# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1684 #=============================================================================== data_global #=============================================================================== _audit_creation_date 18-05-98 # 1. SUBMISSION DETAILS _publ_contact_author_name # Name of author for correspondance ; ; _publ_contact_author_address # Address of author for correspondance ; ; _publ_contact_author_phone 'xxxxxxxxxx' _publ_contact_author_fax 'xxxxxxxxxx' _publ_contact_author_email xxx@xx.xx.xx _publ_requested_journal 'J. Chem Soc., Dalton Trans' _publ_contact_letter ; Please consider this CIF submission for publication as a new structure paper in Acta Crystallographica Section C. The figures, chemical structure diagram (scheme), Transfert of Copyright Agreement form and structure factors will be sent on receipt of your acknowledgement letter ; _publ_requested_category FM #=============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _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 ;Co-ordination chemistry of macrocyclic compounds with dangling phosphines. Unusual NMR shifts in metallo-calix[4]arenes. ; # 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 'Cedric B. Dieleman' ;Groupe de Chimie Inorganique Moleculaire UMR 7513 CNRS 1, rue Blaise Pascal 67008 Strasbourg Cedex France ; 'Claire Marsol' ;Groupe de Chimie Inorganique Moleculaire UMR 7513 CNRS 1, rue Blaise Pascal 67008 Strasbourg Cedex France ; 'Dominique Matt' ;Groupe de Chimie Inorganique Moleculaire UMR 7513 CNRS 1, rue Blaise Pascal 67008 Strasbourg Cedex France ; 'Nathalie Kyritsakas' ;Laboratoire de Cristallographie UMR 7513 CNRS 4, rue Blaise Pascal 67008 Strasbourg Cedex France ; 'Anthony Harriman' ;Ecole Europeenne de Chimie Polymeres et Materiaux 1, rue Blaise Pascal 67008 Strabourg Cedex France ; 'Jean-Pierre Kintzinger' ;Laboratoire de RMN et Modelisation Moleculaire UMR 7513 CNRS 4, rue Blaise Pascal 67008 Strasbourg Cedex France ; # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_references ; Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. OpenMoleN, Interactive Intelligent Structure solution (1997) Nonius B.V., Delft, The Netherlands. KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands. Otwinowski, Z. & Minor, W. (1997), Methods in Enzymology, 276, 307-326. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #=============================================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the ? in the data_? line below # by a unique identifier. data_st165 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C144 H166 O13 P4' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C144 H166 O13 P4' _chemical_formula_weight 2228.82 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 P ? 0.090 0.095 International_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' -x,-y,-z _cell_length_a 14.9993(8) _cell_length_b 15.351(1) _cell_length_c 15.4699(9) _cell_angle_alpha 102.912(9) _cell_angle_beta 106.361(9) _cell_angle_gamma 103.676(9) _cell_volume 3156(1) _cell_formula_units_Z 1 _cell_measurement_temperature 173 _cell_measurement_reflns_used 22148 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 26.4 _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.17 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 1194 _exptl_absorpt_coefficient_mu 0.116 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #=============================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 180 frames, 50 sec/frame, delta phi = 1.0 deg. Each frame measured 2 times. Detector to crystal distance 25 mm. ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 22148 _diffrn_reflns_av_R_equivalents 0.075 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 26.38 _reflns_number_total 11952 _reflns_number_gt 5805 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '4Fo^2^/(\s^2^(Fo^2^)+0.0016 Fo^4^)+4.0' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 5805 _refine_ls_number_parameters 712 _refine_ls_number_restraints 3 _refine_ls_number_constraints 0 _refine_ls_abs_structure_details ; ? ; _refine_ls_R_factor_all 0.177 _refine_ls_R_factor_gt 0.085 _refine_ls_wR_factor_all 0.181 _refine_ls_wR_factor_ref 0.109 _refine_ls_goodness_of_fit_all 2.047 _refine_ls_goodness_of_fit_ref 1.225 _refine_ls_shift/su_max 0.036 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_max 1.038 _refine_diff_density_min -0.121 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS 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_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol C1 0.7491(4) -0.1804(4) 0.9096(4) 0.028(3) 1.000 Uani ? ? C C2 0.6754(4) -0.1388(4) 0.9049(4) 0.027(3) 1.000 Uani ? ? C C3 0.6393(4) -0.1224(4) 0.9785(4) 0.029(3) 1.000 Uani ? ? C C4 0.6860(4) -0.1387(4) 1.0619(4) 0.034(3) 1.000 Uani ? ? C C5 0.7650(4) -0.1743(4) 1.0717(4) 0.033(3) 1.000 Uani ? ? C C6 0.7938(4) -0.1952(4) 0.9947(4) 0.031(3) 1.000 Uani ? ? C C7 0.8149(5) -0.1912(4) 1.1657(4) 0.047(3) 1.000 Uani ? ? C C8 0.765(1) -0.2862(7) 1.1610(7) 0.136(8) 1.000 Uani ? ? C C9 0.805(1) -0.1277(7) 1.2480(6) 0.101(6) 1.000 Uani ? ? C C10 0.9217(7) -0.169(1) 1.1849(7) 0.188(7) 1.000 Uani ? ? C O1 0.6259(3) -0.1230(2) 0.8211(2) 0.031(2) 1.000 Uani ? ? O C11 0.6802(4) -0.0512(4) 0.7923(4) 0.036(3) 1.000 Uani ? ? C P1 0.6987(1) 0.0671(1) 0.8649(1) 0.0350(7) 1.000 Uani ? ? P O2 0.6064(3) 0.0756(3) 0.8798(3) 0.037(2) 1.000 Uani ? ? O C12 0.7368(4) 0.1444(4) 0.8005(4) 0.045(3) 1.000 Uani ? ? C C13 0.6703(5) 0.1789(5) 0.7537(5) 0.093(4) 1.000 Uani ? ? C C14 0.6885(6) 0.2335(5) 0.6973(6) 0.103(4) 1.000 Uani ? ? C C15 0.7763(6) 0.2576(6) 0.6899(6) 0.105(4) 1.000 Uani ? ? C C16 0.8487(7) 0.2332(7) 0.7428(7) 0.136(6) 1.000 Uani ? ? C C17 0.8276(7) 0.1733(7) 0.7961(6) 0.135(5) 1.000 Uani ? ? C C18 0.7981(4) 0.0899(4) 0.9737(4) 0.034(3) 1.000 Uani ? ? C C19 0.8880(4) 0.0771(4) 0.9742(4) 0.041(3) 1.000 Uani ? ? C C20 0.9605(5) 0.0921(5) 1.0589(5) 0.049(4) 1.000 Uani ? ? C C21 0.9442(5) 0.1170(5) 1.1435(5) 0.049(4) 1.000 Uani ? ? C C22 0.8566(5) 0.1284(5) 1.1434(5) 0.051(4) 1.000 Uani ? ? C C23 0.7834(5) 0.1163(4) 1.0594(4) 0.044(3) 1.000 Uani ? ? C C24 0.5527(4) -0.0860(4) 0.9730(4) 0.034(3) 1.000 Uani ? ? C C25 0.4554(4) -0.1564(4) 0.9038(4) 0.034(3) 1.000 Uani ? ? C C26 0.4107(4) -0.2321(4) 0.9292(4) 0.036(3) 1.000 Uani ? ? C C27 0.3221(4) -0.3001(4) 0.8723(4) 0.039(3) 1.000 Uani ? ? C C28 0.2768(4) -0.2900(4) 0.7837(4) 0.036(3) 1.000 Uani ? ? C C29 0.3177(4) -0.2152(4) 0.7549(4) 0.032(3) 1.000 Uani ? ? C C30 0.4059(4) -0.1479(4) 0.8163(4) 0.034(3) 1.000 Uani ? ? C C31 0.2686(5) -0.3790(5) 0.9034(5) 0.049(3) 1.000 Uani ? ? C C32 0.1800(6) -0.3560(5) 0.9214(6) 0.068(4) 1.000 Uani ? ? C C33 0.3350(7) -0.3875(5) 0.9941(5) 0.068(4) 1.000 Uani ? ? C C34 0.2325(5) -0.4748(5) 0.8275(5) 0.050(4) 1.000 Uani ? ? C O3 0.4413(3) -0.0744(3) 0.7842(3) 0.036(2) 1.000 Uani ? ? O C35 0.2667(4) -0.2106(4) 0.6572(4) 0.040(3) 1.000 Uani ? ? C C36 0.2784(4) -0.2822(4) 0.5798(4) 0.032(3) 1.000 Uani ? ? C C37 0.1991(4) -0.3612(4) 0.5177(4) 0.037(3) 1.000 Uani ? ? C C38 0.2070(4) -0.4318(4) 0.4491(4) 0.036(3) 1.000 Uani ? ? C C39 0.3020(4) -0.4224(4) 0.4461(4) 0.035(3) 1.000 Uani ? ? C C40 0.3831(4) -0.3456(4) 0.5066(4) 0.035(2) 1.000 Uani ? ? C C41 0.3708(4) -0.2735(4) 0.5708(4) 0.031(3) 1.000 Uani ? ? C C42 0.1187(4) -0.5166(4) 0.3838(5) 0.041(3) 1.000 Uani ? ? C C43 0.0907(7) -0.5789(6) 0.4428(6) 0.077(5) 1.000 Uani ? ? C C44 0.1392(5) -0.5763(5) 0.3037(6) 0.055(4) 1.000 Uani ? ? C C45 0.0316(5) -0.4854(5) 0.3403(6) 0.056(4) 1.000 Uani ? ? C O4 0.6756(3) -0.2169(3) 0.6341(3) 0.036(2) 1.000 Uani ? ? O C46 0.4848(4) -0.3435(4) 0.5101(4) 0.036(3) 1.000 Uani ? ? C C47 0.5432(4) -0.3554(4) 0.6025(4) 0.031(3) 1.000 Uani ? ? C C48 0.5007(4) -0.4295(4) 0.6322(4) 0.030(3) 1.000 Uani ? ? C C49 0.5473(4) -0.4407(4) 0.7186(4) 0.031(3) 1.000 Uani ? ? C C50 0.6383(4) -0.3744(4) 0.7760(4) 0.033(3) 1.000 Uani ? ? C C51 0.6814(4) -0.2987(4) 0.7502(4) 0.029(3) 1.000 Uani ? ? C C52 0.6337(4) -0.2920(4) 0.6613(4) 0.030(2) 1.000 Uani ? ? C C53 0.5016(5) -0.5189(4) 0.7549(4) 0.040(3) 1.000 Uani ? ? C C54 0.5634(6) -0.5853(5) 0.7630(5) 0.056(4) 1.000 Uani ? ? C C55 0.3967(5) -0.5773(5) 0.6896(5) 0.048(4) 1.000 Uani ? ? C C56 0.5000(5) -0.4742(5) 0.8541(4) 0.050(4) 1.000 Uani ? ? C O5 0.4518(3) -0.1977(3) 0.6247(3) 0.036(2) 1.000 Uani ? ? O C57 0.7488(4) -0.2324(4) 0.5952(4) 0.034(3) 1.000 Uani ? ? C P2 0.8166(1) -0.1199(1) 0.5917(1) 0.0364(7) 1.000 Uani ? ? P O6 0.8665(3) -0.0490(3) 0.6876(3) 0.041(2) 1.000 Uani ? ? O C58 0.9016(4) -0.1498(4) 0.5370(4) 0.051(3) 1.000 Uani ? ? C C59 0.8787(5) -0.2292(5) 0.4622(4) 0.059(3) 1.000 Uani ? ? C C60 0.9515(6) -0.2480(5) 0.4269(5) 0.089(4) 1.000 Uani ? ? C C61 1.0461(5) -0.1837(6) 0.4706(6) 0.099(4) 1.000 Uani ? ? C C62 1.0694(6) -0.1032(8) 0.5437(7) 0.093(6) 1.000 Uani ? ? C C63 0.9978(5) -0.0873(6) 0.5771(5) 0.066(4) 1.000 Uani ? ? C C64 0.7295(4) -0.0864(4) 0.5114(4) 0.042(3) 1.000 Uani ? ? C C65 0.6753(6) -0.1405(6) 0.4219(6) 0.080(5) 1.000 Uani ? ? C C66 0.6087(7) -0.1109(7) 0.3618(6) 0.094(5) 1.000 Uani ? ? C C67 0.5961(6) -0.0272(5) 0.3920(5) 0.074(4) 1.000 Uani ? ? C C68 0.6463(7) 0.0275(6) 0.4819(7) 0.117(5) 1.000 Uani ? ? C C69 0.7161(7) 0.0016(6) 0.5426(6) 0.084(5) 1.000 Uani ? ? C C70 0.7721(4) -0.2207(4) 0.8216(4) 0.032(3) 1.000 Uani ? ? C O7 1.0000 -0.5000 1.0000 0.165(5) 0.500 Uiso ? ? O C71 1.081(2) -0.512(2) 1.070(2) 0.33(2) 1.000 Uiso ? ? C C72 1.096(2) -0.589(1) 1.044(1) 0.225(9) 1.000 Uiso ? ? C H1 0.6637 -0.1254 1.1136 0.0465 1.000 Uiso calc C4 H H2 0.8462 -0.2207 0.9997 0.0434 1.000 Uiso calc C6 H H3 0.7947 -0.2975 1.2184 0.2824 1.000 Uiso calc C8 H H4 0.6978 -0.2931 1.1520 0.2824 1.000 Uiso calc C8 H H5 0.7688 -0.3302 1.1094 0.2824 1.000 Uiso calc C8 H H6 0.8360 -0.1399 1.3044 0.1809 1.000 Uiso calc C9 H H7 0.8343 -0.0638 1.2533 0.1809 1.000 Uiso calc C9 H H8 0.7371 -0.1388 1.2388 0.1809 1.000 Uiso calc C9 H H9 0.9523 -0.1792 1.2427 0.3038 1.000 Uiso calc C10 H H10 0.9323 -0.2082 1.1346 0.3038 1.000 Uiso calc C10 H H11 0.9489 -0.1046 1.1898 0.3038 1.000 Uiso calc C10 H H12 0.6450 -0.0585 0.7281 0.0464 1.000 Uiso calc C11 H H13 0.7424 -0.0587 0.7975 0.0464 1.000 Uiso calc C11 H H14 0.6077 0.1650 0.7600 0.0951 1.000 Uiso calc C13 H H15 0.6382 0.2538 0.6636 0.1057 1.000 Uiso calc C14 H H16 0.7881 0.2917 0.6478 0.1117 1.000 Uiso calc C15 H H17 0.9138 0.2565 0.7441 0.1567 1.000 Uiso calc C16 H H18 0.8778 0.1528 0.8297 0.1517 1.000 Uiso calc C17 H H19 0.8987 0.0580 0.9162 0.0553 1.000 Uiso calc C19 H H20 1.0220 0.0854 1.0593 0.0683 1.000 Uiso calc C20 H H21 0.9940 0.1261 1.2016 0.0692 1.000 Uiso calc C21 H H22 0.8457 0.1449 1.2016 0.0682 1.000 Uiso calc C22 H H23 0.7233 0.1259 1.0603 0.0559 1.000 Uiso calc C23 H H24 0.5644 -0.0310 0.9538 0.0437 1.000 Uiso calc C24 H H25 0.5482 -0.0703 1.0342 0.0437 1.000 Uiso calc C24 H H26 0.4432 -0.2373 0.9892 0.0467 1.000 Uiso calc C26 H H27 0.2161 -0.3358 0.7420 0.0503 1.000 Uiso calc C28 H H28 0.1460 -0.4041 0.9408 0.0865 1.000 Uiso calc C32 H H29 0.2019 -0.2972 0.9698 0.0865 1.000 Uiso calc C32 H H30 0.1373 -0.3525 0.8648 0.0865 1.000 Uiso calc C32 H H31 0.2996 -0.4367 1.0112 0.0944 1.000 Uiso calc C33 H H32 0.3903 -0.4013 0.9837 0.0944 1.000 Uiso calc C33 H H33 0.3563 -0.3296 1.0437 0.0944 1.000 Uiso calc C33 H H34 0.1998 -0.5219 0.8489 0.0691 1.000 Uiso calc C34 H H35 0.1883 -0.4728 0.7708 0.0691 1.000 Uiso calc C34 H H36 0.2868 -0.4894 0.8154 0.0691 1.000 Uiso calc C34 H H37 0.2940 -0.1492 0.6545 0.0506 1.000 Uiso calc C35 H H38 0.1988 -0.2226 0.6468 0.0506 1.000 Uiso calc C35 H H39 0.1365 -0.3669 0.5228 0.0443 1.000 Uiso calc C37 H H40 0.3107 -0.4701 0.4014 0.0435 1.000 Uiso calc C39 H H41 0.0355 -0.6324 0.4034 0.1053 1.000 Uiso calc C43 H H42 0.1444 -0.5990 0.4698 0.1053 1.000 Uiso calc C43 H H43 0.0749 -0.5440 0.4920 0.1053 1.000 Uiso calc C43 H H44 0.0818 -0.6280 0.2653 0.0837 1.000 Uiso calc C44 H H45 0.1576 -0.5390 0.2663 0.0837 1.000 Uiso calc C44 H H46 0.1909 -0.5992 0.3295 0.0837 1.000 Uiso calc C44 H H47 -0.0227 -0.5393 0.2998 0.0893 1.000 Uiso calc C45 H H48 0.0145 -0.4520 0.3893 0.0893 1.000 Uiso calc C45 H H49 0.0489 -0.4455 0.3046 0.0893 1.000 Uiso calc C45 H H50 0.5179 -0.2847 0.5054 0.0451 1.000 Uiso calc C46 H H51 0.4803 -0.3933 0.4583 0.0451 1.000 Uiso calc C46 H H52 0.4383 -0.4733 0.5922 0.0414 1.000 Uiso calc C48 H H53 0.6720 -0.3813 0.8348 0.0449 1.000 Uiso calc C50 H H54 0.5349 -0.6336 0.7855 0.0757 1.000 Uiso calc C54 H H55 0.5656 -0.6129 0.7025 0.0757 1.000 Uiso calc C54 H H56 0.6281 -0.5506 0.8061 0.0757 1.000 Uiso calc C54 H H57 0.3714 -0.6247 0.7146 0.0687 1.000 Uiso calc C55 H H58 0.3570 -0.5374 0.6851 0.0687 1.000 Uiso calc C55 H H59 0.3965 -0.6061 0.6284 0.0687 1.000 Uiso calc C55 H H60 0.4718 -0.5224 0.8768 0.0698 1.000 Uiso calc C56 H H61 0.5652 -0.4400 0.8965 0.0698 1.000 Uiso calc C56 H H62 0.4622 -0.4326 0.8502 0.0698 1.000 Uiso calc C56 H H63 0.7185 -0.2760 0.5330 0.0438 1.000 Uiso calc C57 H H64 0.7916 -0.2563 0.6342 0.0438 1.000 Uiso calc C57 H H65 0.8136 -0.2717 0.4342 0.0692 1.000 Uiso calc C59 H H66 0.9366 -0.3025 0.3752 0.0981 1.000 Uiso calc C60 H H67 1.0965 -0.1963 0.4489 0.1141 1.000 Uiso calc C61 H H68 1.1339 -0.0595 0.5705 0.1255 1.000 Uiso calc C62 H H69 1.0136 -0.0324 0.6287 0.0883 1.000 Uiso calc C63 H H70 0.6823 -0.2004 0.3989 0.1054 1.000 Uiso calc C65 H H71 0.5717 -0.1506 0.2986 0.1330 1.000 Uiso calc C66 H H72 0.5521 -0.0069 0.3499 0.0908 1.000 Uiso calc C67 H H73 0.6341 0.0848 0.5047 0.1422 1.000 Uiso calc C68 H H74 0.7544 0.0431 0.6048 0.1109 1.000 Uiso calc C69 H H75 0.8246 -0.2455 0.8388 0.0427 1.000 Uiso calc C70 H H76 0.7901 -0.1723 0.7948 0.0427 1.000 Uiso calc C70 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol C1 0.029(3) 0.027(3) 0.029(3) 0.005(2) 0.005(2) 0.005(2) C C2 0.028(3) 0.027(3) 0.026(3) 0.007(2) 0.002(2) 0.004(2) C C3 0.036(3) 0.024(3) 0.028(3) 0.007(2) 0.010(2) 0.005(2) C C4 0.038(3) 0.034(3) 0.031(3) 0.008(2) 0.010(2) 0.009(2) C C5 0.035(3) 0.031(3) 0.033(3) 0.007(2) 0.005(2) 0.009(2) C C6 0.031(3) 0.032(3) 0.030(3) 0.011(2) 0.000(2) 0.008(2) C C7 0.058(3) 0.056(3) 0.032(3) 0.025(3) 0.016(3) 0.022(2) C C8 0.31(2) 0.080(5) 0.103(5) -0.052(8) -0.102(7) 0.070(3) C C9 0.25(1) 0.137(6) 0.030(4) 0.119(5) -0.001(5) 0.024(4) C C10 0.091(5) 0.60(1) 0.121(5) 0.183(6) 0.059(4) 0.221(6) C O1 0.036(2) 0.033(2) 0.025(2) 0.015(1) 0.007(1) 0.010(1) O C11 0.044(3) 0.036(3) 0.030(3) 0.019(2) 0.012(2) 0.013(2) C P1 0.0401(7) 0.0297(6) 0.0360(7) 0.0166(5) 0.0158(6) 0.0111(5) P O2 0.038(2) 0.033(2) 0.042(2) 0.016(1) 0.017(2) 0.012(2) O C12 0.046(3) 0.041(3) 0.049(3) 0.021(2) 0.025(2) 0.023(2) C C13 0.073(3) 0.106(4) 0.105(4) 0.065(3) 0.059(3) 0.080(3) C C14 0.103(4) 0.102(4) 0.103(4) 0.076(3) 0.060(3) 0.077(3) C C15 0.094(5) 0.105(4) 0.116(4) 0.054(4) 0.061(4) 0.090(3) C C16 0.093(6) 0.171(6) 0.158(6) 0.054(5) 0.064(5) 0.129(4) C C17 0.080(5) 0.189(6) 0.162(5) 0.071(4) 0.068(4) 0.146(4) C C18 0.044(3) 0.022(2) 0.040(3) 0.012(2) 0.016(2) 0.008(2) C C19 0.040(3) 0.042(3) 0.042(3) 0.011(2) 0.014(3) 0.009(3) C C20 0.041(3) 0.047(3) 0.061(4) 0.018(3) 0.008(3) 0.008(3) C C21 0.053(4) 0.048(4) 0.047(4) 0.017(3) 0.005(3) 0.008(3) C C22 0.054(4) 0.058(4) 0.042(3) 0.022(3) 0.012(3) 0.011(3) C C23 0.052(3) 0.043(3) 0.038(3) 0.020(2) 0.017(2) 0.011(3) C C24 0.044(3) 0.031(3) 0.030(3) 0.018(2) 0.015(2) 0.007(2) C C25 0.037(3) 0.032(3) 0.032(3) 0.016(2) 0.012(2) 0.005(2) C C26 0.038(3) 0.039(3) 0.032(3) 0.015(2) 0.010(2) 0.011(2) C C27 0.042(3) 0.039(3) 0.038(3) 0.015(2) 0.016(2) 0.010(2) C C28 0.037(3) 0.040(3) 0.032(3) 0.011(2) 0.008(2) 0.003(3) C C29 0.032(3) 0.039(3) 0.027(3) 0.017(2) 0.010(2) 0.007(2) C C30 0.034(2) 0.039(3) 0.029(3) 0.019(2) 0.014(2) 0.011(2) C C31 0.060(4) 0.041(3) 0.047(3) 0.011(3) 0.019(3) 0.015(3) C C32 0.073(4) 0.053(4) 0.082(4) 0.014(3) 0.045(3) 0.020(3) C C33 0.091(6) 0.063(4) 0.056(4) 0.008(4) 0.017(4) 0.030(3) C C34 0.051(4) 0.040(3) 0.061(4) 0.012(3) 0.011(3) 0.016(3) C O3 0.040(2) 0.036(2) 0.032(2) 0.017(1) 0.013(2) 0.014(1) O C35 0.036(3) 0.049(3) 0.036(3) 0.023(2) 0.013(2) 0.013(2) C C36 0.035(3) 0.039(3) 0.025(2) 0.019(2) 0.006(2) 0.010(2) C C37 0.032(2) 0.047(3) 0.034(3) 0.021(2) 0.014(2) 0.021(2) C C38 0.038(3) 0.039(3) 0.031(3) 0.019(2) 0.011(2) 0.016(2) C C39 0.040(3) 0.036(3) 0.029(3) 0.020(2) 0.012(2) 0.010(2) C C40 0.037(3) 0.041(3) 0.027(2) 0.022(2) 0.014(2) 0.018(2) C C41 0.032(3) 0.035(3) 0.026(2) 0.013(2) 0.005(2) 0.013(2) C C42 0.039(3) 0.034(3) 0.050(3) 0.014(2) 0.014(3) 0.008(3) C C43 0.091(5) 0.051(4) 0.100(5) 0.007(4) 0.045(4) 0.025(4) C C44 0.045(4) 0.052(4) 0.072(5) 0.011(3) 0.013(3) -0.012(4) C C45 0.039(3) 0.060(4) 0.078(5) 0.020(3) -0.002(4) -0.010(4) C O4 0.034(2) 0.037(2) 0.036(2) 0.016(1) 0.017(1) 0.015(1) O C46 0.039(3) 0.040(3) 0.029(3) 0.019(2) 0.013(2) 0.010(2) C C47 0.034(3) 0.036(3) 0.026(3) 0.016(2) 0.008(2) 0.006(2) C C48 0.031(3) 0.029(3) 0.030(3) 0.009(2) 0.007(2) 0.004(2) C C49 0.035(3) 0.029(3) 0.030(2) 0.013(2) 0.014(2) 0.010(2) C C50 0.043(3) 0.031(3) 0.027(3) 0.016(2) 0.007(2) 0.008(2) C C51 0.028(2) 0.028(2) 0.031(3) 0.013(2) 0.007(2) 0.005(2) C C52 0.031(2) 0.028(2) 0.032(3) 0.013(2) 0.013(2) 0.010(2) C C53 0.054(3) 0.037(3) 0.031(3) 0.012(3) 0.011(3) 0.010(2) C C54 0.083(5) 0.045(3) 0.047(4) 0.025(3) 0.018(3) 0.016(3) C C55 0.058(4) 0.043(3) 0.044(3) -0.006(3) 0.015(3) 0.015(3) C C56 0.068(4) 0.050(4) 0.037(3) 0.007(3) 0.019(3) 0.013(3) C O5 0.033(2) 0.042(2) 0.034(2) 0.011(2) 0.012(2) 0.007(2) O C57 0.037(3) 0.038(3) 0.027(3) 0.013(2) 0.012(2) 0.010(2) C P2 0.0337(7) 0.0414(7) 0.0344(7) 0.0136(6) 0.0142(6) 0.0145(6) P O6 0.041(2) 0.046(2) 0.037(2) 0.006(2) 0.009(2) 0.006(2) O C58 0.051(3) 0.064(3) 0.041(3) 0.032(2) 0.026(2) 0.030(2) C C59 0.061(3) 0.076(4) 0.045(3) 0.042(3) 0.027(3) 0.029(3) C C60 0.114(4) 0.112(4) 0.056(3) 0.082(3) 0.055(3) 0.051(3) C C61 0.067(3) 0.153(5) 0.095(5) 0.075(3) 0.046(3) 0.071(4) C C62 0.060(4) 0.157(8) 0.085(5) 0.042(5) 0.036(4) 0.039(5) C C63 0.044(3) 0.104(5) 0.064(4) 0.027(3) 0.026(3) 0.027(4) C C64 0.051(3) 0.039(3) 0.038(3) 0.020(2) 0.027(2) 0.021(2) C C65 0.096(5) 0.093(4) 0.057(4) 0.063(3) 0.010(4) 0.013(4) C C66 0.135(6) 0.131(6) 0.047(4) 0.089(4) 0.010(4) 0.022(4) C C67 0.084(5) 0.075(4) 0.065(4) 0.045(3) 0.018(4) 0.039(3) C C68 0.147(6) 0.119(5) 0.093(6) 0.105(3) 0.031(5) 0.038(4) C C69 0.107(6) 0.090(5) 0.061(5) 0.051(4) 0.016(4) 0.022(4) C C70 0.031(3) 0.033(3) 0.032(3) 0.015(2) 0.005(2) 0.008(2) C # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.393(8) . . ? C1 C6 1.393(8) . . ? C1 C70 1.532(9) . . ? C2 C3 1.393(8) . . ? C2 O1 1.406(7) . . ? C3 C4 1.390(9) . . ? C3 C24 1.519(9) . . ? C4 C5 1.403(9) . . ? C5 C6 1.376(9) . . ? C5 C7 1.546(9) . . ? C7 C8 1.45(1) . . ? C7 C9 1.49(1) . . ? C7 C10 1.48(1) . . ? O1 C11 1.441(8) . . ? C11 P1 1.820(6) . . ? P1 O2 1.496(4) . . ? P1 C12 1.804(7) . . ? P1 C18 1.803(7) . . ? C12 C13 1.35(1) . . ? C12 C17 1.35(1) . . ? C13 C14 1.37(1) . . ? C14 C15 1.33(1) . . ? C15 C16 1.35(1) . . ? C16 C17 1.41(1) . . ? C18 C19 1.406(9) . . ? C18 C23 1.393(9) . . ? C19 C20 1.38(1) . . ? C20 C21 1.39(1) . . ? C21 C22 1.37(1) . . ? C22 C23 1.39(1) . . ? C24 C25 1.517(9) . . ? C25 C26 1.392(9) . . ? C25 C30 1.399(8) . . ? C26 C27 1.381(9) . . ? C27 C28 1.410(9) . . ? C27 C31 1.54(1) . . ? C28 C29 1.392(9) . . ? C29 C30 1.389(9) . . ? C29 C35 1.516(9) . . ? C30 O3 1.384(7) . . ? C31 C32 1.53(1) . . ? C31 C33 1.53(1) . . ? C31 C34 1.53(1) . . ? C35 C36 1.516(9) . . ? C36 C37 1.400(9) . . ? C36 C41 1.410(9) . . ? C37 C38 1.390(9) . . ? C38 C39 1.413(9) . . ? C38 C42 1.520(9) . . ? C39 C40 1.391(9) . . ? C40 C41 1.398(8) . . ? C40 C46 1.503(9) . . ? C41 O5 1.361(7) . . ? C42 C43 1.53(1) . . ? C42 C44 1.52(1) . . ? C42 C45 1.53(1) . . ? O4 C52 1.388(7) . . ? O4 C57 1.433(7) . . ? C46 C47 1.526(8) . . ? C47 C48 1.402(9) . . ? C47 C52 1.379(8) . . ? C48 C49 1.392(8) . . ? C49 C50 1.394(9) . . ? C49 C53 1.535(9) . . ? C50 C51 1.388(9) . . ? C51 C52 1.399(8) . . ? C51 C70 1.516(9) . . ? C53 C54 1.53(1) . . ? C53 C55 1.53(1) . . ? C53 C56 1.54(1) . . ? C57 P2 1.806(7) . . ? P2 O6 1.488(5) . . ? P2 C58 1.806(7) . . ? P2 C64 1.790(7) . . ? C58 C59 1.38(1) . . ? C58 C63 1.40(1) . . ? C59 C60 1.41(1) . . ? C60 C61 1.39(1) . . ? C61 C62 1.37(2) . . ? C62 C63 1.36(1) . . ? C64 C65 1.34(1) . . ? C64 C69 1.41(1) . . ? C65 C66 1.40(1) . . ? C66 C67 1.34(1) . . ? C67 C68 1.34(1) . . ? C68 C69 1.39(1) . . ? O7 C71 1.47(4) . . ? C71 C72 1.25(4) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 118.0(6) . . . ? C2 C1 C70 121.8(5) . . . ? C6 C1 C70 119.8(5) . . . ? C1 C2 C3 121.3(5) . . . ? C1 C2 O1 121.3(5) . . . ? C3 C2 O1 116.9(5) . . . ? C2 C3 C4 118.2(6) . . . ? C2 C3 C24 123.3(5) . . . ? C4 C3 C24 118.5(6) . . . ? C3 C4 C5 121.8(6) . . . ? C4 C5 C6 117.6(6) . . . ? C4 C5 C7 120.1(6) . . . ? C6 C5 C7 122.2(6) . . . ? C1 C6 C5 122.6(6) . . . ? C5 C7 C8 108.6(7) . . . ? C5 C7 C9 111.7(6) . . . ? C5 C7 C10 109.5(7) . . . ? C8 C7 C9 105(1) . . . ? C8 C7 C10 115(1) . . . ? C9 C7 C10 106(1) . . . ? C2 O1 C11 117.5(5) . . . ? O1 C11 P1 112.1(4) . . . ? C11 P1 O2 111.3(3) . . . ? C11 P1 C12 105.4(3) . . . ? C11 P1 C18 106.0(3) . . . ? O2 P1 C12 110.6(3) . . . ? O2 P1 C18 113.4(3) . . . ? C12 P1 C18 109.7(3) . . . ? P1 C12 C13 117.9(6) . . . ? P1 C12 C17 126.0(6) . . . ? C13 C12 C17 116.1(7) . . . ? C12 C13 C14 123.2(8) . . . ? C13 C14 C15 120.1(8) . . . ? C14 C15 C16 119.2(9) . . . ? C15 C16 C17 119(1) . . . ? C12 C17 C16 121.1(9) . . . ? P1 C18 C19 122.0(5) . . . ? P1 C18 C23 118.8(5) . . . ? C19 C18 C23 119.1(6) . . . ? C18 C19 C20 120.0(7) . . . ? C19 C20 C21 120.2(7) . . . ? C20 C21 C22 120.1(7) . . . ? C21 C22 C23 120.8(7) . . . ? C18 C23 C22 119.8(7) . . . ? C3 C24 C25 113.9(5) . . . ? C24 C25 C26 118.8(6) . . . ? C24 C25 C30 123.4(6) . . . ? C26 C25 C30 117.7(6) . . . ? C25 C26 C27 123.9(6) . . . ? C26 C27 C28 116.1(6) . . . ? C26 C27 C31 124.0(6) . . . ? C28 C27 C31 119.7(6) . . . ? C27 C28 C29 122.4(6) . . . ? C28 C29 C30 118.7(6) . . . ? C28 C29 C35 119.6(6) . . . ? C30 C29 C35 121.7(6) . . . ? C25 C30 C29 121.1(6) . . . ? C25 C30 O3 123.2(6) . . . ? C29 C30 O3 115.6(5) . . . ? C27 C31 C32 108.3(6) . . . ? C27 C31 C33 111.8(6) . . . ? C27 C31 C34 111.6(6) . . . ? C32 C31 C33 108.9(7) . . . ? C32 C31 C34 108.8(7) . . . ? C33 C31 C34 107.4(6) . . . ? C29 C35 C36 112.0(5) . . . ? C35 C36 C37 121.3(6) . . . ? C35 C36 C41 120.8(6) . . . ? C37 C36 C41 117.9(6) . . . ? C36 C37 C38 123.6(6) . . . ? C37 C38 C39 116.4(6) . . . ? C37 C38 C42 121.6(6) . . . ? C39 C38 C42 122.0(6) . . . ? C38 C39 C40 122.1(6) . . . ? C39 C40 C41 119.5(6) . . . ? C39 C40 C46 120.8(6) . . . ? C41 C40 C46 119.5(6) . . . ? C36 C41 C40 120.2(6) . . . ? C36 C41 O5 122.7(6) . . . ? C40 C41 O5 117.0(6) . . . ? C38 C42 C43 108.0(6) . . . ? C38 C42 C44 113.0(6) . . . ? C38 C42 C45 110.8(6) . . . ? C43 C42 C44 107.7(6) . . . ? C43 C42 C45 108.9(7) . . . ? C44 C42 C45 108.2(6) . . . ? C52 O4 C57 112.9(4) . . . ? C40 C46 C47 111.2(5) . . . ? C46 C47 C48 119.1(6) . . . ? C46 C47 C52 122.3(6) . . . ? C48 C47 C52 118.5(5) . . . ? C47 C48 C49 122.0(6) . . . ? C48 C49 C50 117.5(6) . . . ? C48 C49 C53 123.4(6) . . . ? C50 C49 C53 119.1(5) . . . ? C49 C50 C51 122.2(6) . . . ? C50 C51 C52 118.4(6) . . . ? C50 C51 C70 119.7(5) . . . ? C52 C51 C70 121.5(6) . . . ? O4 C52 C47 119.2(5) . . . ? O4 C52 C51 119.3(5) . . . ? C47 C52 C51 121.4(6) . . . ? C49 C53 C54 109.8(6) . . . ? C49 C53 C55 112.3(5) . . . ? C49 C53 C56 109.3(5) . . . ? C54 C53 C55 108.4(6) . . . ? C54 C53 C56 108.6(6) . . . ? C55 C53 C56 108.4(6) . . . ? O4 C57 P2 107.2(4) . . . ? C57 P2 O6 112.3(3) . . . ? C57 P2 C58 102.8(3) . . . ? C57 P2 C64 105.4(3) . . . ? O6 P2 C58 112.9(3) . . . ? O6 P2 C64 113.8(3) . . . ? C58 P2 C64 108.8(3) . . . ? P2 C58 C59 124.8(6) . . . ? P2 C58 C63 116.0(6) . . . ? C59 C58 C63 119.2(7) . . . ? C58 C59 C60 120.4(9) . . . ? C59 C60 C61 117.7(9) . . . ? C60 C61 C62 122.5(9) . . . ? C61 C62 C63 118(1) . . . ? C58 C63 C62 121.6(9) . . . ? P2 C64 C65 123.7(6) . . . ? P2 C64 C69 119.1(6) . . . ? C65 C64 C69 117.2(7) . . . ? C64 C65 C66 121.5(8) . . . ? C65 C66 C67 121.0(9) . . . ? C66 C67 C68 119.4(8) . . . ? C67 C68 C69 120.9(9) . . . ? C64 C69 C68 119.8(9) . . . ? C1 C70 C51 108.6(5) . . . ? O7 C71 C72 113(3) . . . ? data_st329 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C146 H170 Cl16 O9 P4 Pt2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C146 H170 Cl16 O9 P4 Pt2' _chemical_formula_weight 3150.30 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 Cl ? 0.132 0.159 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 P ? 0.090 0.095 International_Tables_Vol_IV_Table_2.3.1 Pt ? -2.352 8.388 International_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall ' P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' 1/2-x,-y,1/2+z -x,1/2+y,1/2-z 1/2+x,1/2-y,-z _cell_length_a 12.571(1) _cell_length_b 22.5546(3) _cell_length_c 26.4894(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 7510.6(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used 50394 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 32.4 _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.39 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 3212 _exptl_absorpt_coefficient_mu 2.241 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #=============================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 144 frames,109 sec/frame, delta phi = 1.3 deg. Each frame measured 2 times. Detector to crystal distance 32 mm. ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 50394 _diffrn_reflns_av_R_equivalents 0.063 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 32.39 _reflns_number_total 13123 _reflns_number_gt 9230 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '4Fo^2^/(\s^2^(Fo^2^) + 0.0064 Fo^4^)' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack 0.02(1) _refine_ls_number_reflns 9230 _refine_ls_number_parameters 824 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_R_factor_all 0.068 _refine_ls_R_factor_gt 0.050 _refine_ls_wR_factor_all 0.371 _refine_ls_wR_factor_ref 0.068 _refine_ls_goodness_of_fit_all 5.859 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_shift/su_max 0.030 _refine_ls_shift/esd_mean 0.002 _refine_diff_density_max 1.416 _refine_diff_density_min -0.190 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS 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_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol PT 0.27765(2) 0.77664(1) 0.89389(1) 0.02681(9) 1.000 Uani ? ? Pt CL1 0.3619(1) 0.73818(9) 0.96564(8) 0.0356(8) 1.000 Uani ? ? Cl CL2 0.4499(2) 0.7983(1) 0.86239(8) 0.042(1) 1.000 Uani ? ? Cl C1 0.2367(7) 1.0298(4) 0.8729(3) 0.034(3) 1.000 Uani ? ? C C2 0.3013(6) 1.0752(3) 0.8897(3) 0.035(3) 1.000 Uani ? ? C C3 0.3780(7) 1.0685(4) 0.9261(3) 0.036(4) 1.000 Uani ? ? C C4 0.3853(6) 1.0142(4) 0.9491(3) 0.033(4) 1.000 Uani ? ? C C5 0.3228(6) 0.9659(3) 0.9356(3) 0.028(3) 1.000 Uani ? ? C C6 0.2513(6) 0.9737(3) 0.8943(3) 0.029(3) 1.000 Uani ? ? C C7 0.4532(8) 1.1205(4) 0.9384(4) 0.046(5) 1.000 Uani ? ? C C8 0.5085(9) 1.1106(5) 0.9908(4) 0.061(6) 1.000 Uani ? ? C C9 0.393(1) 1.1796(5) 0.9390(6) 0.069(6) 1.000 Uani ? ? C C10 0.5387(9) 1.1254(5) 0.8973(6) 0.069(7) 1.000 Uani ? ? C O1 0.1981(4) 0.9241(2) 0.8758(2) 0.030(2) 1.000 Uani ? ? O C11 0.2522(7) 0.9017(3) 0.8315(3) 0.036(4) 1.000 Uani ? ? C P1 0.2171(2) 0.82266(9) 0.82463(7) 0.0310(8) 1.000 Uani ? ? P C12 0.0805(7) 0.8200(4) 0.8042(3) 0.035(4) 1.000 Uani ? ? C C13 0.0231(8) 0.8736(5) 0.7921(4) 0.058(6) 1.000 Uani ? ? C C14 -0.0781(9) 0.8680(6) 0.7708(5) 0.069(6) 1.000 Uani ? ? C C15 -0.1233(9) 0.8134(7) 0.7642(4) 0.064(6) 1.000 Uani ? ? C C16 -0.0730(9) 0.7617(5) 0.7782(3) 0.053(5) 1.000 Uani ? ? C C17 0.0319(8) 0.7667(5) 0.7976(3) 0.047(5) 1.000 Uani ? ? C C18 0.2884(7) 0.8020(4) 0.7661(3) 0.036(4) 1.000 Uani ? ? C C19 0.292(1) 0.8413(4) 0.7258(4) 0.057(5) 1.000 Uani ? ? C C20 0.344(1) 0.8260(5) 0.6825(4) 0.062(6) 1.000 Uani ? ? C C21 0.3843(9) 0.7698(6) 0.6767(4) 0.058(6) 1.000 Uani ? ? C C22 0.3762(9) 0.7276(5) 0.7148(4) 0.060(5) 1.000 Uani ? ? C C23 0.3282(8) 0.7452(4) 0.7609(3) 0.040(4) 1.000 Uani ? ? C C24 0.3281(6) 0.9075(3) 0.9642(3) 0.027(3) 1.000 Uani ? ? C C25 0.2782(6) 0.9136(3) 1.0165(3) 0.028(3) 1.000 Uani ? ? C C26 0.3328(6) 0.9396(3) 1.0559(3) 0.032(3) 1.000 Uani ? ? C C27 0.2869(6) 0.9522(3) 1.1020(3) 0.034(3) 1.000 Uani ? ? C C28 0.1789(6) 0.9384(3) 1.1071(3) 0.034(3) 1.000 Uani ? ? C C29 0.1208(6) 0.9109(3) 1.0691(3) 0.028(3) 1.000 Uani ? ? C C30 0.1724(6) 0.8965(3) 1.0241(3) 0.026(3) 1.000 Uani ? ? C C31 0.3498(8) 0.9782(5) 1.1460(4) 0.050(5) 1.000 Uani ? ? C C32 0.422(1) 0.9289(8) 1.1669(6) 0.175(8) 1.000 Uani ? ? C C33 0.411(2) 1.033(1) 1.1251(9) 0.184(8) 1.000 Uani ? ? C C34 0.282(1) 0.9956(6) 1.1909(4) 0.077(6) 1.000 Uani ? ? C O2 0.1197(4) 0.8640(2) 0.9865(2) 0.027(2) 1.000 Uani ? ? O C35 0.1285(6) 0.8011(3) 0.9968(3) 0.026(3) 1.000 Uani ? ? C P2 0.1284(2) 0.75688(9) 0.93787(7) 0.0272(8) 1.000 Uani ? ? P C36 -0.0075(5) 0.7650(3) 0.9143(3) 0.029(3) 1.000 Uani ? ? C C37 -0.0458(7) 0.8223(4) 0.9048(3) 0.036(4) 1.000 Uani ? ? C C38 -0.1535(7) 0.8289(4) 0.8927(3) 0.043(4) 1.000 Uani ? ? C C39 -0.2197(7) 0.7808(5) 0.8885(3) 0.047(4) 1.000 Uani ? ? C C40 -0.1799(7) 0.7251(5) 0.8975(3) 0.045(4) 1.000 Uani ? ? C C41 -0.0763(7) 0.7168(4) 0.9112(3) 0.039(4) 1.000 Uani ? ? C C42 0.1328(6) 0.6811(3) 0.9610(3) 0.030(3) 1.000 Uani ? ? C C43 0.1034(7) 0.6657(4) 1.0107(3) 0.040(4) 1.000 Uani ? ? C C44 0.1084(7) 0.6070(4) 1.0248(4) 0.051(5) 1.000 Uani ? ? C C45 0.1412(7) 0.5635(4) 0.9907(5) 0.051(5) 1.000 Uani ? ? C C46 0.1675(8) 0.5784(4) 0.9429(5) 0.047(5) 1.000 Uani ? ? C C47 0.1646(7) 0.6365(3) 0.9279(4) 0.038(4) 1.000 Uani ? ? C C48 0.0002(7) 0.9014(4) 1.0765(3) 0.032(3) 1.000 Uani ? ? C C49 -0.0607(6) 0.9582(3) 1.0622(3) 0.033(4) 1.000 Uani ? ? C C50 -0.0868(6) 0.9989(3) 1.0995(3) 0.032(3) 1.000 Uani ? ? C C51 -0.1457(7) 1.0502(4) 1.0886(4) 0.038(4) 1.000 Uani ? ? C C52 -0.1722(7) 1.0597(4) 1.0380(3) 0.039(4) 1.000 Uani ? ? C C53 -0.1449(6) 1.0198(3) 1.0003(3) 0.033(4) 1.000 Uani ? ? C C54 -0.0860(6) 0.9707(3) 1.0126(3) 0.031(3) 1.000 Uani ? ? C C55 -0.1818(8) 1.0955(4) 1.1294(4) 0.048(5) 1.000 Uani ? ? C C56 -0.127(1) 1.0849(6) 1.1797(5) 0.078(8) 1.000 Uani ? ? C C57 -0.3001(9) 1.0884(5) 1.1359(5) 0.063(6) 1.000 Uani ? ? C C58 -0.156(1) 1.1586(5) 1.1129(5) 0.071(7) 1.000 Uani ? ? C O3 -0.0626(5) 0.9322(3) 0.9742(2) 0.038(3) 1.000 Uani ? ? O C59 -0.1805(7) 1.0311(4) 0.9463(3) 0.036(4) 1.000 Uani ? ? C C60 -0.0987(7) 1.0672(4) 0.9160(3) 0.036(4) 1.000 Uani ? ? C C61 -0.1053(7) 1.1294(4) 0.9144(3) 0.043(4) 1.000 Uani ? ? C C62 -0.0320(7) 1.1647(4) 0.8880(3) 0.042(4) 1.000 Uani ? ? C C63 0.0464(7) 1.1356(4) 0.8610(3) 0.037(4) 1.000 Uani ? ? C C64 0.0569(7) 1.0734(4) 0.8620(3) 0.036(4) 1.000 Uani ? ? C C65 -0.0171(6) 1.0407(4) 0.8884(3) 0.036(4) 1.000 Uani ? ? C C66 -0.043(1) 1.2328(4) 0.8862(4) 0.053(5) 1.000 Uani ? ? C C67 -0.080(1) 1.2506(6) 0.8339(5) 0.085(8) 1.000 Uani ? ? C C68 0.062(1) 1.2609(5) 0.8989(6) 0.074(8) 1.000 Uani ? ? C C69 -0.124(1) 1.2576(5) 0.9237(5) 0.063(6) 1.000 Uani ? ? C O4 -0.0094(5) 0.9789(3) 0.8852(2) 0.044(3) 1.000 Uani ? ? O C70 0.1479(7) 1.0426(4) 0.8355(3) 0.038(4) 1.000 Uani ? ? C C71 0.102(1) 1.1159(6) 1.0036(5) 0.070(7) 1.000 Uani ? ? C CL3 0.1116(4) 1.1894(2) 1.0309(2) 0.098(3) 1.000 Uani ? ? Cl CL4 0.1751(4) 1.0675(2) 1.0367(2) 0.108(3) 1.000 Uani ? ? Cl C72 0.528(2) 0.958(1) 0.8281(7) 0.13(1) 1.000 Uani ? ? C CL5 0.6638(5) 0.9582(4) 0.8336(3) 0.183(5) 1.000 Uani ? ? Cl CL6 0.4807(4) 0.9963(5) 0.7815(2) 0.157(5) 1.000 Uani ? ? Cl C73 0.825(3) 1.091(1) 0.772(1) 0.09(2) 0.500 Uani ? ? C CL7 0.8829(7) 1.0181(5) 0.7681(3) 0.104(5) 0.500 Uani ? ? Cl CL8 0.763(1) 1.0954(3) 0.7040(3) 0.129(6) 0.500 Uani ? ? Cl C74 0.383(2) 1.209(1) 0.7242(9) 0.08(1) 0.500 Uani ? ? C CL9 0.3257(5) 1.2074(3) 0.7818(2) 0.074(3) 0.500 Uani ? ? Cl CL10 0.429(1) 1.1461(5) 0.7100(4) 0.228(7) 0.500 Uani ? ? Cl O5 0.479(1) 1.1178(6) 0.7212(5) 0.051(3) 0.500 Uiso ? ? O H1 0.2923 1.1134 0.8752 0.0462 1.000 Uiso calc C2 H H2 0.4355 1.0093 0.9756 0.0444 1.000 Uiso calc C4 H H3 0.5542 1.1432 0.9978 0.0804 1.000 Uiso calc C8 H H4 0.4556 1.1081 1.0164 0.0804 1.000 Uiso calc C8 H H5 0.5485 1.0751 0.9900 0.0804 1.000 Uiso calc C8 H H6 0.4419 1.2107 0.9466 0.1019 1.000 Uiso calc C9 H H7 0.3628 1.1864 0.9067 0.1019 1.000 Uiso calc C9 H H8 0.3392 1.1783 0.9638 0.1019 1.000 Uiso calc C9 H H9 0.5854 1.1573 0.9050 0.0923 1.000 Uiso calc C10 H H10 0.5788 1.0894 0.8962 0.0923 1.000 Uiso calc C10 H H11 0.5063 1.1319 0.8656 0.0923 1.000 Uiso calc C10 H H12 0.3265 0.9060 0.8352 0.0540 1.000 Uiso calc C11 H H13 0.2290 0.9231 0.8025 0.0540 1.000 Uiso calc C11 H H14 0.0533 0.9114 0.7984 0.0763 1.000 Uiso calc C13 H H15 -0.1158 0.9027 0.7607 0.0964 1.000 Uiso calc C14 H H16 -0.1922 0.8108 0.7495 0.0928 1.000 Uiso calc C15 H H17 -0.1068 0.7243 0.7750 0.0750 1.000 Uiso calc C16 H H18 0.0695 0.7318 0.8063 0.0666 1.000 Uiso calc C17 H H19 0.2568 0.8787 0.7281 0.0787 1.000 Uiso calc C19 H H20 0.3538 0.8543 0.6564 0.0863 1.000 Uiso calc C20 H H21 0.4185 0.7599 0.6459 0.0824 1.000 Uiso calc C21 H H22 0.4015 0.6882 0.7100 0.0791 1.000 Uiso calc C22 H H23 0.3235 0.7181 0.7883 0.0529 1.000 Uiso calc C23 H H24 0.4005 0.8960 0.9678 0.0356 1.000 Uiso calc C24 H H25 0.2908 0.8779 0.9458 0.0356 1.000 Uiso calc C24 H H26 0.4056 0.9494 1.0510 0.0417 1.000 Uiso calc C26 H H27 0.1438 0.9483 1.1377 0.0441 1.000 Uiso calc C28 H H28 0.4636 0.9440 1.1940 0.2181 1.000 Uiso calc C32 H H29 0.3813 0.8965 1.1776 0.2181 1.000 Uiso calc C32 H H30 0.4700 0.9163 1.1405 0.2181 1.000 Uiso calc C32 H H31 0.4516 1.0510 1.1511 0.2403 1.000 Uiso calc C33 H H32 0.4574 1.0209 1.0985 0.2403 1.000 Uiso calc C33 H H33 0.3616 1.0613 1.1120 0.2403 1.000 Uiso calc C33 H H34 0.3262 1.0114 1.2167 0.1064 1.000 Uiso calc C34 H H35 0.2315 1.0246 1.1809 0.1064 1.000 Uiso calc C34 H H36 0.2459 0.9616 1.2034 0.1064 1.000 Uiso calc C34 H H37 0.0698 0.7890 1.0170 0.0382 1.000 Uiso calc C35 H H38 0.1928 0.7937 1.0145 0.0382 1.000 Uiso calc C35 H H39 -0.0002 0.8557 0.9067 0.0469 1.000 Uiso calc C37 H H40 -0.1815 0.8676 0.8875 0.0564 1.000 Uiso calc C38 H H41 -0.2923 0.7859 0.8793 0.0656 1.000 Uiso calc C39 H H42 -0.2254 0.6917 0.8942 0.0603 1.000 Uiso calc C40 H H43 -0.0510 0.6780 0.9186 0.0512 1.000 Uiso calc C41 H H44 0.0803 0.6950 1.0338 0.0530 1.000 Uiso calc C43 H H45 0.0890 0.5963 1.0583 0.0685 1.000 Uiso calc C44 H H46 0.1452 0.5233 1.0012 0.0776 1.000 Uiso calc C45 H H47 0.1879 0.5485 0.9195 0.0698 1.000 Uiso calc C46 H H48 0.1846 0.6466 0.8943 0.0541 1.000 Uiso calc C47 H H49 -0.0135 0.8919 1.1108 0.0422 1.000 Uiso calc C48 H H50 -0.0229 0.8696 1.0555 0.0422 1.000 Uiso calc C48 H H51 -0.0641 0.9920 1.1332 0.0409 1.000 Uiso calc C50 H H52 -0.2102 1.0947 1.0292 0.0513 1.000 Uiso calc C52 H H53 -0.1508 1.1133 1.2036 0.1068 1.000 Uiso calc C56 H H54 -0.1435 1.0461 1.1914 0.1068 1.000 Uiso calc C56 H H55 -0.0521 1.0884 1.1755 0.1068 1.000 Uiso calc C56 H H56 -0.3250 1.1157 1.1604 0.0809 1.000 Uiso calc C57 H H57 -0.3346 1.0963 1.1044 0.0809 1.000 Uiso calc C57 H H58 -0.3157 1.0492 1.1462 0.0809 1.000 Uiso calc C57 H H59 -0.1794 1.1855 1.1383 0.1004 1.000 Uiso calc C58 H H60 -0.0823 1.1626 1.1079 0.1004 1.000 Uiso calc C58 H H61 -0.1930 1.1671 1.0823 0.1004 1.000 Uiso calc C58 H H62 -0.2458 1.0524 0.9469 0.0470 1.000 Uiso calc C59 H H63 -0.1910 0.9941 0.9300 0.0470 1.000 Uiso calc C59 H H64 -0.1618 1.1482 0.9320 0.0562 1.000 Uiso calc C61 H H65 0.0948 1.1580 0.8414 0.0479 1.000 Uiso calc C63 H H66 -0.0868 1.2925 0.8324 0.1183 1.000 Uiso calc C67 H H67 -0.0292 1.2379 0.8096 0.1183 1.000 Uiso calc C67 H H68 -0.1466 1.2327 0.8270 0.1183 1.000 Uiso calc C67 H H69 0.0552 1.3030 0.8977 0.1095 1.000 Uiso calc C68 H H70 0.0835 1.2494 0.9319 0.1095 1.000 Uiso calc C68 H H71 0.1145 1.2488 0.8752 0.1095 1.000 Uiso calc C68 H H72 -0.1265 1.2996 0.9205 0.0874 1.000 Uiso calc C69 H H73 -0.1921 1.2415 0.9168 0.0874 1.000 Uiso calc C69 H H74 -0.1032 1.2474 0.9571 0.0874 1.000 Uiso calc C69 H H75 0.1235 1.0064 0.8214 0.0500 1.000 Uiso calc C70 H H76 0.1744 1.0674 0.8094 0.0500 1.000 Uiso calc C70 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol PT 0.02506(9) 0.02883(9) 0.02666(9) 0.0002(1) 0.0009(1) -0.0041(1) Pt CL1 0.0297(8) 0.0390(9) 0.0390(9) 0.0049(7) -0.0026(7) 0.0028(8) Cl CL2 0.0308(8) 0.063(1) 0.039(1) -0.0048(9) 0.0064(8) -0.004(1) Cl C1 0.036(4) 0.035(3) 0.030(3) 0.002(3) 0.002(3) -0.000(3) C C2 0.042(4) 0.023(3) 0.042(4) -0.000(3) 0.008(3) 0.004(3) C C3 0.036(4) 0.037(4) 0.035(4) -0.006(3) -0.000(3) -0.002(3) C C4 0.026(3) 0.042(4) 0.035(4) -0.005(3) -0.002(3) -0.003(3) C C5 0.026(3) 0.027(3) 0.030(3) 0.003(3) 0.003(3) -0.003(3) C C6 0.030(3) 0.031(3) 0.026(3) -0.001(3) 0.000(3) -0.006(3) C C7 0.044(4) 0.035(4) 0.061(5) -0.006(4) -0.008(4) 0.001(4) C C8 0.061(5) 0.054(6) 0.070(6) -0.018(5) -0.026(5) 0.004(5) C C9 0.075(6) 0.036(5) 0.123(9) -0.011(5) -0.047(6) 0.015(6) C C10 0.053(5) 0.063(6) 0.098(9) -0.019(5) 0.008(7) 0.006(7) C O1 0.032(3) 0.030(2) 0.029(2) -0.002(2) 0.002(2) -0.010(2) O C11 0.046(4) 0.026(3) 0.038(4) -0.001(3) 0.006(3) -0.006(3) C P1 0.0346(8) 0.0333(8) 0.0257(7) -0.0023(9) 0.0011(9) -0.0035(7) P C12 0.041(4) 0.041(4) 0.025(3) 0.001(4) -0.003(3) 0.000(3) C C13 0.047(5) 0.071(6) 0.059(6) 0.003(5) -0.012(5) 0.019(5) C C14 0.040(5) 0.108(8) 0.074(6) 0.011(6) -0.011(5) 0.044(6) C C15 0.048(5) 0.12(1) 0.045(5) -0.009(7) -0.019(4) 0.003(6) C C16 0.062(5) 0.081(7) 0.030(4) -0.018(6) -0.013(4) -0.010(4) C C17 0.051(4) 0.077(7) 0.027(3) -0.019(5) 0.000(4) -0.005(4) C C18 0.045(4) 0.049(4) 0.022(3) -0.008(4) 0.004(3) -0.007(3) C C19 0.091(7) 0.044(5) 0.046(4) -0.007(6) 0.029(5) -0.003(4) C C20 0.097(8) 0.065(6) 0.037(4) -0.021(7) 0.022(5) -0.016(5) C C21 0.074(6) 0.083(7) 0.032(4) -0.002(7) 0.011(4) -0.017(5) C C22 0.067(5) 0.071(6) 0.045(5) 0.027(6) 0.011(5) -0.009(5) C C23 0.046(4) 0.041(4) 0.034(4) 0.006(4) -0.001(4) -0.003(4) C C24 0.022(3) 0.034(3) 0.026(3) -0.000(3) -0.004(3) 0.000(3) C C25 0.028(3) 0.024(3) 0.033(3) -0.000(3) 0.005(3) -0.002(3) C C26 0.027(3) 0.032(3) 0.037(4) 0.000(3) -0.002(3) -0.001(3) C C27 0.037(3) 0.036(3) 0.031(3) -0.007(3) -0.007(3) -0.006(3) C C28 0.037(3) 0.032(3) 0.033(3) 0.001(3) -0.002(4) -0.009(3) C C29 0.033(3) 0.023(3) 0.029(3) 0.004(3) 0.003(3) -0.004(3) C C30 0.024(3) 0.023(3) 0.033(3) 0.002(3) -0.005(3) -0.002(3) C C31 0.049(5) 0.057(5) 0.044(4) -0.006(5) -0.005(4) -0.020(4) C C32 0.184(8) 0.16(1) 0.179(7) 0.115(9) -0.155(6) -0.112(9) C C33 0.208(8) 0.19(1) 0.160(7) -0.119(9) -0.102(6) 0.026(9) C C34 0.067(6) 0.119(8) 0.057(5) -0.011(9) -0.004(6) -0.051(5) C O2 0.023(2) 0.031(2) 0.028(2) 0.001(2) -0.004(2) -0.005(2) O C35 0.027(3) 0.025(3) 0.025(3) 0.003(3) 0.004(3) -0.003(3) C P2 0.0275(8) 0.0251(7) 0.0291(8) 0.0007(7) 0.0005(7) -0.0016(7) P C36 0.019(3) 0.038(4) 0.033(3) 0.002(3) 0.000(3) -0.008(3) C C37 0.040(4) 0.032(4) 0.036(4) 0.004(3) -0.003(3) -0.007(3) C C38 0.044(4) 0.050(4) 0.036(3) 0.015(4) -0.008(4) -0.008(4) C C39 0.035(3) 0.083(6) 0.035(4) 0.010(5) -0.010(3) -0.005(5) C C40 0.036(3) 0.067(5) 0.037(4) -0.006(5) -0.001(4) -0.003(5) C C41 0.037(4) 0.054(5) 0.029(3) -0.000(4) -0.001(3) 0.001(4) C C42 0.024(3) 0.032(3) 0.037(4) -0.000(3) 0.004(3) -0.004(3) C C43 0.034(4) 0.043(4) 0.044(4) -0.006(4) -0.004(4) 0.008(4) C C44 0.035(4) 0.051(5) 0.075(6) -0.008(4) -0.013(4) 0.028(4) C C45 0.028(4) 0.042(4) 0.110(8) 0.002(4) 0.005(5) 0.031(5) C C46 0.034(4) 0.033(4) 0.093(7) 0.009(4) 0.001(5) -0.004(5) C C47 0.032(4) 0.024(3) 0.069(6) 0.001(3) 0.004(4) 0.001(4) C C48 0.032(3) 0.031(3) 0.034(4) 0.002(3) 0.004(3) 0.004(3) C C49 0.031(3) 0.029(3) 0.042(4) -0.002(3) 0.002(3) -0.002(3) C C50 0.031(3) 0.034(3) 0.030(4) 0.001(3) 0.002(3) -0.004(3) C C51 0.031(4) 0.036(4) 0.049(4) -0.002(3) 0.001(4) 0.000(4) C C52 0.033(4) 0.039(4) 0.045(4) 0.009(4) 0.006(4) 0.003(4) C C53 0.032(3) 0.030(3) 0.038(4) -0.004(3) 0.001(3) -0.000(3) C C54 0.031(3) 0.027(3) 0.036(4) -0.003(3) 0.006(3) -0.003(3) C C55 0.053(5) 0.045(4) 0.048(5) 0.011(4) 0.004(4) -0.012(4) C C56 0.12(1) 0.070(7) 0.058(6) 0.018(8) -0.021(8) -0.015(6) C C57 0.056(6) 0.059(6) 0.073(6) 0.009(5) 0.021(5) -0.012(6) C C58 0.12(1) 0.048(5) 0.065(7) 0.002(7) -0.002(8) -0.012(5) C O3 0.041(3) 0.039(3) 0.034(3) 0.007(3) -0.003(3) -0.006(2) O C59 0.034(3) 0.039(4) 0.036(4) -0.001(4) -0.002(3) 0.005(3) C C60 0.041(4) 0.034(4) 0.034(4) 0.005(4) -0.004(3) 0.003(3) C C61 0.043(4) 0.050(5) 0.036(4) 0.013(4) -0.005(4) 0.005(4) C C62 0.052(4) 0.039(4) 0.036(4) 0.015(4) 0.001(4) 0.003(4) C C63 0.042(4) 0.036(4) 0.032(4) 0.003(4) 0.002(3) 0.002(3) C C64 0.036(4) 0.041(4) 0.031(3) -0.001(4) -0.004(3) -0.002(3) C C65 0.027(3) 0.042(4) 0.041(4) -0.001(3) -0.006(3) -0.003(4) C C66 0.074(6) 0.037(4) 0.055(5) 0.005(5) 0.006(5) 0.014(4) C C67 0.13(1) 0.078(7) 0.059(6) 0.028(9) 0.018(8) 0.040(5) C C68 0.079(8) 0.039(5) 0.13(1) -0.003(6) 0.011(9) -0.009(7) C C69 0.099(9) 0.040(5) 0.063(6) -0.002(6) 0.005(7) -0.001(5) C O4 0.044(3) 0.035(3) 0.055(4) 0.001(3) 0.011(3) 0.004(3) O C70 0.039(4) 0.045(4) 0.031(4) 0.004(4) 0.004(3) 0.002(3) C C71 0.077(7) 0.067(7) 0.068(7) 0.004(7) -0.019(6) -0.017(6) C CL3 0.129(3) 0.065(2) 0.112(3) 0.013(2) 0.001(3) -0.021(2) Cl CL4 0.117(3) 0.076(2) 0.141(3) 0.035(2) 0.016(3) 0.032(2) Cl C72 0.12(1) 0.20(2) 0.09(1) -0.07(1) -0.00(1) 0.01(1) C CL5 0.098(3) 0.339(9) 0.183(5) -0.041(5) -0.004(4) 0.108(5) Cl CL6 0.089(3) 0.35(1) 0.122(4) 0.034(6) 0.012(3) 0.002(6) Cl C73 0.14(2) 0.07(1) 0.07(1) 0.05(2) 0.03(2) 0.00(1) C CL7 0.086(4) 0.181(9) 0.072(4) -0.024(6) -0.027(4) 0.024(5) Cl CL8 0.24(1) 0.082(4) 0.108(5) 0.084(5) 0.055(7) 0.039(4) Cl C74 0.047(8) 0.19(2) 0.06(1) -0.06(1) -0.031(8) 0.06(1) C CL9 0.050(2) 0.108(4) 0.075(3) 0.020(3) 0.007(2) 0.053(3) Cl CL10 0.186(8) 0.290(6) 0.219(5) -0.131(7) 0.095(6) -0.220(3) Cl # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag PT CL1 2.342(2) . . ? PT CL2 2.372(2) . . ? PT P1 2.241(2) . . ? PT P2 2.253(2) . . ? C1 C2 1.38(1) . . ? C1 C6 1.40(1) . . ? C1 C70 1.52(1) . . ? C2 C3 1.37(1) . . ? C3 C4 1.37(1) . . ? C3 C7 1.54(1) . . ? C4 C5 1.39(1) . . ? C5 C6 1.43(1) . . ? C5 C24 1.52(1) . . ? C6 O1 1.393(9) . . ? C7 C8 1.57(2) . . ? C7 C9 1.53(2) . . ? C7 C10 1.53(2) . . ? O1 C11 1.45(1) . . ? C11 P1 1.844(9) . . ? P1 C12 1.80(1) . . ? P1 C18 1.851(9) . . ? C12 C13 1.44(2) . . ? C12 C17 1.36(1) . . ? C13 C14 1.40(2) . . ? C14 C15 1.37(2) . . ? C15 C16 1.38(2) . . ? C16 C17 1.42(2) . . ? C18 C19 1.39(1) . . ? C18 C23 1.38(1) . . ? C19 C20 1.37(1) . . ? C20 C21 1.37(2) . . ? C21 C22 1.39(2) . . ? C22 C23 1.42(1) . . ? C24 C25 1.53(1) . . ? C25 C26 1.38(1) . . ? C25 C30 1.40(1) . . ? C26 C27 1.38(1) . . ? C27 C28 1.40(1) . . ? C27 C31 1.53(1) . . ? C28 C29 1.39(1) . . ? C29 C30 1.40(1) . . ? C29 C48 1.54(1) . . ? C30 O2 1.403(9) . . ? C31 C32 1.54(2) . . ? C31 C33 1.56(3) . . ? C31 C34 1.51(2) . . ? O2 C35 1.448(9) . . ? C35 P2 1.852(8) . . ? P2 C36 1.829(8) . . ? P2 C42 1.816(9) . . ? C36 C37 1.40(1) . . ? C36 C41 1.39(1) . . ? C37 C38 1.40(1) . . ? C38 C39 1.37(2) . . ? C39 C40 1.37(2) . . ? C40 C41 1.36(1) . . ? C42 C43 1.41(1) . . ? C42 C47 1.39(1) . . ? C43 C44 1.38(1) . . ? C44 C45 1.40(2) . . ? C45 C46 1.35(2) . . ? C46 C47 1.37(1) . . ? C48 C49 1.54(1) . . ? C49 C50 1.39(1) . . ? C49 C54 1.38(1) . . ? C50 C51 1.40(1) . . ? C51 C52 1.40(1) . . ? C51 C55 1.56(1) . . ? C52 C53 1.39(1) . . ? C53 C54 1.37(1) . . ? C53 C59 1.52(1) . . ? C54 O3 1.37(1) . . ? C55 C56 1.52(2) . . ? C55 C57 1.51(2) . . ? C55 C58 1.52(2) . . ? C59 C60 1.54(1) . . ? C60 C61 1.41(1) . . ? C60 C65 1.39(1) . . ? C61 C62 1.41(1) . . ? C62 C63 1.38(1) . . ? C62 C66 1.54(1) . . ? C63 C64 1.41(1) . . ? C64 C65 1.38(1) . . ? C64 C70 1.51(1) . . ? C65 O4 1.40(1) . . ? C66 C67 1.52(2) . . ? C66 C68 1.51(2) . . ? C66 C69 1.52(2) . . ? C71 CL3 1.81(1) . . ? C71 CL4 1.67(2) . . ? C72 CL5 1.72(2) . . ? C72 CL6 1.62(3) . . ? C73 CL7 1.79(3) . . ? C73 CL8 1.96(4) . . ? C74 CL9 1.69(3) . . ? C74 CL10 1.58(5) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag CL1 PT CL2 87.06(8) . . . ? CL1 PT P1 171.61(8) . . . ? CL1 PT P2 83.32(8) . . . ? CL2 PT P1 85.79(9) . . . ? CL2 PT P2 169.44(8) . . . ? P1 PT P2 103.43(8) . . . ? C2 C1 C6 117.6(8) . . . ? C2 C1 C70 120.0(8) . . . ? C6 C1 C70 122.2(8) . . . ? C1 C2 C3 123.9(8) . . . ? C2 C3 C4 117.3(8) . . . ? C2 C3 C7 119.8(8) . . . ? C4 C3 C7 123.0(8) . . . ? C3 C4 C5 123.2(8) . . . ? C4 C5 C6 117.2(7) . . . ? C4 C5 C24 121.7(7) . . . ? C6 C5 C24 121.1(7) . . . ? C1 C6 C5 120.4(7) . . . ? C1 C6 O1 121.4(7) . . . ? C5 C6 O1 118.2(7) . . . ? C3 C7 C8 110.5(9) . . . ? C3 C7 C9 111.4(9) . . . ? C3 C7 C10 109.5(9) . . . ? C8 C7 C9 109(1) . . . ? C8 C7 C10 109(1) . . . ? C9 C7 C10 106(1) . . . ? C6 O1 C11 109.9(6) . . . ? O1 C11 P1 107.8(6) . . . ? C11 P1 C12 106.8(4) . . . ? C11 P1 C18 102.2(4) . . . ? C12 P1 C18 101.6(4) . . . ? P1 C12 C13 121.0(8) . . . ? P1 C12 C17 119.8(8) . . . ? C13 C12 C17 119.2(9) . . . ? C12 C13 C14 117(1) . . . ? C13 C14 C15 120(1) . . . ? C14 C15 C16 122(1) . . . ? C15 C16 C17 117(1) . . . ? C12 C17 C16 122(1) . . . ? P1 C18 C19 119.8(8) . . . ? P1 C18 C23 119.5(7) . . . ? C19 C18 C23 120.3(8) . . . ? C18 C19 C20 119(1) . . . ? C19 C20 C21 120(1) . . . ? C20 C21 C22 121(1) . . . ? C21 C22 C23 117(1) . . . ? C18 C23 C22 120.0(9) . . . ? C5 C24 C25 110.9(6) . . . ? C24 C25 C26 121.3(8) . . . ? C24 C25 C30 119.8(7) . . . ? C26 C25 C30 118.7(7) . . . ? C25 C26 C27 123.2(8) . . . ? C26 C27 C28 116.5(8) . . . ? C26 C27 C31 122.5(8) . . . ? C28 C27 C31 121.0(9) . . . ? C27 C28 C29 122.6(9) . . . ? C28 C29 C30 118.6(8) . . . ? C28 C29 C48 119.1(7) . . . ? C30 C29 C48 122.2(7) . . . ? C25 C30 C29 120.1(7) . . . ? C25 C30 O2 119.4(7) . . . ? C29 C30 O2 120.5(7) . . . ? C27 C31 C32 107(1) . . . ? C27 C31 C33 106(1) . . . ? C27 C31 C34 114.0(9) . . . ? C32 C31 C33 114(1) . . . ? C32 C31 C34 103(1) . . . ? C33 C31 C34 110(1) . . . ? C30 O2 C35 110.0(6) . . . ? O2 C35 P2 111.6(5) . . . ? C35 P2 C36 103.5(4) . . . ? C35 P2 C42 102.9(4) . . . ? C36 P2 C42 103.8(4) . . . ? P2 C36 C37 118.3(6) . . . ? P2 C36 C41 121.4(7) . . . ? C37 C36 C41 119.8(8) . . . ? C36 C37 C38 118.1(9) . . . ? C37 C38 C39 121.4(9) . . . ? C38 C39 C40 119.2(8) . . . ? C39 C40 C41 121(1) . . . ? C36 C41 C40 120(1) . . . ? P2 C42 C43 122.5(7) . . . ? P2 C42 C47 118.5(7) . . . ? C43 C42 C47 119.0(9) . . . ? C42 C43 C44 118(1) . . . ? C43 C44 C45 120(1) . . . ? C44 C45 C46 120(1) . . . ? C45 C46 C47 120(1) . . . ? C42 C47 C46 121(1) . . . ? C29 C48 C49 110.0(7) . . . ? C48 C49 C50 119.5(8) . . . ? C48 C49 C54 121.3(8) . . . ? C50 C49 C54 119.2(8) . . . ? C49 C50 C51 121.5(8) . . . ? C50 C51 C52 116.8(9) . . . ? C50 C51 C55 123.5(9) . . . ? C52 C51 C55 119.6(9) . . . ? C51 C52 C53 122.1(9) . . . ? C52 C53 C54 119.1(8) . . . ? C52 C53 C59 119.8(8) . . . ? C54 C53 C59 121.2(8) . . . ? C49 C54 C53 121.1(8) . . . ? C49 C54 O3 121.8(8) . . . ? C53 C54 O3 116.9(8) . . . ? C51 C55 C56 111(1) . . . ? C51 C55 C57 107(1) . . . ? C51 C55 C58 110.8(9) . . . ? C56 C55 C57 109(1) . . . ? C56 C55 C58 107(1) . . . ? C57 C55 C58 109(1) . . . ? C53 C59 C60 112.6(8) . . . ? C59 C60 C61 120.2(9) . . . ? C59 C60 C65 122.6(8) . . . ? C61 C60 C65 117.2(9) . . . ? C60 C61 C62 122.7(9) . . . ? C61 C62 C63 117.2(9) . . . ? C61 C62 C66 121.3(9) . . . ? C63 C62 C66 121(1) . . . ? C62 C63 C64 121.9(9) . . . ? C63 C64 C65 118.7(9) . . . ? C63 C64 C70 121.3(9) . . . ? C65 C64 C70 120.0(8) . . . ? C60 C65 C64 122.2(9) . . . ? C60 C65 O4 120.6(9) . . . ? C64 C65 O4 117.1(8) . . . ? C62 C66 C67 108(1) . . . ? C62 C66 C68 109(1) . . . ? C62 C66 C69 114.0(9) . . . ? C67 C66 C68 110(1) . . . ? C67 C66 C69 107(1) . . . ? C68 C66 C69 106(1) . . . ? C1 C70 C64 109.8(7) . . . ? CL3 C71 CL4 110.7(8) . . . ? CL5 C72 CL6 115(1) . . . ? CL7 C73 CL8 99(1) . . . ? CL9 C74 CL10 110(2) . . . ?