? #footnote for author 1 ; 'Ross, Steven. A.' ; The Dyson Perrins Laboratory, Department of Chemistry, Oxford University, South Parks Road, Oxford OX1 3QY ; ; ? # footnote 2 ; 'Probert, Michael. R.' ; Chemical Crystallography, Department of Chemistry, Oxford University, 9 Parks Road, Oxford OX1 3PD ; ; ? # footnote 2 ; 'Cowley, Andrew. R.' ; Chemical Crystallography, Department of Chemistry, Oxford University, 9 Parks Road, Oxford OX1 3PD ; ; ? # footnote 2 ; #============================================================================== # 4. TEXT _publ_section_abstract #Text of the abstract ; ? ; _publ_section_comment #Text of the paper ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions #Captions to figures ; ? ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen for refinement keywords. ; H atoms placed geometrically after each cycle ; _publ_section_exptl_prep ; ? ; #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point 'not measured' # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment noref #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et all 200 ; _computing_publication_material ; CRYSTALS (Watkin et all 200 ; _computing_molecular_graphics ; CAMERON (Watkin et al 1996) ; #============================================================= _cell_length_a 11.9306(1) _cell_angle_alpha 97.1106(5) _cell_length_b 14.3873(2) _cell_angle_beta 112.5601(5) _cell_length_c 15.3729(2) _cell_angle_gamma 109.7985(5) _cell_volume 2192.8 _symmetry_cell_setting 'Triclinic ' _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-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 ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International_Tables_Vol_IV_Table_2.2B' 'F ' 0.0140 0.0100 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International_Tables_Vol_IV_Table_2.2B' 'Pt ' -2.3520 8.3880 27.0059 1.5129 17.7639 8.8117 15.7131 0.4246 5.7837 38.6103 11.6883 'International_Tables_Vol_IV_Table_2.2B' 'S ' 0.1100 0.1240 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C33 H23 Cl2 F18 N8 O2 P3 Pt2 S1 ' _chemical_formula_moiety ' C33 H23 Cl2 F18 N8 O2 P3 Pt2 S1 ' _chemical_compound_source ; ? ; _chemical_formula_weight 1491.63 _cell_measurement_reflns_used 8443 _cell_measurement_theta_min 4 _cell_measurement_theta_max 26 _cell_measurement_temperature 190 _cell_formula_units_Z 2 _exptl_crystal_description ' block ' _exptl_crystal_colour ' red ' _exptl_crystal_size_min 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.30 _exptl_crystal_density_diffrn 2.259 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1404.710 _exptl_absorpt_coefficient_mu 6.773 # Sheldrick geometric definitions 0.26 0.26 _diffrn_measurement_device_type ; Enraf Nonius Kappa CCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; COLLECT (Nonius BV, 1997) ; _computing_data_reduction ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.23 _exptl_absorpt_correction_T_max 0.26 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 190 _diffrn_reflns_number 8930 _reflns_number_total 8930 _diffrn_reflns_av_R_equivalents 0.00 # Number of reflections with Friedels Law is 8930 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 9006 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_gt 7689 _diffrn_reflns_theta_min 4.08 _diffrn_reflns_theta_max 26.41 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _reflns_limit_h_min -14 _reflns_limit_h_max 13 _reflns_limit_k_min -17 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 19 _refine_diff_density_min -1.48 _refine_diff_density_max 1.49 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 7689 _refine_ls_number_parameters 622 _refine_ls_R_factor_gt 0.0302 _refine_ls_wR_factor_ref 0.0375 _refine_ls_goodness_of_fit_ref 1.0083 _refine_ls_shift/su_max 0.008716 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 0.928 0.532 0.651 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 COLLECT Software, Nonius BV 1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Watkin, D.J., Prout, C.K., Carruthers, J.R., Betteridge, P.W. & Cooper R.I. (2001) CRYSTALS Issue 11. Chemical Crystallography Laboratory, OXFORD, UK. 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 loop_ _atom_site_label _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 Pt1 0.091865(15) 0.050087(13) 0.119712(11) 0.0255 1.0000 Uani Pt2 0.195145(15) 0.183962(12) 0.346612(11) 0.0258 1.0000 Uani Cl1 0.74324(14) 0.51655(12) 0.39637(14) 0.0600 1.0000 Uani Cl2 0.64216(16) 0.08516(16) 0.12653(15) 0.0694 1.0000 Uani S1 -0.10611(11) 0.0374(1) 0.12068(8) 0.0348 1.0000 Uani P1 0.08469(16) 0.74857(12) 0.45923(13) 0.0515 1.0000 Uani P2 0.52562(14) 0.74208(9) 0.3346(1) 0.0386 1.0000 Uani P3 0.76992(17) 0.38530(13) 0.06353(13) 0.0548 1.0000 Uani F1 0.2037(4) 0.7403(3) 0.4386(4) 0.0694 1.0000 Uani F2 0.0336(7) 0.7834(8) 0.3628(5) 0.1435 1.0000 Uani F3 0.1751(7) 0.8716(4) 0.5032(6) 0.1144 1.0000 Uani F4 0.1571(8) 0.742(1) 0.5634(7) 0.1987 1.0000 Uani F5 0.0016(8) 0.6383(4) 0.4092(11) 0.2551 1.0000 Uani F6 -0.0313(4) 0.7557(4) 0.4822(3) 0.0732 1.0000 Uani F7 0.6477(5) 0.7274(4) 0.3288(4) 0.0889 1.0000 Uani F8 0.4280(4) 0.6319(3) 0.2559(3) 0.0703 1.0000 Uani F9 0.5370(5) 0.6881(3) 0.4204(3) 0.0705 1.0000 Uani F10 0.4021(5) 0.7567(4) 0.3377(5) 0.0921 1.0000 Uani F11 0.5124(5) 0.7977(3) 0.2503(3) 0.0789 1.0000 Uani F12 0.6267(4) 0.8514(3) 0.4139(3) 0.0583 1.0000 Uani F13 0.7258(5) 0.3564(4) 0.1444(4) 0.0838 1.0000 Uani F14 0.6539(5) 0.2749(4) -0.0135(4) 0.0865 1.0000 Uani F15 0.8691(5) 0.3323(4) 0.0944(4) 0.0847 1.0000 Uani F16 0.8096(7) 0.4113(5) -0.0204(4) 0.1101 1.0000 Uani F17 0.8831(6) 0.4915(4) 0.1409(4) 0.0971 1.0000 Uani F18 0.6678(7) 0.4371(5) 0.0302(5) 0.1157 1.0000 Uani O1 0.6266(5) 0.7634(4) 0.0929(4) 0.0737 1.0000 Uani O2 0.6841(12) 0.6114(8) 0.1716(7) 0.1578 1.0000 Uani N1 0.2998(4) 0.0965(3) 0.3647(3) 0.0322 1.0000 Uani N2 0.3635(4) 0.2869(3) 0.3659(3) 0.0272 1.0000 Uani N3 0.1473(4) 0.3057(3) 0.3415(3) 0.0331 1.0000 Uani N4 0.0776(4) -0.0935(3) 0.1286(3) 0.0346 1.0000 Uani N5 0.2599(4) 0.0608(3) 0.1203(3) 0.0314 1.0000 Uani N6 0.1629(4) 0.1977(3) 0.1118(3) 0.0311 1.0000 Uani N7 0.0187(4) 0.0736(3) 0.3223(3) 0.0326 1.0000 Uani N8 -0.1792(4) -0.0557(3) 0.2462(3) 0.0408 1.0000 Uani C1 0.2597(5) -0.0017(4) 0.3667(3) 0.0378 1.0000 Uani C2 0.3422(6) -0.0530(4) 0.3757(4) 0.0450 1.0000 Uani C3 0.4648(6) -0.0032(4) 0.3817(4) 0.0462 1.0000 Uani C4 0.5097(5) 0.1006(4) 0.3824(4) 0.0380 1.0000 Uani C5 0.4259(5) 0.1480(3) 0.3745(3) 0.0336 1.0000 Uani C6 0.4645(5) 0.2583(4) 0.3763(3) 0.0324 1.0000 Uani C7 0.5836(5) 0.3280(4) 0.3860(4) 0.0352 1.0000 Uani C8 0.5947(5) 0.4268(4) 0.3842(4) 0.0397 1.0000 Uani C9 0.4916(5) 0.4559(4) 0.3739(4) 0.0377 1.0000 Uani C10 0.3744(5) 0.3830(3) 0.3648(3) 0.0335 1.0000 Uani C11 0.2512(5) 0.3944(4) 0.3534(4) 0.0350 1.0000 Uani C12 0.2373(6) 0.4853(4) 0.3528(4) 0.0416 1.0000 Uani C13 0.1161(6) 0.4883(4) 0.3417(5) 0.0504 1.0000 Uani C14 0.0151(6) 0.3997(5) 0.3325(4) 0.0483 1.0000 Uani C15 0.0328(5) 0.3093(4) 0.3326(4) 0.0387 1.0000 Uani C16 -0.0186(5) -0.1689(4) 0.1362(4) 0.0399 1.0000 Uani C17 -0.0144(7) -0.2624(5) 0.1453(4) 0.0518 1.0000 Uani C18 0.0931(7) -0.2788(5) 0.1462(5) 0.0549 1.0000 Uani C19 0.1921(7) -0.2031(5) 0.1373(4) 0.0506 1.0000 Uani C20 0.1853(5) -0.1096(4) 0.1296(3) 0.0360 1.0000 Uani C21 0.2885(5) -0.0223(4) 0.1255(3) 0.0370 1.0000 Uani C22 0.4088(5) -0.0163(5) 0.1278(4) 0.0451 1.0000 Uani C23 0.4919(5) 0.0748(5) 0.1237(4) 0.0473 1.0000 Uani C24 0.4605(5) 0.1596(5) 0.1181(4) 0.0447 1.0000 Uani C25 0.3406(5) 0.1508(4) 0.1163(3) 0.0344 1.0000 Uani C26 0.2859(5) 0.2288(4) 0.1119(3) 0.0359 1.0000 Uani C27 0.3506(6) 0.3269(4) 0.1089(4) 0.0476 1.0000 Uani C28 0.2911(7) 0.3956(4) 0.1062(5) 0.0523 1.0000 Uani C29 0.1697(7) 0.3638(5) 0.1055(4) 0.0503 1.0000 Uani C30 0.1066(5) 0.2641(4) 0.1086(4) 0.0385 1.0000 Uani C31 -0.0116(6) 0.0337(5) 0.3917(4) 0.0547 1.0000 Uani C32 -0.1341(6) -0.0466(5) 0.3445(4) 0.0579 1.0000 Uani C33 -0.0853(4) 0.0188(3) 0.2344(3) 0.0291 1.0000 Uani H11 0.1688 -0.0391 0.3617 0.0393 1.0000 Uiso H21 0.3110 -0.1262 0.3776 0.0479 1.0000 Uiso H31 0.5232 -0.0403 0.3856 0.0549 1.0000 Uiso H41 0.6010 0.1391 0.3885 0.0437 1.0000 Uiso H71 0.6591 0.3084 0.3942 0.0416 1.0000 Uiso H81 -0.2668 -0.1086 0.1922 0.0427 1.0000 Uiso H91 0.5023 0.5277 0.3731 0.0439 1.0000 Uiso H121 0.3128 0.5489 0.3602 0.0504 1.0000 Uiso H131 0.1038 0.5536 0.3404 0.0642 1.0000 Uiso H141 -0.0713 0.4003 0.3258 0.0609 1.0000 Uiso H151 -0.0418 0.2453 0.3257 0.0478 1.0000 Uiso H161 -0.0969 -0.1570 0.1354 0.0473 1.0000 Uiso H171 -0.0879 -0.3167 0.1510 0.0614 1.0000 Uiso H181 0.0992 -0.3453 0.1532 0.0637 1.0000 Uiso H191 0.2694 -0.2153 0.1364 0.0620 1.0000 Uiso H221 0.4336 -0.0759 0.1322 0.0562 1.0000 Uiso H241 0.5231 0.2250 0.1156 0.0534 1.0000 Uiso H271 0.4394 0.3487 0.1086 0.0559 1.0000 Uiso H281 0.3373 0.4675 0.1048 0.0622 1.0000 Uiso H291 0.1256 0.4121 0.1028 0.0658 1.0000 Uiso H301 0.0174 0.2418 0.1084 0.0488 1.0000 Uiso H311 0.0470 0.0597 0.4645 0.0576 1.0000 Uiso H321 -0.1824 -0.0907 0.3756 0.0601 1.0000 Uiso 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 0.02220(9) 0.0365(1) 0.02129(9) 0.00966(7) 0.01167(7) 0.01362(7) Pt2 0.0236(1) 0.02409(9) 0.02298(9) 0.00720(6) 0.01019(7) 0.00288(7) Cl1 0.0313(6) 0.0514(8) 0.0893(11) 0.0347(8) 0.0258(7) 0.0054(6) Cl2 0.0403(8) 0.0969(13) 0.0886(12) 0.026(1) 0.0387(8) 0.0379(8) S1 0.0251(5) 0.0554(7) 0.0285(5) 0.0162(5) 0.0133(4) 0.0193(5) P1 0.0483(8) 0.0516(8) 0.071(1) 0.0194(7) 0.0392(8) 0.0247(7) P2 0.0414(7) 0.0298(6) 0.0431(7) 0.0103(5) 0.0193(6) 0.0135(5) P3 0.0518(9) 0.0527(8) 0.0585(9) 0.0171(7) 0.0221(8) 0.0238(7) F1 0.061(2) 0.0519(19) 0.113(3) 0.016(2) 0.066(2) 0.0174(17) F2 0.109(5) 0.233(9) 0.119(5) 0.088(6) 0.066(4) 0.077(6) F3 0.131(5) 0.079(3) 0.177(6) 0.032(4) 0.110(5) 0.050(3) F4 0.154(6) 0.454(16) 0.196(7) 0.25(1) 0.148(6) 0.226(9) F5 0.153(6) 0.054(3) 0.56(2) -0.064(6) 0.266(11) -0.025(3) F6 0.060(2) 0.104(3) 0.086(3) 0.030(2) 0.046(2) 0.051(2) F7 0.072(3) 0.072(3) 0.139(4) 0.015(3) 0.062(3) 0.038(2) F8 0.079(3) 0.0438(19) 0.055(2) 0.0032(16) 0.018(2) 0.0069(18) F9 0.098(3) 0.0412(18) 0.049(2) 0.0198(15) 0.024(2) 0.0122(19) F10 0.067(3) 0.076(3) 0.150(5) 0.024(3) 0.065(3) 0.034(2) F11 0.093(3) 0.065(2) 0.065(3) 0.034(2) 0.029(2) 0.021(2) F12 0.065(2) 0.0361(16) 0.056(2) 0.0081(15) 0.0206(18) 0.0114(16) F13 0.080(3) 0.087(3) 0.084(3) 0.023(2) 0.048(3) 0.024(2) F14 0.063(3) 0.086(3) 0.076(3) -0.006(2) 0.011(2) 0.028(2) F15 0.069(3) 0.089(3) 0.095(3) 0.023(3) 0.024(3) 0.049(3) F16 0.156(6) 0.113(4) 0.095(4) 0.050(3) 0.079(4) 0.062(4) F17 0.095(4) 0.057(2) 0.108(4) 0.016(3) 0.039(3) 0.008(2) F18 0.130(5) 0.124(5) 0.117(4) 0.040(4) 0.039(4) 0.098(4) O1 0.055(3) 0.077(3) 0.056(3) -0.000(2) 0.025(2) -0.003(2) O2 0.209(11) 0.175(9) 0.124(7) 0.028(6) 0.071(7) 0.129(9) N1 0.0304(19) 0.0290(18) 0.0280(18) 0.0101(15) 0.0081(15) 0.0076(15) N2 0.0248(17) 0.0259(17) 0.0248(17) 0.0082(14) 0.0090(14) 0.0063(14) N3 0.030(2) 0.0342(19) 0.0327(19) 0.0090(16) 0.0145(16) 0.0115(16) N4 0.037(2) 0.040(2) 0.0253(18) 0.0072(16) 0.0151(17) 0.0154(17) N5 0.0281(19) 0.045(2) 0.0249(17) 0.0088(15) 0.0134(15) 0.0182(17) N6 0.033(2) 0.037(2) 0.0260(18) 0.0105(15) 0.0155(16) 0.0156(16) N7 0.0276(19) 0.0327(19) 0.0308(19) 0.0095(15) 0.0142(16) 0.0042(15) N8 0.027(2) 0.041(2) 0.039(2) 0.0089(18) 0.0143(17) -0.0012(17) C1 0.040(3) 0.029(2) 0.029(2) 0.0099(18) 0.010(2) 0.0042(19) C2 0.054(3) 0.029(2) 0.037(3) 0.008(2) 0.011(2) 0.012(2) C3 0.053(3) 0.045(3) 0.040(3) 0.013(2) 0.016(2) 0.024(2) C4 0.036(2) 0.036(2) 0.037(2) 0.0089(19) 0.012(2) 0.016(2) C5 0.034(2) 0.028(2) 0.033(2) 0.0108(18) 0.0121(19) 0.0104(18) C6 0.030(2) 0.033(2) 0.032(2) 0.0118(18) 0.0119(18) 0.0108(18) C7 0.030(2) 0.035(2) 0.039(2) 0.015(2) 0.014(2) 0.0120(19) C8 0.025(2) 0.036(2) 0.044(3) 0.012(2) 0.012(2) 0.0016(19) C9 0.033(2) 0.032(2) 0.045(3) 0.014(2) 0.017(2) 0.0092(19) C10 0.034(2) 0.030(2) 0.030(2) 0.0072(17) 0.0131(19) 0.0090(18) C11 0.033(2) 0.032(2) 0.035(2) 0.0086(18) 0.015(2) 0.0095(19) C12 0.046(3) 0.035(2) 0.046(3) 0.012(2) 0.021(2) 0.018(2) C13 0.058(3) 0.044(3) 0.058(3) 0.018(3) 0.029(3) 0.028(3) C14 0.040(3) 0.062(3) 0.050(3) 0.015(3) 0.024(3) 0.026(3) C15 0.035(2) 0.044(3) 0.041(3) 0.011(2) 0.023(2) 0.014(2) C16 0.037(3) 0.042(3) 0.039(3) 0.008(2) 0.021(2) 0.012(2) C17 0.063(4) 0.044(3) 0.047(3) 0.016(2) 0.026(3) 0.019(3) C18 0.065(4) 0.044(3) 0.051(3) 0.014(3) 0.022(3) 0.022(3) C19 0.058(4) 0.054(3) 0.042(3) 0.012(2) 0.019(3) 0.033(3) C20 0.040(3) 0.040(3) 0.028(2) 0.0066(19) 0.014(2) 0.020(2) C21 0.036(2) 0.054(3) 0.025(2) 0.010(2) 0.0114(19) 0.025(2) C22 0.035(3) 0.065(3) 0.040(3) 0.014(2) 0.017(2) 0.028(3) C23 0.034(3) 0.077(4) 0.040(3) 0.012(3) 0.019(2) 0.032(3) C24 0.031(2) 0.063(3) 0.040(3) 0.013(2) 0.021(2) 0.014(2) C25 0.029(2) 0.051(3) 0.023(2) 0.0089(19) 0.0133(18) 0.016(2) C26 0.031(2) 0.049(3) 0.028(2) 0.0130(19) 0.0157(19) 0.014(2) C27 0.045(3) 0.048(3) 0.048(3) 0.011(2) 0.026(3) 0.011(2) C28 0.065(4) 0.042(3) 0.049(3) 0.017(2) 0.028(3) 0.017(3) C29 0.071(4) 0.050(3) 0.043(3) 0.020(2) 0.030(3) 0.033(3) C30 0.044(3) 0.047(3) 0.032(2) 0.013(2) 0.020(2) 0.023(2) C31 0.050(3) 0.058(3) 0.036(3) 0.017(2) 0.022(2) -0.004(3) C32 0.047(3) 0.063(4) 0.040(3) 0.018(3) 0.021(3) -0.005(3) C33 0.025(2) 0.035(2) 0.027(2) 0.0079(17) 0.0145(17) 0.0080(17) _refine_ls_extinction_method 'None' 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 . Pt1 2_555 3.2841(3) yes Pt1 . Pt2 . 3.2903(2) yes Pt1 . S1 . 2.3126(11) yes Pt1 . N4 . 2.041(4) yes Pt1 . N5 . 1.954(4) yes Pt1 . N6 . 2.042(4) yes Pt2 . N1 . 2.025(4) yes Pt2 . N2 . 1.933(3) yes Pt2 . N3 . 2.019(4) yes Pt2 . N7 . 2.019(4) yes Cl1 . C8 . 1.725(5) yes Cl2 . C23 . 1.731(5) yes S1 . C33 . 1.737(4) yes P1 . F1 . 1.607(4) yes P1 . F2 . 1.587(7) yes P1 . F3 . 1.614(6) yes P1 . F4 . 1.536(7) yes P1 . F5 . 1.462(5) yes P1 . F6 . 1.585(4) yes P2 . F7 . 1.575(4) yes P2 . F8 . 1.590(4) yes P2 . F9 . 1.597(4) yes P2 . F10 . 1.574(4) yes P2 . F11 . 1.591(4) yes P2 . F12 . 1.590(3) yes P3 . F13 . 1.573(5) yes P3 . F14 . 1.621(5) yes P3 . F15 . 1.574(4) yes P3 . F16 . 1.581(6) yes P3 . F17 . 1.579(5) yes P3 . F18 . 1.591(5) yes N1 . C1 . 1.339(6) yes N1 . C5 . 1.371(6) yes N2 . C6 . 1.360(6) yes N2 . C10 . 1.347(6) yes N3 . C11 . 1.377(6) yes N3 . C15 . 1.339(6) yes N4 . C16 . 1.341(7) yes N4 . C20 . 1.375(7) yes N5 . C21 . 1.353(6) yes N5 . C25 . 1.352(6) yes N6 . C26 . 1.381(6) yes N6 . C30 . 1.338(6) yes N7 . C31 . 1.380(6) yes N7 . C33 . 1.332(6) yes N8 . C32 . 1.367(7) yes N8 . C33 . 1.352(6) yes N8 . H81 . 1.000(4) no C1 . C2 . 1.395(8) yes C1 . H11 . 1.000(5) no C2 . C3 . 1.353(9) yes C2 . H21 . 1.000(5) no C3 . C4 . 1.403(8) yes C3 . H31 . 1.000(6) no C4 . C5 . 1.367(7) yes C4 . H41 . 1.000(5) no C5 . C6 . 1.488(6) yes C6 . C7 . 1.372(7) yes C7 . C8 . 1.388(7) yes C7 . H71 . 1.000(5) no C8 . C9 . 1.388(8) yes C9 . C10 . 1.377(7) yes C9 . H91 . 1.000(5) no C10 . C11 . 1.479(7) yes C11 . C12 . 1.375(7) yes C12 . C13 . 1.405(8) yes C12 . H121 . 1.000(5) no C13 . C14 . 1.372(9) yes C13 . H131 . 1.000(5) no C14 . C15 . 1.386(8) yes C14 . H141 . 1.000(5) no C15 . H151 . 1.000(5) no C16 . C17 . 1.385(8) yes C16 . H161 . 1.000(5) no C17 . C18 . 1.38(1) yes C17 . H171 . 1.000(6) no C18 . C19 . 1.374(9) yes C18 . H181 . 1.000(6) no C19 . C20 . 1.393(8) yes C19 . H191 . 1.000(6) no C20 . C21 . 1.459(7) yes C21 . C22 . 1.394(7) yes C22 . C23 . 1.375(9) yes C22 . H221 . 1.000(6) no C23 . C24 . 1.396(9) yes C24 . C25 . 1.381(7) yes C24 . H241 . 1.000(6) no C25 . C26 . 1.473(7) yes C26 . C27 . 1.377(8) yes C27 . C28 . 1.395(9) yes C27 . H271 . 1.000(6) no C28 . C29 . 1.359(9) yes C28 . H281 . 1.000(6) no C29 . C30 . 1.392(8) yes C29 . H291 . 1.000(6) no C30 . H301 . 1.000(5) no C31 . C32 . 1.354(8) yes C31 . H311 . 1.000(6) no C32 . H321 . 1.000(5) 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 Pt1 2_555 Pt1 . Pt2 . 159.339(8) yes Pt1 2_555 Pt1 . S1 . 84.76(3) yes Pt2 . Pt1 . S1 . 77.58(3) yes Pt1 2_555 Pt1 . N4 . 88.40(11) yes Pt2 . Pt1 . N4 . 104.80(11) yes S1 . Pt1 . N4 . 99.15(12) yes Pt1 2_555 Pt1 . N5 . 95.78(11) yes Pt2 . Pt1 . N5 . 101.93(11) yes S1 . Pt1 . N5 . 179.41(11) yes N4 . Pt1 . N5 . 80.64(17) yes Pt1 2_555 Pt1 . N6 . 93.8(1) yes Pt2 . Pt1 . N6 . 78.8(1) yes S1 . Pt1 . N6 . 99.30(11) yes N4 . Pt1 . N6 . 161.54(17) yes N5 . Pt1 . N6 . 80.90(16) yes Pt1 . Pt2 . N1 . 76.74(11) yes Pt1 . Pt2 . N2 . 98.08(11) yes N1 . Pt2 . N2 . 81.27(15) yes Pt1 . Pt2 . N3 . 108.45(11) yes N1 . Pt2 . N3 . 162.30(16) yes N2 . Pt2 . N3 . 81.24(16) yes Pt1 . Pt2 . N7 . 80.04(11) yes N1 . Pt2 . N7 . 97.88(16) yes N2 . Pt2 . N7 . 178.08(15) yes N3 . Pt2 . N7 . 99.68(16) yes Pt1 . S1 . C33 . 103.13(15) yes F1 . P1 . F2 . 89.8(3) yes F1 . P1 . F3 . 86.9(2) yes F2 . P1 . F3 . 79.5(5) yes F1 . P1 . F4 . 88.4(3) yes F2 . P1 . F4 . 166.6(6) yes F3 . P1 . F4 . 87.1(6) yes F1 . P1 . F5 . 90.7(3) yes F2 . P1 . F5 . 94.9(7) yes F3 . P1 . F5 . 173.9(6) yes F4 . P1 . F5 . 98.4(8) yes F1 . P1 . F6 . 178.4(3) yes F2 . P1 . F6 . 91.8(3) yes F3 . P1 . F6 . 93.4(3) yes F4 . P1 . F6 . 90.1(3) yes F5 . P1 . F6 . 89.2(3) yes F7 . P2 . F8 . 89.2(3) yes F7 . P2 . F9 . 91.6(3) yes F8 . P2 . F9 . 89.2(2) yes F7 . P2 . F10 . 178.6(3) yes F8 . P2 . F10 . 90.1(3) yes F9 . P2 . F10 . 89.6(3) yes F7 . P2 . F11 . 89.9(3) yes F8 . P2 . F11 . 91.6(2) yes F9 . P2 . F11 . 178.3(3) yes F10 . P2 . F11 . 88.9(3) yes F7 . P2 . F12 . 89.2(2) yes F8 . P2 . F12 . 178.4(2) yes F9 . P2 . F12 . 90.4(2) yes F10 . P2 . F12 . 91.4(3) yes F11 . P2 . F12 . 88.9(2) yes F13 . P3 . F14 . 89.0(3) yes F13 . P3 . F15 . 90.3(3) yes F14 . P3 . F15 . 88.6(3) yes F13 . P3 . F16 . 178.1(3) yes F14 . P3 . F16 . 89.1(3) yes F15 . P3 . F16 . 90.2(3) yes F13 . P3 . F17 . 89.6(3) yes F14 . P3 . F17 . 178.5(3) yes F15 . P3 . F17 . 90.7(3) yes F16 . P3 . F17 . 92.3(4) yes F13 . P3 . F18 . 90.1(3) yes F14 . P3 . F18 . 90.3(3) yes F15 . P3 . F18 . 178.8(3) yes F16 . P3 . F18 . 89.3(4) yes F17 . P3 . F18 . 90.4(4) yes Pt2 . N1 . C1 . 128.1(4) yes Pt2 . N1 . C5 . 112.9(3) yes C1 . N1 . C5 . 119.0(4) yes Pt2 . N2 . C6 . 118.6(3) yes Pt2 . N2 . C10 . 118.7(3) yes C6 . N2 . C10 . 122.7(4) yes Pt2 . N3 . C11 . 112.7(3) yes Pt2 . N3 . C15 . 127.9(3) yes C11 . N3 . C15 . 119.3(4) yes Pt1 . N4 . C16 . 128.4(4) yes Pt1 . N4 . C20 . 112.8(3) yes C16 . N4 . C20 . 118.8(4) yes Pt1 . N5 . C21 . 117.8(3) yes Pt1 . N5 . C25 . 118.1(3) yes C21 . N5 . C25 . 124.1(4) yes Pt1 . N6 . C26 . 112.6(3) yes Pt1 . N6 . C30 . 128.1(3) yes C26 . N6 . C30 . 119.2(4) yes Pt2 . N7 . C31 . 126.7(3) yes Pt2 . N7 . C33 . 125.6(3) yes C31 . N7 . C33 . 107.4(4) yes C32 . N8 . C33 . 108.5(4) yes C32 . N8 . H81 . 125.8(4) no C33 . N8 . H81 . 125.8(4) no N1 . C1 . C2 . 121.2(5) yes N1 . C1 . H11 . 119.4(5) no C2 . C1 . H11 . 119.4(5) no C1 . C2 . C3 . 119.7(5) yes C1 . C2 . H21 . 120.1(6) no C3 . C2 . H21 . 120.1(6) no C2 . C3 . C4 . 119.7(5) yes C2 . C3 . H31 . 120.1(5) no C4 . C3 . H31 . 120.1(6) no C3 . C4 . C5 . 118.5(5) yes C3 . C4 . H41 . 120.8(5) no C5 . C4 . H41 . 120.7(5) no N1 . C5 . C4 . 121.8(4) yes N1 . C5 . C6 . 115.4(4) yes C4 . C5 . C6 . 122.8(4) yes N2 . C6 . C5 . 111.7(4) yes N2 . C6 . C7 . 120.4(4) yes C5 . C6 . C7 . 127.9(4) yes C6 . C7 . C8 . 117.0(4) yes C6 . C7 . H71 . 121.5(5) no C8 . C7 . H71 . 121.5(5) no Cl1 . C8 . C7 . 118.3(4) yes Cl1 . C8 . C9 . 119.3(4) yes C7 . C8 . C9 . 122.4(4) yes C8 . C9 . C10 . 118.2(5) yes C8 . C9 . H91 . 120.9(5) no C10 . C9 . H91 . 120.9(5) no N2 . C10 . C9 . 119.3(5) yes N2 . C10 . C11 . 112.1(4) yes C9 . C10 . C11 . 128.6(4) yes N3 . C11 . C10 . 115.3(4) yes N3 . C11 . C12 . 120.9(5) yes C10 . C11 . C12 . 123.9(4) yes C11 . C12 . C13 . 119.6(5) yes C11 . C12 . H121 . 120.2(5) no C13 . C12 . H121 . 120.2(5) no C12 . C13 . C14 . 118.5(5) yes C12 . C13 . H131 . 120.7(6) no C14 . C13 . H131 . 120.7(6) no C13 . C14 . C15 . 120.1(5) yes C13 . C14 . H141 . 119.9(6) no C15 . C14 . H141 . 120.0(6) no N3 . C15 . C14 . 121.6(5) yes N3 . C15 . H151 . 119.2(5) no C14 . C15 . H151 . 119.2(5) no N4 . C16 . C17 . 122.9(5) yes N4 . C16 . H161 . 118.5(5) no C17 . C16 . H161 . 118.6(5) no C16 . C17 . C18 . 118.5(6) yes C16 . C17 . H171 . 120.7(6) no C18 . C17 . H171 . 120.7(6) no C17 . C18 . C19 . 119.5(6) yes C17 . C18 . H181 . 120.2(6) no C19 . C18 . H181 . 120.2(7) no C18 . C19 . C20 . 120.3(6) yes C18 . C19 . H191 . 119.8(6) no C20 . C19 . H191 . 119.9(6) no N4 . C20 . C19 . 120.0(5) yes N4 . C20 . C21 . 115.4(4) yes C19 . C20 . C21 . 124.6(5) yes N5 . C21 . C20 . 113.3(4) yes N5 . C21 . C22 . 119.1(5) yes C20 . C21 . C22 . 127.6(5) yes C21 . C22 . C23 . 117.4(5) yes C21 . C22 . H221 . 121.3(6) no C23 . C22 . H221 . 121.3(5) no Cl2 . C23 . C22 . 118.7(4) yes Cl2 . C23 . C24 . 118.6(5) yes C22 . C23 . C24 . 122.7(5) yes C23 . C24 . C25 . 118.1(5) yes C23 . C24 . H241 . 120.9(5) no C25 . C24 . H241 . 120.9(6) no N5 . C25 . C24 . 118.6(5) yes N5 . C25 . C26 . 113.0(4) yes C24 . C25 . C26 . 128.4(5) yes N6 . C26 . C25 . 115.4(4) yes N6 . C26 . C27 . 120.8(5) yes C25 . C26 . C27 . 123.8(5) yes C26 . C27 . C28 . 119.4(5) yes C26 . C27 . H271 . 120.3(6) no C28 . C27 . H271 . 120.3(6) no C27 . C28 . C29 . 119.1(5) yes C27 . C28 . H281 . 120.4(6) no C29 . C28 . H281 . 120.4(6) no C28 . C29 . C30 . 120.2(5) yes C28 . C29 . H291 . 119.9(6) no C30 . C29 . H291 . 119.9(6) no N6 . C30 . C29 . 121.2(5) yes N6 . C30 . H301 . 119.4(5) no C29 . C30 . H301 . 119.4(5) no N7 . C31 . C32 . 108.5(5) yes N7 . C31 . H311 . 125.8(5) no C32 . C31 . H311 . 125.8(5) no N8 . C32 . C31 . 106.7(4) yes N8 . C32 . H321 . 126.6(5) no C31 . C32 . H321 . 126.6(6) no S1 . C33 . N7 . 127.8(3) yes S1 . C33 . N8 . 123.2(3) yes N7 . C33 . N8 . 108.9(4) yes