Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_coden_ASTM ? _journal_coeditor_code ? _journal_coeditor_name ? _journal_coeditor_notes ; ? ; _journal_date_accepted ? _journal_date_from_coeditor ? _journal_date_printers_final ? _journal_date_printers_first ? _journal_date_proofs_in ? _journal_date_proofs_out ? #============================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_volume ? _journal_year ? loop_ _publ_author_name _publ_author_address J.Bennett ; Department of Chemistry, The Faculties, Australian National University, Canberra, A. C. T. 0200, Australia ; R.J.Doyle ; Department of Chemistry, The Faculties, Australian National University, Canberra, A. C. T. 0200, Australia ; G.Salem ; Department of Chemistry, The Faculties, Australian National University, Canberra, A. C. T. 0200, Australia ; A.C.Willis ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_contact_author_address ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_contact_author_email willis@rsc.anu.edu.au _publ_contact_author_fax ' 61 2 6125 0750 ' _publ_contact_author_phone ' 61 2 6125 4109 ' _publ_contact_author_name 'Anthony C. Willis' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_category 'FM ' _publ_requested_coeditor_name ? #============================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis of a chelating hexadentate ligand with a P3N3 donor set. Crystal and molecular structure of [OC-6-22]-[Co{(RP*,RP*,RP*)-CH3C(CH2PPhC6H4NH2-2)3}](PF6)3 ; data_rxd20 _database_code_depnum_ccdc_archive 'CCDC 609895' _audit_creation_date 03-27-10 _audit_creation_method CRYSTALS_ver_12-03-99 # 10271243 rxd20 _audit_update_record ; 2003-10-26 - Report on C44 H48 Co F18 N3 O P3 by Anthony C. Willis for Geoff Salem, Roy Doyle and Justine Bennett 2002-10-26 - passes checkcif tests with minor warnings ; #============================================================================== # 4. TEXT _publ_section_abstract #Text of the abstract ; The crystal structure of [Co(C~41~H~42~N~3~P~3~)](PF~6~)~3~.C~3~H~6~O is reported. ; _publ_section_comment #Text of the paper ; The crystallographic asymmetric unit consists of a [Co(C~41~H~42~N~3~P~3~)]^3+^ cation, three PF~6~^-^ anions and a solvate acetone molecule. Hydrogen atoms were included at idealized positions and ride on the atoms to which they were bonded. The methyl groups were oriented to best-fit peaks in a difference electron density map. The biggest peaks in the final difference electron density map were located close to atoms of the anions. ; _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 ride on the atoms to which they were bonded. ; _publ_section_exptl_prep ; The compound was prepared by JB and recrystallized by RJD from acetone/2-propanol. The sample ID is P~3~N~3~-F~7~-1/03. ; #========================================================================== _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 al 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al 2001) ; _computing_molecular_graphics ; ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997) ; #============================================================= _cell_length_a 27.1248(3) _cell_angle_alpha 90 _cell_length_b 10.8041(1) _cell_angle_beta 92.1000(4) _cell_length_c 34.2865(4) _cell_angle_gamma 90 _cell_volume 10041.2(2) _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 ' 0.0033 0.0016 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 'Co ' 0.2990 0.9730 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692 1.0118 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_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 '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 _chemical_formula_sum ' C44 H48 Co F18 N3 O P6 ' _chemical_formula_moiety ' C41 H42 Co N3 P3 3+, 3(P F6 -), C3 H6 O' _chemical_compound_source ; ? ; _chemical_formula_weight 1221.62 _cell_measurement_reflns_used 181484 _cell_measurement_theta_min 3 _cell_measurement_theta_max 25 _cell_measurement_temperature 200 _cell_formula_units_Z 8 _exptl_crystal_description ' plate ' _exptl_crystal_colour ' green ' _exptl_crystal_size_min 0.03 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_max 0.52 _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 4960.00 _exptl_absorpt_coefficient_mu 0.639 # Sheldrick geometric definitions 0.83 0.98 _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 ' \f and \w scans with CCD ' _diffrn_special_details ; CCD data collecting conditions- phi and omega scans of width 0.6 deg at rate 90 sec/frame, crystal-detector distance 55mm, multiple scan sets so over 90 percent of data collected with 4-fold redundancy or more. ; # Absorption correction loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 1 0.140 -1 0 -1 0.160 -1 0 1 0.020 1 0 -1 0.010 -1 -1 0 0.260 1 1 1 0.155 1 -1 1 0.200 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.807 _exptl_absorpt_correction_T_max 0.981 _exptl_absorpt_process_details ; via Gaussian method (Coppens, 1970) implemented in maXus (2000) ; _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 200 _diffrn_reflns_number 62348 _reflns_number_total 8844 _diffrn_reflns_av_R_equivalents 0.08 # Number of reflections with Friedels Law is 8844 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 8867 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _reflns_number_gt 5526 _diffrn_reflns_theta_min 4.08 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_full 25.02 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _reflns_limit_h_min -32 _reflns_limit_h_max 32 _reflns_limit_k_min 0 _reflns_limit_k_max 12 _reflns_limit_l_min 0 _reflns_limit_l_max 40 _refine_diff_density_min -0.37 _refine_diff_density_max 0.50 _reflns_threshold_expression >2.00\s(I) _refine_ls_number_reflns 5526 _refine_ls_number_parameters 658 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0382 _refine_ls_goodness_of_fit_ref 1.0826 _refine_ls_shift/su_max 0.001964 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 4 parameters, Carruthers & Watkin , 1979, 0.554 -.191 0.278 -.145 ; _refine_ls_extinction_method None _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Mackay, S., Gilmore, C. J.,Edwards, C., Stewart, N. & Shankland, K. (2000). maXus Computer Program for the Solution and Refinement of Crystal Structures. Nonius, The Netherlands, MacScience, Japan & The University of Glasgow. Coppens, P. (1970). The Evaluation of Absorption and Extinction in Single-Crystal Structure Analysis. Crystallographic Computing. F. R. Ahmed, S. R. Hall and C. P. Huber, eds., Munksgaard. Copenhagen. pp 255-270. Carruthers, J.R. & Watkin, D.J. (1979) Acta Cryst., A35, 698-699. Altomare, A., Cascarano, G., Giacovazzo C., 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. Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.8. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Johnson, C.K. (1976) ORTEP-II, A Fortran Thermal-Ellipsoid Plot Program, Report ORNL-5138, Oak Ridge National Laboratory, Oak Ridge, Tennessee, USA. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Co1 co 0.136549(15) 0.41367(4) 0.632309(11) 0.0280 1.0000 Uani P1 p 0.16174(3) 0.32978(7) 0.57784(2) 0.0328 1.0000 Uani P2 p 0.20442(3) 0.35186(7) 0.66332(2) 0.0306 1.0000 Uani P3 p 0.10077(3) 0.23830(7) 0.64694(2) 0.0296 1.0000 Uani P4 p 0.10609(3) 0.81482(8) 0.54504(3) 0.0425 1.0000 Uani P5 p 0.13751(4) 0.82198(8) 0.72766(3) 0.0475 1.0000 Uani P6 p 0.36771(4) 0.08174(12) 0.60259(4) 0.0696 1.0000 Uani F41 f 0.16203(8) 0.7716(2) 0.55368(6) 0.0563 1.0000 Uani F42 f 0.12404(9) 0.9531(2) 0.54067(9) 0.0806 1.0000 Uani F43 f 0.1119(1) 0.7914(2) 0.50061(6) 0.0731 1.0000 Uani F44 f 0.05063(8) 0.8556(2) 0.53790(8) 0.0755 1.0000 Uani F45 f 0.0886(1) 0.6759(2) 0.55042(9) 0.0821 1.0000 Uani F46 f 0.1012(1) 0.8397(3) 0.59046(7) 0.0983 1.0000 Uani F51 f 0.09880(9) 0.8741(2) 0.69542(8) 0.0706 1.0000 Uani F52 f 0.1026(1) 0.7063(2) 0.73436(8) 0.0766 1.0000 Uani F53 f 0.11109(11) 0.8975(2) 0.76042(8) 0.0807 1.0000 Uani F54 f 0.17682(11) 0.7690(2) 0.75885(7) 0.0797 1.0000 Uani F55 f 0.17261(9) 0.9357(2) 0.71992(7) 0.0656 1.0000 Uani F56 f 0.16308(9) 0.7430(2) 0.69386(7) 0.0708 1.0000 Uani F61 f 0.34745(12) -0.0519(3) 0.60949(11) 0.1031 1.0000 Uani F62 f 0.34365(15) 0.1275(4) 0.6408(1) 0.1374 1.0000 Uani F63 f 0.41648(13) 0.0465(4) 0.62570(14) 0.1488 1.0000 Uani F64 f 0.38716(17) 0.2154(4) 0.59460(18) 0.1724 1.0000 Uani F65 f 0.38940(15) 0.0335(4) 0.56356(11) 0.1377 1.0000 Uani F66 f 0.31750(12) 0.1190(3) 0.5803(1) 0.1134 1.0000 Uani O1 o 0.02940(13) 0.6304(4) 0.65002(9) 0.0947 1.0000 Uani N1 n 0.0772(1) 0.4708(2) 0.59961(7) 0.0360 1.0000 Uani N2 n 0.17350(9) 0.5762(2) 0.62374(7) 0.0345 1.0000 Uani N3 n 0.10664(9) 0.4800(2) 0.68160(7) 0.0320 1.0000 Uani C1 c 0.21332(12) -0.0115(3) 0.6214(1) 0.0401 1.0000 Uani C2 c 0.19014(11) 0.1184(3) 0.62417(9) 0.0331 1.0000 Uani C11 c 0.18409(12) 0.1702(3) 0.58254(9) 0.0385 1.0000 Uani C21 c 0.22615(11) 0.1981(3) 0.64966(9) 0.0362 1.0000 Uani C31 c 0.13984(11) 0.1012(3) 0.64341(9) 0.0351 1.0000 Uani C41 c 0.00220(15) 0.7115(4) 0.65973(12) 0.0578 1.0000 Uani C42 c -0.0229(2) 0.7047(6) 0.69668(16) 0.1008 1.0000 Uani C43 c -0.00739(19) 0.8213(5) 0.63497(18) 0.0990 1.0000 Uani C101 c 0.10495(12) 0.3312(3) 0.54902(9) 0.0375 1.0000 Uani C102 c 0.06721(12) 0.4026(3) 0.56323(9) 0.0362 1.0000 Uani C103 c 0.02133(13) 0.4083(3) 0.5442(1) 0.0456 1.0000 Uani C104 c 0.01377(15) 0.3407(3) 0.5100(1) 0.0516 1.0000 Uani C105 c 0.05180(15) 0.2717(4) 0.4950(1) 0.0524 1.0000 Uani C106 c 0.09725(14) 0.2663(3) 0.5141(1) 0.0462 1.0000 Uani C111 c 0.20588(12) 0.4119(3) 0.54924(9) 0.0391 1.0000 Uani C112 c 0.18840(15) 0.5014(3) 0.5231(1) 0.0515 1.0000 Uani C113 c 0.22107(19) 0.5696(4) 0.50151(13) 0.0731 1.0000 Uani C114 c 0.2708(2) 0.5483(4) 0.50613(15) 0.0788 1.0000 Uani C115 c 0.28846(16) 0.4588(4) 0.53156(14) 0.0685 1.0000 Uani C116 c 0.25621(14) 0.3895(4) 0.55357(11) 0.0508 1.0000 Uani C201 c 0.24760(11) 0.4672(3) 0.64769(9) 0.0341 1.0000 Uani C202 c 0.22720(12) 0.5692(3) 0.62869(9) 0.0344 1.0000 Uani C203 c 0.25726(13) 0.6611(3) 0.6141(1) 0.0429 1.0000 Uani C204 c 0.30795(14) 0.6482(3) 0.61866(11) 0.0506 1.0000 Uani C205 c 0.32870(13) 0.5474(4) 0.63774(11) 0.0503 1.0000 Uani C206 c 0.29885(12) 0.4563(3) 0.6530(1) 0.0437 1.0000 Uani C211 c 0.20571(11) 0.3577(3) 0.71598(9) 0.0349 1.0000 Uani C212 c 0.20888(11) 0.4732(3) 0.73418(9) 0.0368 1.0000 Uani C213 c 0.20412(13) 0.4818(4) 0.7744(1) 0.0451 1.0000 Uani C214 c 0.19812(13) 0.3759(4) 0.7964(1) 0.0486 1.0000 Uani C215 c 0.19616(13) 0.2615(4) 0.7784(1) 0.0469 1.0000 Uani C216 c 0.19935(12) 0.2512(3) 0.7385(1) 0.0407 1.0000 Uani C301 c 0.08679(11) 0.2662(3) 0.69738(9) 0.0332 1.0000 Uani C302 c 0.09099(11) 0.3867(3) 0.70962(9) 0.0337 1.0000 Uani C303 c 0.08149(12) 0.4192(3) 0.74783(9) 0.0404 1.0000 Uani C304 c 0.06857(13) 0.3270(4) 0.7735(1) 0.0480 1.0000 Uani C305 c 0.06396(13) 0.2047(3) 0.7612(1) 0.0468 1.0000 Uani C306 c 0.07256(11) 0.1737(3) 0.72303(9) 0.0388 1.0000 Uani C311 c 0.04152(11) 0.2024(3) 0.62340(9) 0.0329 1.0000 Uani C312 c -0.00016(12) 0.2665(3) 0.6355(1) 0.0420 1.0000 Uani C313 c -0.04570(12) 0.2489(4) 0.61690(11) 0.0512 1.0000 Uani C314 c -0.05013(13) 0.1666(4) 0.58629(11) 0.0509 1.0000 Uani C315 c -0.00956(13) 0.1019(3) 0.5739(1) 0.0456 1.0000 Uani C316 c 0.03623(12) 0.1204(3) 0.59215(9) 0.0375 1.0000 Uani H11 h 0.21771 -0.0476 0.6481 0.0480 1.0000 Uiso H12 h 0.24615 -0.0050 0.6092 0.0480 1.0000 Uiso H13 h 0.19114 -0.0661 0.6050 0.0480 1.0000 Uiso H101 h 0.0490 0.4637 0.61508 0.0431 1.0000 Uiso H102 h 0.0822 0.5553 0.59310 0.0431 1.0000 Uiso H111 h 0.21702 0.1661 0.57041 0.0463 1.0000 Uiso H112 h 0.16023 0.1157 0.56770 0.0463 1.0000 Uiso H201 h 0.16201 0.6352 0.64181 0.0415 1.0000 Uiso H202 h 0.16581 0.6035 0.59790 0.0415 1.0000 Uiso H211 h 0.23390 0.1512 0.67427 0.0434 1.0000 Uiso H212 h 0.25698 0.2092 0.63493 0.0434 1.0000 Uiso H301 h 0.13053 0.5315 0.69447 0.0385 1.0000 Uiso H302 h 0.07856 0.5281 0.67404 0.0385 1.0000 Uiso H311 h 0.14661 0.0697 0.67050 0.0421 1.0000 Uiso H312 h 0.12080 0.0377 0.62791 0.0421 1.0000 Uiso H421 h -0.0133 0.6264 0.71055 0.1219 1.0000 Uiso H422 h -0.0132 0.7773 0.71332 0.1219 1.0000 Uiso H423 h -0.0594 0.7058 0.69143 0.1219 1.0000 Uiso H431 h 0.01187 0.8146 0.61074 0.1190 1.0000 Uiso H432 h 0.00287 0.8976 0.64964 0.1190 1.0000 Uiso H433 h -0.04340 0.8261 0.62776 0.1190 1.0000 Uiso H1031 h -0.00571 0.4599 0.5548 0.0544 1.0000 Uiso H1041 h -0.01932 0.3418 0.4962 0.0614 1.0000 Uiso H1051 h 0.04612 0.2254 0.4700 0.0625 1.0000 Uiso H1061 h 0.12450 0.2164 0.5031 0.0554 1.0000 Uiso H1121 h 0.15212 0.5168 0.5199 0.0624 1.0000 Uiso H1131 h 0.20845 0.6339 0.48269 0.0886 1.0000 Uiso H1141 h 0.2944 0.5982 0.49087 0.0960 1.0000 Uiso H1151 h 0.32477 0.4433 0.53427 0.0832 1.0000 Uiso H1161 h 0.26908 0.3248 0.57215 0.0614 1.0000 Uiso H2031 h 0.24258 0.7351 0.6005 0.0518 1.0000 Uiso H2041 h 0.32994 0.7132 0.60794 0.0611 1.0000 Uiso H2051 h 0.36540 0.5399 0.64058 0.0606 1.0000 Uiso H2061 h 0.31369 0.3843 0.6675 0.0523 1.0000 Uiso H2121 h 0.21453 0.5494 0.71840 0.0439 1.0000 Uiso H2131 h 0.20505 0.5647 0.7874 0.0540 1.0000 Uiso H2141 h 0.19521 0.3822 0.8254 0.0581 1.0000 Uiso H2151 h 0.19238 0.1851 0.7946 0.0562 1.0000 Uiso H2161 h 0.19712 0.1681 0.7257 0.0487 1.0000 Uiso H3031 h 0.08393 0.5073 0.75657 0.0487 1.0000 Uiso H3041 h 0.06248 0.3485 0.8013 0.0578 1.0000 Uiso H3051 h 0.05438 0.1391 0.7800 0.0563 1.0000 Uiso H3061 h 0.06865 0.0862 0.71388 0.0466 1.0000 Uiso H3121 h 0.00307 0.3256 0.6579 0.0504 1.0000 Uiso H3131 h -0.07518 0.2956 0.62558 0.0615 1.0000 Uiso H3141 h -0.08306 0.1535 0.57285 0.0607 1.0000 Uiso H3151 h -0.01331 0.0418 0.5518 0.0545 1.0000 Uiso H3161 h 0.06563 0.0746 0.58287 0.0450 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 Co1 0.0341(2) 0.0231(2) 0.0269(2) 0.00067(16) 0.00188(15) 0.00015(17) P1 0.0413(4) 0.0279(4) 0.0294(4) -0.0005(3) 0.0047(3) -0.0023(3) P2 0.0335(4) 0.0260(4) 0.0323(4) -0.0002(3) 0.0008(3) -0.0011(3) P3 0.0318(4) 0.0254(4) 0.0318(4) 0.0015(3) 0.0025(3) -0.0001(3) P4 0.0492(5) 0.0358(5) 0.0424(5) -0.0018(4) -0.0002(4) -0.0062(4) P5 0.0643(6) 0.0309(5) 0.0478(5) 0.0019(4) 0.0063(4) -0.0012(4) P6 0.0598(7) 0.0619(7) 0.0884(9) 0.0035(6) 0.0194(6) 0.0008(6) F41 0.0527(12) 0.0576(13) 0.0581(13) -0.001(1) -0.004(1) 0.004(1) F42 0.0693(16) 0.0383(13) 0.134(2) -0.0127(14) -0.0029(15) -0.0117(11) F43 0.0943(18) 0.0834(17) 0.0408(12) -0.0014(12) -0.0064(12) 0.0051(14) F44 0.0457(12) 0.0654(16) 0.114(2) -0.0259(15) -0.0123(13) -0.0003(11) F45 0.0877(18) 0.0470(14) 0.111(2) 0.0256(14) -0.0099(15) -0.0220(13) F46 0.0759(17) 0.166(3) 0.0541(14) -0.0282(17) 0.0159(13) -0.0208(19) F51 0.0668(15) 0.0572(14) 0.0865(17) 0.0082(13) -0.0163(13) -0.0067(12) F52 0.1024(19) 0.0437(13) 0.0854(17) 0.0010(12) 0.0284(15) -0.0215(13) F53 0.111(2) 0.0564(15) 0.0771(17) -0.0133(13) 0.0353(15) -0.0000(14) F54 0.112(2) 0.0584(15) 0.0672(15) 0.0123(12) -0.0144(14) 0.0131(14) F55 0.0740(15) 0.0512(13) 0.0712(15) 0.0087(11) -0.0041(12) -0.0178(11) F56 0.0872(17) 0.0630(16) 0.0635(14) -0.0106(12) 0.0202(13) 0.0056(13) F61 0.103(2) 0.0668(18) 0.141(3) 0.0243(18) 0.020(2) -0.0045(16) F62 0.148(3) 0.165(4) 0.101(3) -0.030(2) 0.017(2) 0.064(3) F63 0.089(2) 0.132(3) 0.221(5) -0.049(3) -0.057(3) 0.032(2) F64 0.145(4) 0.079(2) 0.295(6) 0.010(3) 0.042(4) -0.032(2) F65 0.144(3) 0.155(4) 0.119(3) -0.003(3) 0.072(3) 0.011(3) F66 0.106(2) 0.113(3) 0.121(3) 0.028(2) -0.009(2) 0.028(2) O1 0.101(3) 0.115(3) 0.067(2) -0.0156(19) -0.0065(18) 0.068(2) N1 0.0443(15) 0.0288(14) 0.0346(14) 0.0001(11) -0.0026(11) 0.0018(12) N2 0.0417(14) 0.0302(14) 0.0320(13) 0.0016(11) 0.0038(11) 0.0005(12) N3 0.0351(14) 0.0258(13) 0.0352(14) 0.0026(11) 0.0039(11) -0.0005(11) C1 0.0384(18) 0.0308(17) 0.0509(19) -0.0031(15) 0.0001(15) 0.0037(14) C2 0.0366(16) 0.0251(15) 0.0376(16) -0.0030(13) -0.0001(13) 0.0032(13) C11 0.0468(18) 0.0310(16) 0.0380(17) -0.0044(14) 0.0074(14) 0.0031(14) C21 0.0359(17) 0.0306(17) 0.0420(18) -0.0029(14) 0.0004(14) 0.0026(14) C31 0.0378(17) 0.0237(16) 0.0437(18) 0.0033(13) 0.0025(14) -0.0008(13) C41 0.059(2) 0.057(2) 0.058(2) 0.0023(19) 0.0080(19) 0.012(2) C42 0.116(5) 0.111(5) 0.077(3) 0.003(3) 0.034(3) 0.020(4) C43 0.071(3) 0.096(4) 0.130(5) 0.052(4) 0.009(3) 0.012(3) C101 0.0513(19) 0.0320(17) 0.0293(15) 0.0043(13) 0.0036(14) -0.0071(15) C102 0.0451(18) 0.0296(16) 0.0337(16) 0.0074(13) -0.0022(13) -0.0032(15) C103 0.055(2) 0.0334(18) 0.048(2) 0.0097(16) -0.0106(16) -0.0043(16) C104 0.067(2) 0.041(2) 0.046(2) 0.0096(17) -0.0176(18) -0.0100(18) C105 0.074(3) 0.049(2) 0.0329(18) -0.0000(16) -0.0090(17) -0.014(2) C106 0.060(2) 0.045(2) 0.0339(17) -0.0039(15) 0.0000(16) -0.0066(17) C111 0.052(2) 0.0303(17) 0.0362(17) -0.0068(14) 0.0163(14) -0.0081(15) C112 0.066(2) 0.041(2) 0.048(2) 0.0042(17) 0.0216(18) -0.0044(18) C113 0.093(4) 0.059(3) 0.069(3) 0.015(2) 0.035(3) -0.010(2) C114 0.100(4) 0.060(3) 0.080(3) -0.001(2) 0.051(3) -0.023(3) C115 0.060(3) 0.068(3) 0.080(3) -0.019(2) 0.035(2) -0.013(2) C116 0.055(2) 0.049(2) 0.049(2) -0.0128(17) 0.0163(17) -0.0047(17) C201 0.0374(17) 0.0304(16) 0.0346(16) -0.0044(13) 0.0041(13) -0.0049(14) C202 0.0437(18) 0.0278(16) 0.0321(15) -0.0074(13) 0.0063(13) -0.0058(14) C203 0.054(2) 0.0315(18) 0.0438(19) -0.0025(15) 0.0116(15) -0.0067(16) C204 0.054(2) 0.042(2) 0.058(2) -0.0078(17) 0.0182(17) -0.0169(18) C205 0.0376(19) 0.051(2) 0.063(2) -0.0092(18) 0.0104(17) -0.0093(17) C206 0.0389(18) 0.047(2) 0.0449(19) -0.0024(16) -0.0015(15) -0.0061(15) C211 0.0333(16) 0.0356(17) 0.0353(16) 0.0016(14) -0.0038(13) -0.0000(14) C212 0.0386(17) 0.0346(18) 0.0366(17) -0.0004(14) -0.0071(14) -0.0045(14) C213 0.0456(19) 0.052(2) 0.0376(18) -0.0092(16) -0.0040(15) -0.0036(17) C214 0.051(2) 0.062(2) 0.0324(17) 0.0009(17) -0.0043(15) -0.0010(18) C215 0.051(2) 0.051(2) 0.0378(18) 0.0143(16) -0.0016(15) -0.0016(17) C216 0.0385(18) 0.0349(18) 0.048(2) 0.0070(15) -0.0027(15) 0.0011(15) C301 0.0322(16) 0.0363(17) 0.0313(16) 0.0007(13) 0.0012(12) -0.0008(13) C302 0.0321(16) 0.0359(17) 0.0334(16) 0.0042(13) 0.0046(13) 0.0017(13) C303 0.0430(18) 0.0406(18) 0.0382(17) -0.0006(15) 0.0081(14) -0.0002(15) C304 0.053(2) 0.057(2) 0.0352(17) 0.0028(16) 0.0094(15) -0.0056(18) C305 0.048(2) 0.053(2) 0.0398(19) 0.0143(16) 0.0069(15) -0.0057(17) C306 0.0364(17) 0.0354(17) 0.0446(18) 0.0059(15) 0.0002(14) -0.0044(14) C311 0.0319(16) 0.0300(16) 0.0370(16) 0.0060(13) 0.0027(13) -0.0026(13) C312 0.0353(17) 0.049(2) 0.0418(18) -0.0022(16) 0.0024(14) 0.0004(15) C313 0.0346(18) 0.069(3) 0.050(2) -0.0021(19) 0.0009(15) 0.0043(18) C314 0.0381(19) 0.064(2) 0.050(2) 0.0041(19) -0.0095(15) -0.0057(18) C315 0.052(2) 0.044(2) 0.0395(18) -0.0002(15) -0.0052(15) -0.0089(17) C316 0.0421(18) 0.0305(16) 0.0398(17) -0.0000(14) 0.0018(14) -0.0018(14) 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 Co1 . P1 . 2.2067(9) yes Co1 . P2 . 2.1958(9) yes Co1 . P3 . 2.1954(9) yes Co1 . N1 . 2.024(3) yes Co1 . N2 . 2.048(3) yes Co1 . N3 . 2.032(2) yes P1 . C11 . 1.832(3) yes P1 . C101 . 1.799(3) yes P1 . C111 . 1.808(3) yes P2 . C21 . 1.829(3) yes P2 . C201 . 1.805(3) yes P2 . C211 . 1.806(3) yes P3 . C31 . 1.828(3) yes P3 . C301 . 1.809(3) yes P3 . C311 . 1.814(3) yes P4 . F41 . 1.605(2) yes P4 . F42 . 1.581(2) yes P4 . F43 . 1.558(2) yes P4 . F44 . 1.578(2) yes P4 . F45 . 1.588(2) yes P4 . F46 . 1.591(3) yes P5 . F51 . 1.599(2) yes P5 . F52 . 1.591(2) yes P5 . F53 . 1.581(2) yes P5 . F54 . 1.589(3) yes P5 . F55 . 1.583(2) yes P5 . F56 . 1.616(2) yes P6 . F61 . 1.566(3) yes P6 . F62 . 1.565(3) yes P6 . F63 . 1.564(4) yes P6 . F64 . 1.565(4) yes P6 . F65 . 1.570(4) yes P6 . F66 . 1.589(3) yes O1 . C41 . 1.200(5) yes N1 . C102 . 1.466(4) yes N1 . H101 . 0.950 no N1 . H102 . 0.950 no N2 . C202 . 1.462(4) yes N2 . H201 . 0.950 no N2 . H202 . 0.950 no N3 . C302 . 1.466(4) yes N3 . H301 . 0.950 no N3 . H302 . 0.950 no C1 . C2 . 1.543(4) yes C1 . H11 . 1.000 no C1 . H12 . 1.000 no C1 . H13 . 1.000 no C2 . C11 . 1.536(4) yes C2 . C21 . 1.548(4) yes C2 . C31 . 1.548(4) yes C11 . H111 . 1.000 no C11 . H112 . 1.000 no C21 . H211 . 1.000 no C21 . H212 . 1.000 no C31 . H311 . 1.000 no C31 . H312 . 1.000 no C41 . C42 . 1.462(6) yes C41 . C43 . 1.477(6) yes C42 . H421 . 1.000 no C42 . H422 . 1.000 no C42 . H423 . 1.000 no C43 . H431 . 1.000 no C43 . H432 . 1.000 no C43 . H433 . 1.000 no C101 . C102 . 1.385(5) yes C101 . C106 . 1.396(5) yes C102 . C103 . 1.386(5) yes C103 . C104 . 1.388(5) yes C103 . H1031 . 1.000 no C104 . C105 . 1.388(6) yes C104 . H1041 . 1.000 no C105 . C106 . 1.376(5) yes C105 . H1051 . 1.000 no C106 . H1061 . 1.000 no C111 . C112 . 1.389(5) yes C111 . C116 . 1.389(5) yes C112 . C113 . 1.388(5) yes C112 . H1121 . 1.000 no C113 . C114 . 1.371(7) yes C113 . H1131 . 1.000 no C114 . C115 . 1.377(7) yes C114 . H1141 . 1.000 no C115 . C116 . 1.394(5) yes C115 . H1151 . 1.000 no C116 . H1161 . 1.000 no C201 . C202 . 1.385(4) yes C201 . C206 . 1.400(5) yes C202 . C203 . 1.390(4) yes C203 . C204 . 1.385(5) yes C203 . H2031 . 1.000 no C204 . C205 . 1.379(5) yes C204 . H2041 . 1.000 no C205 . C206 . 1.389(5) yes C205 . H2051 . 1.000 no C206 . H2061 . 1.000 no C211 . C212 . 1.397(4) yes C211 . C216 . 1.399(4) yes C212 . C213 . 1.395(4) yes C212 . H2121 . 1.000 no C213 . C214 . 1.383(5) yes C213 . H2131 . 1.000 no C214 . C215 . 1.382(5) yes C214 . H2141 . 1.000 no C215 . C216 . 1.381(5) yes C215 . H2151 . 1.000 no C216 . H2161 . 1.000 no C301 . C302 . 1.371(4) yes C301 . C306 . 1.395(4) yes C302 . C303 . 1.390(4) yes C303 . C304 . 1.383(5) yes C303 . H3031 . 1.000 no C304 . C305 . 1.392(5) yes C304 . H3041 . 1.000 no C305 . C306 . 1.378(5) yes C305 . H3051 . 1.000 no C306 . H3061 . 1.000 no C311 . C312 . 1.402(4) yes C311 . C316 . 1.394(4) yes C312 . C313 . 1.383(5) yes C312 . H3121 . 1.000 no C313 . C314 . 1.378(5) yes C313 . H3131 . 1.000 no C314 . C315 . 1.384(5) yes C314 . H3141 . 1.000 no C315 . C316 . 1.384(5) yes C315 . H3151 . 1.000 no C316 . H3161 . 1.000 no C315 . C316 . 1.384(5) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag P1 . Co1 . P2 . 90.27(3) yes P1 . Co1 . P3 . 89.54(3) yes P2 . Co1 . P3 . 89.81(3) yes P1 . Co1 . N1 . 85.48(8) yes P2 . Co1 . N1 . 175.22(8) yes P3 . Co1 . N1 . 92.34(8) yes P1 . Co1 . N2 . 93.58(7) yes P2 . Co1 . N2 . 85.64(8) yes P3 . Co1 . N2 . 174.49(8) yes N1 . Co1 . N2 . 92.4(1) yes P1 . Co1 . N3 . 173.85(8) yes P2 . Co1 . N3 . 93.32(8) yes P3 . Co1 . N3 . 85.48(7) yes N1 . Co1 . N3 . 91.1(1) yes N2 . Co1 . N3 . 91.7(1) yes Co1 . P1 . C11 . 115.1(1) yes Co1 . P1 . C101 . 100.13(11) yes C11 . P1 . C101 . 109.27(15) yes Co1 . P1 . C111 . 119.3(1) yes C11 . P1 . C111 . 106.62(15) yes C101 . P1 . C111 . 105.57(15) yes Co1 . P2 . C21 . 115.1(1) yes Co1 . P2 . C201 . 100.84(11) yes C21 . P2 . C201 . 109.40(15) yes Co1 . P2 . C211 . 117.3(1) yes C21 . P2 . C211 . 107.04(15) yes C201 . P2 . C211 . 106.48(14) yes Co1 . P3 . C31 . 115.0(1) yes Co1 . P3 . C301 . 100.6(1) yes C31 . P3 . C301 . 109.92(14) yes Co1 . P3 . C311 . 118.3(1) yes C31 . P3 . C311 . 107.70(14) yes C301 . P3 . C311 . 104.35(14) yes F41 . P4 . F42 . 90.02(13) yes F41 . P4 . F43 . 90.23(13) yes F42 . P4 . F43 . 91.02(16) yes F41 . P4 . F44 . 178.11(15) yes F42 . P4 . F44 . 90.94(14) yes F43 . P4 . F44 . 91.39(15) yes F41 . P4 . F45 . 89.35(13) yes F42 . P4 . F45 . 178.70(16) yes F43 . P4 . F45 . 90.11(16) yes F44 . P4 . F45 . 89.67(14) yes F41 . P4 . F46 . 88.89(14) yes F42 . P4 . F46 . 88.28(17) yes F43 . P4 . F46 . 178.88(15) yes F44 . P4 . F46 . 89.51(15) yes F45 . P4 . F46 . 90.57(17) yes F51 . P5 . F52 . 89.82(15) yes F51 . P5 . F53 . 90.34(15) yes F52 . P5 . F53 . 90.84(14) yes F51 . P5 . F54 . 178.56(16) yes F52 . P5 . F54 . 90.49(15) yes F53 . P5 . F54 . 91.06(16) yes F51 . P5 . F55 . 89.68(13) yes F52 . P5 . F55 . 178.50(14) yes F53 . P5 . F55 . 90.57(14) yes F54 . P5 . F55 . 89.98(14) yes F51 . P5 . F56 . 88.77(14) yes F52 . P5 . F56 . 87.83(13) yes F53 . P5 . F56 . 178.40(16) yes F54 . P5 . F56 . 89.84(14) yes F55 . P5 . F56 . 90.75(14) yes F61 . P6 . F62 . 90.3(2) yes F61 . P6 . F63 . 89.7(2) yes F62 . P6 . F63 . 91.4(2) yes F61 . P6 . F64 . 178.4(3) yes F62 . P6 . F64 . 90.5(3) yes F63 . P6 . F64 . 91.7(3) yes F61 . P6 . F65 . 88.1(2) yes F62 . P6 . F65 . 177.3(3) yes F63 . P6 . F65 . 90.8(2) yes F64 . P6 . F65 . 91.0(3) yes F61 . P6 . F66 . 90.4(2) yes F62 . P6 . F66 . 86.9(2) yes F63 . P6 . F66 . 178.3(2) yes F64 . P6 . F66 . 88.3(2) yes F65 . P6 . F66 . 90.9(2) yes Co1 . N1 . C102 . 115.89(19) yes Co1 . N1 . H101 . 107.84 no C102 . N1 . H101 . 107.85 no Co1 . N1 . H102 . 107.84 no C102 . N1 . H102 . 107.84 no H101 . N1 . H102 . 109.467 no Co1 . N2 . C202 . 115.47(19) yes Co1 . N2 . H201 . 107.95 no C202 . N2 . H201 . 107.95 no Co1 . N2 . H202 . 107.95 no C202 . N2 . H202 . 107.95 no H201 . N2 . H202 . 109.467 no Co1 . N3 . C302 . 115.86(19) yes Co1 . N3 . H301 . 107.85 no C302 . N3 . H301 . 107.85 no Co1 . N3 . H302 . 107.85 no C302 . N3 . H302 . 107.85 no H301 . N3 . H302 . 109.466 no C2 . C1 . H11 . 109.47 no C2 . C1 . H12 . 109.47 no H11 . C1 . H12 . 109.476 no C2 . C1 . H13 . 109.47 no H11 . C1 . H13 . 109.475 no H12 . C1 . H13 . 109.477 no C1 . C2 . C11 . 107.7(2) yes C1 . C2 . C21 . 106.9(2) yes C11 . C2 . C21 . 111.5(3) yes C1 . C2 . C31 . 106.6(2) yes C11 . C2 . C31 . 111.9(3) yes C21 . C2 . C31 . 111.9(2) yes P1 . C11 . C2 . 116.6(2) yes P1 . C11 . H111 . 107.7 no C2 . C11 . H111 . 107.66 no P1 . C11 . H112 . 107.66 no C2 . C11 . H112 . 107.66 no H111 . C11 . H112 . 109.467 no P2 . C21 . C2 . 116.5(2) yes P2 . C21 . H211 . 107.7 no C2 . C21 . H211 . 107.68 no P2 . C21 . H212 . 107.7 no C2 . C21 . H212 . 107.68 no H211 . C21 . H212 . 109.466 no P3 . C31 . C2 . 117.0(2) yes P3 . C31 . H311 . 107.6 no C2 . C31 . H311 . 107.57 no P3 . C31 . H312 . 107.6 no C2 . C31 . H312 . 107.57 no H311 . C31 . H312 . 109.466 no O1 . C41 . C42 . 121.0(4) yes O1 . C41 . C43 . 121.6(4) yes C42 . C41 . C43 . 117.4(4) yes C41 . C42 . H421 . 109.5 no C41 . C42 . H422 . 109.5 no H421 . C42 . H422 . 109.475 no C41 . C42 . H423 . 109.5 no H421 . C42 . H423 . 109.476 no H422 . C42 . H423 . 109.477 no C41 . C43 . H431 . 109.5 no C41 . C43 . H432 . 109.5 no H431 . C43 . H432 . 109.475 no C41 . C43 . H433 . 109.5 no H431 . C43 . H433 . 109.478 no H432 . C43 . H433 . 109.476 no P1 . C101 . C102 . 116.1(2) yes P1 . C101 . C106 . 124.4(3) yes C102 . C101 . C106 . 119.5(3) yes N1 . C102 . C101 . 117.6(3) yes N1 . C102 . C103 . 120.9(3) yes C101 . C102 . C103 . 121.4(3) yes C102 . C103 . C104 . 118.5(4) yes C102 . C103 . H1031 . 120.8 no C104 . C103 . H1031 . 120.8 no C103 . C104 . C105 . 120.5(3) yes C103 . C104 . H1041 . 119.8 no C105 . C104 . H1041 . 119.8 no C104 . C105 . C106 . 120.7(3) yes C104 . C105 . H1051 . 119.6 no C106 . C105 . H1051 . 119.6 no C101 . C106 . C105 . 119.4(4) yes C101 . C106 . H1061 . 120.3 no C105 . C106 . H1061 . 120.3 no P1 . C111 . C112 . 118.3(3) yes P1 . C111 . C116 . 121.6(3) yes C112 . C111 . C116 . 120.1(3) yes C111 . C112 . C113 . 120.3(4) yes C111 . C112 . H1121 . 119.9 no C113 . C112 . H1121 . 119.9 no C112 . C113 . C114 . 119.6(4) yes C112 . C113 . H1131 . 120.2 no C114 . C113 . H1131 . 120.2 no C113 . C114 . C115 . 120.6(4) yes C113 . C114 . H1141 . 119.7 no C115 . C114 . H1141 . 119.7 no C114 . C115 . C116 . 120.6(4) yes C114 . C115 . H1151 . 119.7 no C116 . C115 . H1151 . 119.7 no C111 . C116 . C115 . 118.8(4) yes C111 . C116 . H1161 . 120.6 no C115 . C116 . H1161 . 120.6 no P2 . C201 . C202 . 115.9(2) yes P2 . C201 . C206 . 123.8(3) yes C202 . C201 . C206 . 120.4(3) yes N2 . C202 . C201 . 118.3(3) yes N2 . C202 . C203 . 121.1(3) yes C201 . C202 . C203 . 120.6(3) yes C202 . C203 . C204 . 118.7(3) yes C202 . C203 . H2031 . 120.7 no C204 . C203 . H2031 . 120.7 no C203 . C204 . C205 . 121.3(3) yes C203 . C204 . H2041 . 119.4 no C205 . C204 . H2041 . 119.4 no C204 . C205 . C206 . 120.3(3) yes C204 . C205 . H2051 . 119.8 no C206 . C205 . H2051 . 119.8 no C201 . C206 . C205 . 118.8(3) yes C201 . C206 . H2061 . 120.6 no C205 . C206 . H2061 . 120.6 no P2 . C211 . C212 . 118.5(2) yes P2 . C211 . C216 . 121.6(2) yes C212 . C211 . C216 . 119.7(3) yes C211 . C212 . C213 . 119.7(3) yes C211 . C212 . H2121 . 120.15 no C213 . C212 . H2121 . 120.1 no C212 . C213 . C214 . 120.1(3) yes C212 . C213 . H2131 . 119.9 no C214 . C213 . H2131 . 119.9 no C213 . C214 . C215 . 120.0(3) yes C213 . C214 . H2141 . 120.0 no C215 . C214 . H2141 . 120.0 no C214 . C215 . C216 . 120.8(3) yes C214 . C215 . H2151 . 119.6 no C216 . C215 . H2151 . 119.6 no C211 . C216 . C215 . 119.6(3) yes C211 . C216 . H2161 . 120.19 no C215 . C216 . H2161 . 120.2 no P3 . C301 . C302 . 115.7(2) yes P3 . C301 . C306 . 123.8(2) yes C302 . C301 . C306 . 120.6(3) yes N3 . C302 . C301 . 118.4(3) yes N3 . C302 . C303 . 120.8(3) yes C301 . C302 . C303 . 120.8(3) yes C302 . C303 . C304 . 118.6(3) yes C302 . C303 . H3031 . 120.71 no C304 . C303 . H3031 . 120.7 no C303 . C304 . C305 . 120.8(3) yes C303 . C304 . H3041 . 119.6 no C305 . C304 . H3041 . 119.58 no C304 . C305 . C306 . 120.2(3) yes C304 . C305 . H3051 . 119.92 no C306 . C305 . H3051 . 119.9 no C301 . C306 . C305 . 119.0(3) yes C301 . C306 . H3061 . 120.51 no C305 . C306 . H3061 . 120.5 no P3 . C311 . C312 . 118.3(2) yes P3 . C311 . C316 . 122.9(2) yes C312 . C311 . C316 . 118.7(3) yes C311 . C312 . C313 . 120.8(3) yes C311 . C312 . H3121 . 119.62 no C313 . C312 . H3121 . 119 no C312 . C313 . C314 . 119.5(3) yes C312 . C313 . H3131 . 120.3 no C314 . C313 . H3131 . 120.3 no C313 . C314 . C315 . 120.8(3) yes C313 . C314 . H3141 . 119.6 no C315 . C314 . H3141 . 119.6 no C314 . C315 . C316 . 119.9(3) yes C314 . C315 . H3151 . 120.0 no C316 . C315 . H3151 . 120.0 no C311 . C316 . C315 . 120.3(3) yes C311 . C316 . H3161 . 119.86 no C315 . C316 . H3161 . 119.9 no #------------------------------------------------------------------------------ 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 F41 C112 3.192(4) . . no F41 N2 3.204(3) . . no F41 C113 3.277(5) . . no F41 C114 3.404(5) . 4_566 no F41 C203 3.464(4) . . no F41 C1 3.547(4) . 1_565 no F42 C11 3.169(4) . 1_565 no F42 C114 3.324(6) . 4_566 no F42 C316 3.516(4) . 1_565 no F42 C106 3.572(4) . 1_565 no F43 C314 3.395(4) . 2_566 no F44 C104 3.168(4) . 2_566 no F44 C105 3.264(5) . 2_566 no F44 C315 3.379(4) . 1_565 no F44 C316 3.443(4) . 1_565 no F45 N1 2.809(3) . . no F45 C102 3.044(4) . . no F45 C104 3.408(5) . 2_566 no F45 C103 3.421(4) . . no F45 C112 3.456(5) . . no F45 N2 3.516(4) . . no F46 C43 3.372(6) . . no F46 C31 3.498(4) . 1_565 no F46 C316 3.509(4) . 1_565 no F46 C1 3.567(4) . 1_565 no F51 C31 3.253(4) . 1_565 no F51 C41 3.349(5) . . no F51 C306 3.454(4) . 1_565 no F51 C43 3.533(6) . . no F51 O1 3.562(4) . . no F52 N3 3.046(3) . . no F52 C303 3.191(4) . . no F52 C42 3.262(6) . 5_556 no F52 O1 3.543(4) . . no F52 C302 3.567(4) . . no F52 C42 3.597(6) . . no F53 C306 3.397(4) . 1_565 no F53 C42 3.533(7) . 5_556 no F53 C305 3.557(4) . 1_565 no F54 C213 3.230(5) . . no F54 C216 3.362(4) . 7_556 no F54 C211 3.408(4) . 7_556 no F54 C212 3.426(4) . . no F55 C31 3.271(4) . 1_565 no F55 C213 3.379(4) . 7_556 no F55 C216 3.538(4) . 1_565 no F55 C212 3.550(4) . 7_556 no F56 N2 3.026(3) . . no F56 N3 3.248(3) . . no F56 C212 3.439(4) . . no F56 C202 3.439(4) . . no F61 C204 3.431(5) . 1_545 no F61 C214 3.583(5) . 7_546 no F62 C21 3.302(5) . . no F62 C213 3.590(5) . 7_546 no F63 C41 3.122(6) . 3_545 no F63 O1 3.273(5) . 3_545 no F63 C42 3.355(7) . 3_545 no F63 C313 3.392(6) . 3_545 no F64 C43 3.334(7) . 3_545 no F64 C105 3.546(7) . 4_556 no F65 C105 3.352(6) . 4_556 no F65 C106 3.460(5) . 4_556 no F66 C116 3.469(5) . . no F66 C1 3.500(5) . . no F66 C113 3.592(5) . 4_556 no F66 C21 3.600(5) . . no O1 N1 2.794(4) . . no O1 N3 2.835(4) . . no C103 C104 3.404(5) . 2_566 no C104 C104 3.583(7) . 2_566 no C305 C305 3.526(7) . 5_556 no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Co1 P1 C11 C2 . . . . -8.6(3) no Co1 P1 C101 C102 . . . . 13.3(3) no Co1 P1 C101 C106 . . . . -166.9(3) no Co1 P1 C111 C112 . . . . -84.0(3) no Co1 P1 C111 C116 . . . . 94.5(3) no Co1 P2 C21 C2 . . . . -11.3(3) no Co1 P2 C201 C202 . . . . 11.8(3) no Co1 P2 C201 C206 . . . . -166.7(3) no Co1 P2 C211 C212 . . . . -72.3(3) no Co1 P2 C211 C216 . . . . 102.1(3) no Co1 P3 C31 C2 . . . . -10.0(3) no Co1 P3 C301 C302 . . . . 13.4(2) no Co1 P3 C301 C306 . . . . -166.6(2) no Co1 P3 C311 C312 . . . . -73.8(3) no Co1 P3 C311 C316 . . . . 101.6(3) no Co1 N1 C102 C101 . . . . -17.4(4) no Co1 N1 C102 C103 . . . . 161.7(2) no Co1 N2 C202 C201 . . . . -15.9(3) no Co1 N2 C202 C203 . . . . 162.9(2) no Co1 N3 C302 C301 . . . . -14.8(3) no Co1 N3 C302 C303 . . . . 164.1(2) no P1 Co1 P2 C21 . . . . -38.9(1) no P1 Co1 P2 C201 . . . . 78.7(1) no P1 Co1 P2 C211 . . . . -166.3(1) no P1 Co1 P3 C31 . . . . 49.9(1) no P1 Co1 P3 C301 . . . . 167.9(1) no P1 Co1 P3 C311 . . . . -79.3(1) no P1 Co1 N1 C102 . . . . 20.7(2) no P1 Co1 N2 C202 . . . . -71.4(2) no P1 C11 C2 C1 . . . . -175.2(2) no P1 C11 C2 C21 . . . . -58.3(3) no P1 C11 C2 C31 . . . . 68.0(3) no P1 C101 C102 N1 . . . . 0.9(4) no P1 C101 C102 C103 . . . . -178.2(3) no P1 C101 C106 C105 . . . . 178.3(3) no P1 C111 C112 C113 . . . . 177.8(3) no P1 C111 C116 C115 . . . . -177.9(3) no P2 Co1 P1 C11 . . . . 48.6(1) no P2 Co1 P1 C101 . . . . 165.5(1) no P2 Co1 P1 C111 . . . . -80.1(1) no P2 Co1 P3 C31 . . . . -40.4(1) no P2 Co1 P3 C301 . . . . 77.7(1) no P2 Co1 P3 C311 . . . . -169.5(1) no P2 Co1 N2 C202 . . . . 18.6(2) no P2 Co1 N3 C302 . . . . -70.9(2) no P2 C21 C2 C1 . . . . -172.3(2) no P2 C21 C2 C11 . . . . 70.3(3) no P2 C21 C2 C31 . . . . -56.0(3) no P2 C201 C202 N2 . . . . 1.3(4) no P2 C201 C202 C203 . . . . -177.5(3) no P2 C201 C206 C205 . . . . 176.2(3) no P2 C211 C212 C213 . . . . 172.5(2) no P2 C211 C216 C215 . . . . -174.2(3) no P3 Co1 P1 C11 . . . . -41.2(1) no P3 Co1 P1 C101 . . . . 75.7(1) no P3 Co1 P1 C111 . . . . -169.9(1) no P3 Co1 P2 C21 . . . . 50.6(1) no P3 Co1 P2 C201 . . . . 168.2(1) no P3 Co1 P2 C211 . . . . -76.7(1) no P3 Co1 N1 C102 . . . . -68.7(2) no P3 Co1 N3 C302 . . . . 18.6(2) no P3 C31 C2 C1 . . . . -174.9(2) no P3 C31 C2 C11 . . . . -57.4(3) no P3 C31 C2 C21 . . . . 68.6(3) no P3 C301 C302 N3 . . . . -0.7(4) no P3 C301 C302 C303 . . . . -179.6(2) no P3 C301 C306 C305 . . . . 178.4(2) no P3 C311 C312 C313 . . . . 175.7(3) no P3 C311 C316 C315 . . . . -176.3(3) no N1 Co1 P1 C11 . . . . -133.6(1) no N1 Co1 P1 C101 . . . . -16.6(1) no N1 Co1 P1 C111 . . . . 97.8(1) no N1 Co1 P3 C31 . . . . 135.4(1) no N1 Co1 P3 C301 . . . . -106.6(1) no N1 Co1 P3 C311 . . . . 6.2(1) no N1 Co1 N2 C202 . . . . -157.0(2) no N1 Co1 N3 C302 . . . . 110.9(2) no N1 C102 C101 C106 . . . . -179.0(3) no N1 C102 C103 C104 . . . . -179.4(3) no N2 Co1 P1 C11 . . . . 134.2(1) no N2 Co1 P1 C101 . . . . -108.8(1) no N2 Co1 P1 C111 . . . . 5.6(1) no N2 Co1 P2 C21 . . . . -132.5(1) no N2 Co1 P2 C201 . . . . -14.9(1) no N2 Co1 P2 C211 . . . . 100.2(1) no N2 Co1 N1 C102 . . . . 114.1(2) no N2 Co1 N3 C302 . . . . -156.6(2) no N2 C202 C201 C206 . . . . 179.8(3) no N2 C202 C203 C204 . . . . -178.2(3) no N3 Co1 P2 C21 . . . . 136.1(1) no N3 Co1 P2 C201 . . . . -106.3(1) no N3 Co1 P2 C211 . . . . 8.7(1) no N3 Co1 P3 C31 . . . . -133.7(1) no N3 Co1 P3 C301 . . . . -15.7(1) no N3 Co1 P3 C311 . . . . 97.1(1) no N3 Co1 N1 C102 . . . . -154.2(2) no N3 Co1 N2 C202 . . . . 111.8(2) no N3 C302 C301 C306 . . . . 179.3(3) no N3 C302 C303 C304 . . . . -177.7(3) no C2 C11 P1 C101 . . . . -120.3(2) no C2 C11 P1 C111 . . . . 126.1(2) no C2 C21 P2 C201 . . . . -123.9(2) no C2 C21 P2 C211 . . . . 121.1(2) no C2 C31 P3 C301 . . . . -122.6(2) no C2 C31 P3 C311 . . . . 124.3(2) no C11 P1 C101 C102 . . . . 134.5(3) no C11 P1 C101 C106 . . . . -45.6(3) no C11 P1 C111 C112 . . . . 143.6(3) no C11 P1 C111 C116 . . . . -37.9(3) no C21 P2 C201 C202 . . . . 133.5(2) no C21 P2 C201 C206 . . . . -44.9(3) no C21 P2 C211 C212 . . . . 156.5(2) no C21 P2 C211 C216 . . . . -29.1(3) no C31 P3 C301 C302 . . . . 135.1(2) no C31 P3 C301 C306 . . . . -44.9(3) no C31 P3 C311 C312 . . . . 153.7(3) no C31 P3 C311 C316 . . . . -30.8(3) no C101 P1 C111 C112 . . . . 27.5(3) no C101 P1 C111 C116 . . . . -154.1(3) no C101 C102 C103 C104 . . . . -0.3(5) no C101 C106 C105 C104 . . . . 0.1(6) no C102 C101 P1 C111 . . . . -111.1(3) no C102 C101 C106 C105 . . . . -1.8(5) no C102 C103 C104 C105 . . . . -1.5(5) no C103 C102 C101 C106 . . . . 2.0(5) no C103 C104 C105 C106 . . . . 1.6(6) no C106 C101 P1 C111 . . . . 68.7(3) no C111 C112 C113 C114 . . . . -0.1(6) no C111 C116 C115 C114 . . . . 0.3(6) no C112 C111 C116 C115 . . . . 0.5(5) no C112 C113 C114 C115 . . . . 0.9(7) no C113 C112 C111 C116 . . . . -0.6(5) no C113 C114 C115 C116 . . . . -1.1(7) no C201 P2 C211 C212 . . . . 39.6(3) no C201 P2 C211 C216 . . . . -146.0(3) no C201 C202 C203 C204 . . . . 0.5(5) no C201 C206 C205 C204 . . . . 1.7(5) no C202 C201 P2 C211 . . . . -111.2(3) no C202 C201 C206 C205 . . . . -2.1(5) no C202 C203 C204 C205 . . . . -0.9(5) no C203 C202 C201 C206 . . . . 1.0(5) no C203 C204 C205 C206 . . . . -0.2(6) no C206 C201 P2 C211 . . . . 70.4(3) no C211 C212 C213 C214 . . . . 2.4(5) no C211 C216 C215 C214 . . . . 1.4(5) no C212 C211 C216 C215 . . . . 0.2(5) no C212 C213 C214 C215 . . . . -0.9(5) no C213 C212 C211 C216 . . . . -2.0(5) no C213 C214 C215 C216 . . . . -1.0(5) no C301 P3 C311 C312 . . . . 36.9(3) no C301 P3 C311 C316 . . . . -147.6(3) no C301 C302 C303 C304 . . . . 1.2(5) no C301 C306 C305 C304 . . . . 1.2(5) no C302 C301 P3 C311 . . . . -109.7(2) no C302 C301 C306 C305 . . . . -1.6(5) no C302 C303 C304 C305 . . . . -1.6(5) no C303 C302 C301 C306 . . . . 0.4(5) no C303 C304 C305 C306 . . . . 0.4(5) no C306 C301 P3 C311 . . . . 70.3(3) no C311 C312 C313 C314 . . . . 0.5(6) no C311 C316 C315 C314 . . . . 1.1(5) no C312 C311 C316 C315 . . . . -0.8(5) no C312 C313 C314 C315 . . . . -0.3(6) no C313 C312 C311 C316 . . . . 0.1(5) no C313 C314 C315 C316 . . . . -0.5(6) no #------------------------------------------------------------------------------ #===END data_rxd21 _database_code_depnum_ccdc_archive 'CCDC 609896' _audit_creation_date 04-12-02 _audit_creation_method CRYSTALS_ver_12-03-99 # 2111738 rxd21 _audit_update_record ; 2004-02-12 - Report on C51 H47 Cl N2 O4 P2 Pt S2 by Anthony C. Willis for Geoff Salem, Roy Doyle and Justine Bennett 2002-02-16 - passes checkcif tests with minor warnings ; #============================================================================== # 4. TEXT _publ_section_abstract #Text of the abstract ; The crystal structure of [Pt(C~25~H~22~NO~2~PS)~2~(CH~3~)Cl] is reported. The molecule is centred on a crystallographic inversion centre with the Cl and methyl group statistically disordered. ; _publ_section_comment #Text of the paper ; The molecule is centred on a crystallographic inversion centre. Initially the structure was refined as [Pt(C~25~H~22~NO~2~PS)~2~Cl~2~], but the displacement parameters of the Cl atom were much larger than those of the Pt or P atoms and there was a major peak in a difference electron density map between the Cl and Pt atoms. This suggested that the compound was, in fact, [Pt(C~25~H~22~NO~2~PS)~2~(CH~3~)Cl], with the chloro and methyl groups statistically disordered. Structures of other four-coordinate Pt compounds with methyl and chloro groups trans to each other which exhibit this feature include [Pt(Et~3~P)~2~(CH~3~)Cl] [Bardi, R.; Piazzesi, A. M.; Bruno, G. (1981) Cryst. Struct. Commun., 10, 807] and [Pt(Ph~3~P)~2~(CH~3~)Cl] [Otto, S.; Roodt, A.; Leipoldt, J. G. (1995) S. Afr. J. Chem., 48, 114]. To model this effect, carbon atom C(26) (occupancy 0.5) was included between the Pt atom and Cl(1) (occupancy now reduced to 0.5). C(26) and Cl(1) were constrained to have equal displacement parameters. Initially the Pt---C and Pt---Cl distances were restrained to values reported for related compounds which did not have the Me/Cl disorder, such as [Pt(Ph~3~P)~2~(CH~3~)Cl] (a different crystal form from the one above) [Bardi, R.; Piazzesi, A. M. (1981) Inorg. Chim. Acta, 47, 249]; [Pt(Me~2~OS)~2~(CH~3~)Cl] [Romeo, R.; Scolaro, L. M.; Nastasi, N.; Mann, B. E.; Bruno, G.; Nicolo, F. (1996) Inorg. Chem., 35, 7691]; and [Pt(p-tolyl~3~As)~2~(CH~3~)Cl] [Otto, S; Roodt, A. (1996) Acta Crystallogr., Sect. C: Cryst. Struct. Commun., 52,1636]. These restraints were removed for the final cycles of refinement. Distances and angles involving Cl(1) and C(26) are probably not reliable as these sites are only 0.27(2)\%A apart. Substitution of the one full-occupancy Cl site by the half-occupancy Cl and C sites lowered the R-factor from 0.033 to 0.023 and is clearly warranted. The biggest peaks in the final difference electron density map were located near the Pt atom. ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions #Captions to figures ; ? ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen for refinement keywords. ; The hydrogen atoms of the methyl group attached to the Pt atom were not located and have not been included. The hydrogen attached to N(1) was refined positionally. The remaining hydrogen atoms were included at idealized positions and ride on the atoms to which they were bonded. ; _publ_section_exptl_prep ; The compound was prepared by JB and recrystallized from diethylether/dichloromethane. The sample ID is PtClMe(1) ; #========================================================================== _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 mixed #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al 2001) ; _computing_molecular_graphics ; ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997) ; #============================================================= _cell_length_a 11.1852(2) _cell_angle_alpha 90 _cell_length_b 17.7100(3) _cell_angle_beta 92.8833(8) _cell_length_c 11.7952(1) _cell_angle_gamma 90 _cell_volume 2333.55(6) _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 21/n 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_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 ' 0.1484 0.1585 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 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_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 ' 0.1246 0.1234 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 ' C51 H47 Cl N2 O4 P2 Pt S2 ' _chemical_formula_moiety ' C51 H47 Cl N2 O4 P2 Pt S2 ' _chemical_compound_source ; ? ; _chemical_formula_weight 1108.55 _cell_measurement_reflns_used 30909 _cell_measurement_theta_min 3 _cell_measurement_theta_max 27 _cell_measurement_temperature 200 _cell_formula_units_Z 2 _exptl_crystal_description ' needle ' _exptl_crystal_colour ' colourless ' _exptl_crystal_size_min 0.05 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_max 0.46 _exptl_crystal_density_diffrn 1.578 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1112.00 _exptl_absorpt_coefficient_mu 3.269 # Sheldrick geometric definitions 0.70 0.85 _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 ' \f and \w scans with CCD ' _diffrn_special_details ; CCD data collecting conditions- phi and omega scans of width 1.9 deg at rate 57 sec/frame, crystal-detector distance 28mm, multiple scan sets so over 90 percent of data collected with 4-fold redundancy or more. ; # Absorption correction loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.030 -1 0 0 0.040 0 1 0 0.025 0 -1 0 0.070 0 0 1 0.220 0 0 -1 0.240 1 -1 0 0.030 -1 1 0 0.020 1 2 0 0.027 -1 -2 0 0.074 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.431 _exptl_absorpt_correction_T_max 0.858 _exptl_absorpt_process_details ; via Gaussian method (Coppens, 1970) implemented in maXus (2000) ; #_diffrn_reflns_av_R_equivalents 0.042 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 200 _diffrn_reflns_number 50772 _reflns_number_total 5360 _diffrn_reflns_av_R_equivalents 0.05 # Number of reflections with Friedels Law is 5360 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 5353 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _reflns_number_gt 3107 _diffrn_reflns_theta_min 4.12 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_full 27.49 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min -14 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 22 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _refine_diff_density_min -1.00 _refine_diff_density_max 0.52 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 3107 _refine_ls_number_parameters 292 _refine_ls_R_factor_gt 0.0227 _refine_ls_wR_factor_ref 0.0259 _refine_ls_goodness_of_fit_ref 1.0291 _refine_ls_shift/su_max 0.0031 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 0.459 0.0617 0.296 ; _refine_ls_extinction_method None _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Mackay, S., Gilmore, C. J.,Edwards, C., Stewart, N. & Shankland, K. (2000). maXus Computer Program for the Solution and Refinement of Crystal Structures. Nonius, The Netherlands, MacScience, Japan & The University of Glasgow. Coppens, P. (1970). The Evaluation of Absorption and Extinction in Single-Crystal Structure Analysis. Crystallographic Computing. F. R. Ahmed, S. R. Hall and C. P. Huber, eds., Munksgaard. Copenhagen. pp 255-270. Carruthers, J.R. & Watkin, D.J. (1979) Acta Cryst., A35, 698-699. 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. Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.8. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Johnson, C.K. (1976) ORTEP-II, A Fortran Thermal-Ellipsoid Plot Program, Report ORNL-5138, Oak Ridge National Laboratory, Oak Ridge, Tennessee, USA. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Pt1 pt 0.5000 0.5000 0.5000 0.0242 1.0000 Uani Cl1 cl 0.3217(3) 0.4297(4) 0.4741(5) 0.0396 0.5000 Uani S1 s 0.56641(11) 0.24987(6) 0.62746(8) 0.0421 1.0000 Uani P1 p 0.48343(7) 0.50264(8) 0.69440(6) 0.0261 1.0000 Uani O1 o 0.6866(3) 0.22356(18) 0.6166(3) 0.0565 1.0000 Uani O2 o 0.4803(4) 0.24268(19) 0.5339(3) 0.0623 1.0000 Uani N1 n 0.5659(4) 0.34113(19) 0.6548(3) 0.0382 1.0000 Uani C1 c 0.6108(3) 0.4547(2) 0.7645(3) 0.0307 1.0000 Uani C2 c 0.6851(3) 0.4923(3) 0.8448(3) 0.0374 1.0000 Uani C3 c 0.7786(4) 0.4564(3) 0.9026(4) 0.0496 1.0000 Uani C4 c 0.8011(4) 0.3810(3) 0.8811(4) 0.0448 1.0000 Uani C5 c 0.7316(4) 0.3428(2) 0.7993(3) 0.0382 1.0000 Uani C6 c 0.6371(3) 0.3789(2) 0.7403(3) 0.0319 1.0000 Uani C7 c 0.5097(4) 0.2060(2) 0.7476(3) 0.0350 1.0000 Uani C8 c 0.5822(4) 0.1614(3) 0.8171(4) 0.0420 1.0000 Uani C9 c 0.5348(4) 0.1285(3) 0.9122(4) 0.0432 1.0000 Uani C10 c 0.4176(4) 0.1404(2) 0.9380(4) 0.0410 1.0000 Uani C11 c 0.3458(4) 0.1854(3) 0.8663(4) 0.0473 1.0000 Uani C12 c 0.3903(4) 0.2174(3) 0.7711(4) 0.0468 1.0000 Uani C13 c 0.3691(5) 0.1070(3) 1.0443(4) 0.0607 1.0000 Uani C14 c 0.4745(3) 0.5968(2) 0.7580(3) 0.0311 1.0000 Uani C15 c 0.4896(4) 0.6607(2) 0.6937(3) 0.0368 1.0000 Uani C16 c 0.4717(4) 0.7318(2) 0.7387(4) 0.0444 1.0000 Uani C17 c 0.4373(4) 0.7395(3) 0.8488(4) 0.0474 1.0000 Uani C18 c 0.4235(5) 0.6754(3) 0.9150(4) 0.0502 1.0000 Uani C19 c 0.4415(5) 0.6043(2) 0.8706(3) 0.0444 1.0000 Uani C20 c 0.3535(3) 0.4593(2) 0.7561(3) 0.0318 1.0000 Uani C21 c 0.2412(4) 0.4899(3) 0.7243(3) 0.0429 1.0000 Uani C22 c 0.1396(4) 0.4650(3) 0.7785(4) 0.0529 1.0000 Uani C23 c 0.1506(4) 0.4113(3) 0.8626(4) 0.0564 1.0000 Uani C24 c 0.2603(5) 0.3810(3) 0.8935(4) 0.0538 1.0000 Uani C25 c 0.3618(4) 0.4052(2) 0.8400(3) 0.0400 1.0000 Uani C26 c 0.6557(19) 0.5642(18) 0.525(3) 0.0396 0.5000 Uani H1 h 0.508(4) 0.370(3) 0.601(4) 0.0456 1.0000 Uiso H21 h 0.6698 0.5469 0.8608 0.0445 1.0000 Uiso H31 h 0.8302 0.4846 0.9598 0.0590 1.0000 Uiso H41 h 0.8674 0.3542 0.9246 0.0535 1.0000 Uiso H51 h 0.7496 0.2888 0.7824 0.0460 1.0000 Uiso H81 h 0.6677 0.1527 0.7996 0.0506 1.0000 Uiso H91 h 0.5870 0.0957 0.9628 0.0518 1.0000 Uiso H111 h 0.2606 0.1946 0.8841 0.0570 1.0000 Uiso H121 h 0.3373 0.2488 0.7189 0.0556 1.0000 Uiso H131 h 0.2830 0.1214 1.0489 0.0733 1.0000 Uiso H132 h 0.4159 0.1268 1.1123 0.0733 1.0000 Uiso H133 h 0.3761 0.0507 1.0418 0.0733 1.0000 Uiso H151 h 0.5137 0.6557 0.6136 0.0442 1.0000 Uiso H161 h 0.4837 0.7777 0.6913 0.0533 1.0000 Uiso H171 h 0.4226 0.7908 0.8808 0.0568 1.0000 Uiso H181 h 0.4002 0.6808 0.9954 0.0607 1.0000 Uiso H191 h 0.4310 0.5585 0.9185 0.0537 1.0000 Uiso H211 h 0.2335 0.5292 0.6635 0.0515 1.0000 Uiso H221 h 0.0591 0.4863 0.7560 0.0638 1.0000 Uiso H231 h 0.0779 0.3942 0.9015 0.0686 1.0000 Uiso H241 h 0.2675 0.3416 0.9543 0.0655 1.0000 Uiso H251 h 0.4417 0.3831 0.8628 0.0484 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 0.02570(8) 0.02953(9) 0.01740(8) 0.00110(15) 0.00117(5) -0.00308(16) Cl1 0.0253(19) 0.0583(16) 0.0354(8) -0.0112(9) 0.0040(15) -0.0132(14) S1 0.0669(7) 0.0323(5) 0.0274(4) -0.0025(4) 0.0057(4) -0.0018(5) P1 0.0301(3) 0.0295(4) 0.0188(3) 0.0013(6) 0.0021(2) -0.0025(7) O1 0.076(2) 0.0458(18) 0.0501(18) -0.0041(15) 0.0326(17) 0.0072(17) O2 0.113(3) 0.0393(17) 0.0326(15) -0.0020(12) -0.0174(18) -0.0149(19) N1 0.057(2) 0.0325(17) 0.0247(15) 0.0005(13) -0.0028(15) -0.0011(16) C1 0.0328(18) 0.033(2) 0.0262(17) 0.0020(14) 0.0037(14) -0.0029(15) C2 0.0406(17) 0.037(2) 0.0338(16) -0.008(2) -0.0060(13) 0.001(2) C3 0.047(3) 0.061(3) 0.040(2) -0.007(2) -0.0112(19) 0.000(2) C4 0.035(2) 0.058(3) 0.041(2) 0.008(2) -0.0031(17) 0.0066(19) C5 0.038(2) 0.044(2) 0.0330(19) 0.0028(17) 0.0055(15) 0.0071(17) C6 0.0360(19) 0.0364(19) 0.0237(16) -0.0006(14) 0.0041(14) -0.0026(15) C7 0.042(2) 0.0319(19) 0.0316(18) -0.0013(15) 0.0014(15) 0.0015(16) C8 0.037(2) 0.048(2) 0.042(2) 0.0049(19) 0.0061(17) 0.0070(18) C9 0.043(2) 0.046(2) 0.041(2) 0.0089(18) 0.0023(18) 0.0042(19) C10 0.043(2) 0.040(2) 0.040(2) -0.0042(17) 0.0050(17) -0.0074(18) C11 0.034(2) 0.045(2) 0.064(3) 0.005(2) 0.0096(19) -0.0018(18) C12 0.040(2) 0.039(2) 0.060(3) 0.007(2) -0.011(2) 0.0015(18) C13 0.067(3) 0.068(3) 0.048(3) -0.001(2) 0.016(2) -0.024(3) C14 0.0316(18) 0.0313(18) 0.0306(17) -0.0026(15) 0.0031(14) -0.0002(15) C15 0.042(2) 0.036(2) 0.0330(19) 0.0004(16) 0.0040(17) -0.0057(17) C16 0.058(3) 0.032(2) 0.043(2) -0.0008(17) 0.003(2) -0.0063(19) C17 0.051(3) 0.039(2) 0.051(3) -0.014(2) 0.001(2) -0.003(2) C18 0.066(3) 0.051(3) 0.035(2) -0.0093(19) 0.013(2) -0.000(2) C19 0.066(3) 0.038(2) 0.0301(19) 0.0022(17) 0.011(2) -0.001(2) C20 0.0340(19) 0.034(2) 0.0274(17) -0.0047(15) 0.0059(14) -0.0046(16) C21 0.0359(17) 0.057(3) 0.0360(18) 0.001(2) 0.0028(14) -0.002(2) C22 0.037(2) 0.072(3) 0.050(3) -0.013(2) 0.0091(19) -0.005(2) C23 0.051(3) 0.063(3) 0.057(3) -0.023(2) 0.028(2) -0.025(2) C24 0.073(3) 0.042(2) 0.049(3) 0.004(2) 0.027(2) -0.013(2) C25 0.047(2) 0.038(2) 0.036(2) 0.0047(17) 0.0120(18) -0.0062(19) C26 0.0253(19) 0.0583(16) 0.0354(8) -0.0112(9) 0.0040(15) -0.0132(14) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pt1 . Cl1 . 2.358(3) yes Pt1 . P1 . 2.3102(7) yes Pt1 . P1 2_666 2.3102(7) yes Pt1 . C26 . 2.09(2) yes Cl1 . C26 2_666 0.27(2) no S1 . O1 . 1.434(4) yes S1 . O2 . 1.433(3) yes S1 . N1 . 1.648(3) yes S1 . C7 . 1.762(4) yes P1 . C1 . 1.821(4) yes P1 . C14 . 1.833(4) yes P1 . C20 . 1.827(4) yes N1 . C6 . 1.420(5) yes N1 . H1 . 1.02(5) no C1 . C2 . 1.398(5) yes C1 . C6 . 1.407(5) yes C2 . C3 . 1.375(6) yes C2 . H21 . 1.000 no C3 . C4 . 1.384(7) yes C3 . H31 . 1.000 no C4 . C5 . 1.385(6) yes C4 . H41 . 1.000 no C5 . C6 . 1.391(5) yes C5 . H51 . 1.000 no C7 . C8 . 1.373(6) yes C7 . C12 . 1.392(6) yes C8 . C9 . 1.393(6) yes C8 . H81 . 1.000 no C9 . C10 . 1.377(6) yes C9 . H91 . 1.000 no C10 . C11 . 1.389(6) yes C10 . C13 . 1.511(6) yes C11 . C12 . 1.374(6) yes C11 . H111 . 1.000 no C12 . H121 . 1.000 no C13 . H131 . 1.000 no C13 . H132 . 1.000 no C13 . H133 . 1.000 no C14 . C15 . 1.378(5) yes C14 . C19 . 1.402(5) yes C15 . C16 . 1.385(6) yes C15 . H151 . 1.000 no C16 . C17 . 1.379(6) yes C16 . H161 . 1.000 no C17 . C18 . 1.391(7) yes C17 . H171 . 1.000 no C18 . C19 . 1.382(6) yes C18 . H181 . 1.000 no C19 . H191 . 1.000 no C20 . C21 . 1.402(6) yes C20 . C25 . 1.377(5) yes C21 . C22 . 1.403(6) yes C21 . H211 . 1.000 no C22 . C23 . 1.375(8) yes C22 . H221 . 1.000 no C23 . C24 . 1.372(8) yes C23 . H231 . 1.000 no C24 . C25 . 1.394(6) yes C24 . H241 . 1.000 no C25 . H251 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 . Pt1 . Cl1 2_666 180.0 no Cl1 . Pt1 . P1 . 91.70(15) yes Cl1 2_666 Pt1 . P1 . 88.30(15) no Cl1 . Pt1 . P1 2_666 88.30(15) yes Cl1 2_666 Pt1 . P1 2_666 91.70(15) no P1 . Pt1 . P1 2_666 180.0 yes Cl1 . Pt1 . C26 . 178.7(10) yes Cl1 2_666 Pt1 . C26 . 1.3(10) no P1 . Pt1 . C26 . 87.6(8) yes P1 2_666 Pt1 . C26 . 92.4(8) yes Cl1 . Pt1 . C26 2_666 1.3(10) no Cl1 2_666 Pt1 . C26 2_666 178.7(10) no P1 . Pt1 . C26 2_666 92.4(8) no P1 2_666 Pt1 . C26 2_666 87.6(8) no C26 . Pt1 . C26 2_666 179.995 no O1 . S1 . O2 . 119.9(2) yes O1 . S1 . N1 . 110.4(2) yes O2 . S1 . N1 . 103.3(2) yes O1 . S1 . C7 . 107.8(2) yes O2 . S1 . C7 . 109.0(2) yes N1 . S1 . C7 . 105.64(18) yes Pt1 . P1 . C1 . 109.94(12) yes Pt1 . P1 . C14 . 115.68(13) yes C1 . P1 . C14 . 107.19(17) yes Pt1 . P1 . C20 . 119.46(12) yes C1 . P1 . C20 . 104.09(18) yes C14 . P1 . C20 . 99.12(17) yes S1 . N1 . C6 . 126.4(3) yes S1 . N1 . H1 . 111.9(26) no C6 . N1 . H1 . 121.7(27) no P1 . C1 . C2 . 120.7(3) yes P1 . C1 . C6 . 121.3(3) yes C2 . C1 . C6 . 118.0(4) yes C1 . C2 . C3 . 121.7(4) yes C1 . C2 . H21 . 119.1 no C3 . C2 . H21 . 119.1 no C2 . C3 . C4 . 119.8(4) yes C2 . C3 . H31 . 120.1 no C4 . C3 . H31 . 120.1 no C3 . C4 . C5 . 119.9(4) yes C3 . C4 . H41 . 120.1 no C5 . C4 . H41 . 120.1 no C4 . C5 . C6 . 120.7(4) yes C4 . C5 . H51 . 119.7 no C6 . C5 . H51 . 119.7 no N1 . C6 . C1 . 118.5(3) yes N1 . C6 . C5 . 121.6(4) yes C1 . C6 . C5 . 119.9(4) yes S1 . C7 . C8 . 120.5(3) yes S1 . C7 . C12 . 118.9(3) yes C8 . C7 . C12 . 120.6(4) yes C7 . C8 . C9 . 119.0(4) yes C7 . C8 . H81 . 120.5 no C9 . C8 . H81 . 120.5 no C8 . C9 . C10 . 121.3(4) yes C8 . C9 . H91 . 119.3 no C10 . C9 . H91 . 119.4 no C9 . C10 . C11 . 118.7(4) yes C9 . C10 . C13 . 120.7(4) yes C11 . C10 . C13 . 120.6(4) yes C10 . C11 . C12 . 120.9(4) yes C10 . C11 . H111 . 119.6 no C12 . C11 . H111 . 119.6 no C7 . C12 . C11 . 119.5(4) yes C7 . C12 . H121 . 120.2 no C11 . C12 . H121 . 120.2 no C10 . C13 . H131 . 109.5 no C10 . C13 . H132 . 109.5 no H131 . C13 . H132 . 109.476 no C10 . C13 . H133 . 109.5 no H131 . C13 . H133 . 109.476 no H132 . C13 . H133 . 109.476 no P1 . C14 . C15 . 120.8(3) yes P1 . C14 . C19 . 119.8(3) yes C15 . C14 . C19 . 119.2(4) yes C14 . C15 . C16 . 120.8(4) yes C14 . C15 . H151 . 119.6 no C16 . C15 . H151 . 119.6 no C15 . C16 . C17 . 120.2(4) yes C15 . C16 . H161 . 119.9 no C17 . C16 . H161 . 119.9 no C16 . C17 . C18 . 119.5(4) yes C16 . C17 . H171 . 120.3 no C18 . C17 . H171 . 120.3 no C17 . C18 . C19 . 120.5(4) yes C17 . C18 . H181 . 119.7 no C19 . C18 . H181 . 119.8 no C14 . C19 . C18 . 119.8(4) yes C14 . C19 . H191 . 120.1 no C18 . C19 . H191 . 120.1 no P1 . C20 . C21 . 116.9(3) yes P1 . C20 . C25 . 123.5(3) yes C21 . C20 . C25 . 119.2(4) yes C20 . C21 . C22 . 119.5(5) yes C20 . C21 . H211 . 120.3 no C22 . C21 . H211 . 120.2 no C21 . C22 . C23 . 120.1(5) yes C21 . C22 . H221 . 120.0 no C23 . C22 . H221 . 120.0 no C22 . C23 . C24 . 120.6(4) yes C22 . C23 . H231 . 119.7 no C24 . C23 . H231 . 119.7 no C23 . C24 . C25 . 119.8(5) yes C23 . C24 . H241 . 120.1 no C25 . C24 . H241 . 120.1 no C20 . C25 . C24 . 120.9(4) yes C20 . C25 . H251 . 119.6 no C24 . C25 . H251 . 119.6 no #------------------------------------------------------------------------------ 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 Cl1 C9 3.414(6) . 4_454 no Cl1 C8 3.565(7) . 4_454 no O1 C24 3.354(6) . 4_554 no O2 C4 3.421(6) . 4_454 no C5 C13 3.559(6) . 4_554 no C6 C13 3.570(6) . 4_554 no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Pt1 P1 C1 C2 . . . . 122.4(3) no Pt1 P1 C1 C6 . . . . -58.0(3) no Pt1 P1 C14 C15 . . . . -6.5(3) no Pt1 P1 C14 C19 . . . . 167.8(3) no Pt1 P1 C20 C21 . . . . -62.0(3) no Pt1 P1 C20 C25 . . . . 125.5(3) no Pt1 P1 C1 C2 . 2_666 2_666 2_666 -122.4(3) no Pt1 P1 C1 C6 . 2_666 2_666 2_666 58.0(3) no Pt1 P1 C14 C15 . 2_666 2_666 2_666 6.5(3) no Pt1 P1 C14 C19 . 2_666 2_666 2_666 -167.8(3) no Pt1 P1 C20 C21 . 2_666 2_666 2_666 62.0(3) no Pt1 P1 C20 C25 . 2_666 2_666 2_666 -125.5(3) no Cl1 Pt1 P1 C1 . . . . 117.9(2) no Cl1 Pt1 P1 C14 . . . . -120.5(2) no Cl1 Pt1 P1 C20 . . . . -2.2(2) no Cl1 Pt1 P1 C1 . . 2_666 2_666 62.1(2) no Cl1 Pt1 P1 C14 . . 2_666 2_666 -59.5(2) no Cl1 Pt1 P1 C20 . . 2_666 2_666 -177.8(2) no S1 N1 C6 C1 . . . . -169.3(3) no S1 N1 C6 C5 . . . . 11.0(6) no S1 C7 C8 C9 . . . . 179.1(4) no S1 C7 C12 C11 . . . . -178.1(4) no P1 C1 C2 C3 . . . . 177.0(3) no P1 C1 C6 N1 . . . . 3.5(5) no P1 C1 C6 C5 . . . . -176.9(3) no P1 C14 C15 C16 . . . . 173.8(3) no P1 C14 C19 C18 . . . . -173.8(4) no P1 C20 C21 C22 . . . . -172.7(4) no P1 C20 C25 C24 . . . . 172.0(3) no O1 S1 N1 C6 . . . . -50.0(4) no O1 S1 C7 C8 . . . . 5.5(4) no O1 S1 C7 C12 . . . . -174.6(3) no O2 S1 N1 C6 . . . . -179.4(4) no O2 S1 C7 C8 . . . . 137.1(4) no O2 S1 C7 C12 . . . . -43.0(4) no N1 S1 C7 C8 . . . . -112.5(4) no N1 S1 C7 C12 . . . . 67.3(4) no N1 C6 C1 C2 . . . . -176.9(3) no N1 C6 C5 C4 . . . . 179.0(4) no C1 P1 Pt1 C26 . . . . -63.2(8) no C1 P1 Pt1 C26 . . . 2_666 116.8(8) no C1 P1 C14 C15 . . . . 116.6(3) no C1 P1 C14 C19 . . . . -69.1(4) no C1 P1 C20 C21 . . . . 174.9(3) no C1 P1 C20 C25 . . . . 2.4(4) no C1 C2 C3 C4 . . . . 0.3(7) no C1 C6 C5 C4 . . . . -0.7(6) no C2 C1 P1 C14 . . . . -4.1(3) no C2 C1 P1 C20 . . . . -108.5(3) no C2 C1 C6 C5 . . . . 2.7(5) no C2 C3 C4 C5 . . . . 1.9(7) no C3 C2 C1 C6 . . . . -2.6(6) no C3 C4 C5 C6 . . . . -1.7(7) no C6 N1 S1 C7 . . . . 66.3(4) no C6 C1 P1 C14 . . . . 175.5(3) no C6 C1 P1 C20 . . . . 71.1(3) no C7 C8 C9 C10 . . . . -0.6(7) no C7 C12 C11 C10 . . . . -1.5(7) no C8 C7 C12 C11 . . . . 1.8(7) no C8 C9 C10 C11 . . . . 0.8(7) no C8 C9 C10 C13 . . . . -177.3(4) no C9 C8 C7 C12 . . . . -0.8(7) no C9 C10 C11 C12 . . . . 0.2(7) no C12 C11 C10 C13 . . . . 178.4(5) no C14 P1 Pt1 C26 . . . . 58.4(8) no C14 P1 Pt1 C26 . . . 2_666 -121.6(8) no C14 P1 C20 C21 . . . . 64.4(3) no C14 P1 C20 C25 . . . . -108.0(3) no C14 C15 C16 C17 . . . . -0.6(7) no C14 C19 C18 C17 . . . . 0.3(8) no C15 C14 P1 C20 . . . . -135.5(3) no C15 C14 C19 C18 . . . . 0.6(7) no C15 C16 C17 C18 . . . . 1.5(7) no C16 C15 C14 C19 . . . . -0.5(6) no C16 C17 C18 C19 . . . . -1.4(8) no C19 C14 P1 C20 . . . . 38.8(4) no C20 P1 Pt1 C26 . . . . 176.6(8) no C20 P1 Pt1 C26 . . . 2_666 -3.4(8) no C20 C21 C22 C23 . . . . 0.4(7) no C20 C25 C24 C23 . . . . -0.1(7) no C21 C20 C25 C24 . . . . -0.3(6) no C21 C22 C23 C24 . . . . -0.7(8) no C22 C21 C20 C25 . . . . 0.1(6) no C22 C23 C24 C25 . . . . 0.5(7) no #------------------------------------------------------------------------------ # start Validation Reply Form _vrf_PUBL024_GLOBAL ; PROBLEM: The number of authors is greater than 5. RESPONSE: Not so: there are 4 only, but listed for each compound. ; # end Validation Reply Form #===END