# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name _publ_author_address 'Geoffrey Salem' ; Department of Chemistry, The Australian National University, Canberra, A. C. T. 0200, Australia ; 'Justine Bennett' ; Department of Chemistry, The Australian National University, Canberra, A. C. T. 0200, Australia ; 'Roy J. Doyle' ; Department of Chemistry, The Australian National University, Canberra, A. C. T. 0200, Australia ; 'Hwi-Young Lee.' ; Department of Chemistry, The Australian National University, Canberra, A. C. T. 0200, Australia ; 'Di Lu.' ; Research School of Chemistry, The Australian National University, Canberra, A. C. T. 0200, Australia ; 'David J. Speldewinde' '' 'Michelle Tifan' '' 'Anthony C. Willis' '' _publ_contact_author_name 'Geoffrey Salem' _publ_contact_author_email GEOFF.SALEM@ANU.EDU.AU _publ_section_title ; Synthesis of 1,3-Azaphosphol-2-ones. Crystal and Molecular Structures of [SP-4-2]-Dichlorobis (3-phenyl-1,3-dihydrobenzo[1,3]azaphosphol-2-one-P)palladium(II) and its Chloro(methyl)platinum(II) Analogue ; _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_name_full ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _publ_contact_author_address ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_contact_author_fax ' 61 2 6125 0750 ' _publ_contact_author_phone ' 61 2 6125 4109 ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_category 'FM ' _publ_requested_coeditor_name ? # # 1. SUBMISSION DETAILS _publ_requested_journal ' test ' # Attachment 'sal0701.cif' data_sal0701 _database_code_depnum_ccdc_archive 'CCDC 744588' _audit_creation_date 07-11-22 _audit_creation_method CRYSTALS_ver_12.18 _audit_update_record ; 2007-11-22 - Report on C27.66 H24 Cl2 N2 O5.00 P2 Pd1 by Anthony C. Willis for Geoff Salem, Roy Doyle and ????? 2007-11-22 - passes checkcif tests with warnings ; _oxford_structure_analysis_title '10151247 sal0701' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 8.6093(2) _cell_length_b 11.3301(3) _cell_length_c 16.3435(5) _cell_angle_alpha 81.4299(12) _cell_angle_beta 83.0012(16) _cell_angle_gamma 77.0439(16) _cell_volume 1529.80(7) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Pd -0.9988 1.0072 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058 76.8986 5.2659 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C27 H30 Cl2 N2 O6 P2 Pd1 # Dc = 1.56 Fooo = 707.91 Mu = 9.28 M = 717.80 # Found Formula = C27.66 H24 Cl2 N2 O5.00 P2 Pd1 # Dc = 1.53 FOOO = 707.91 Mu = 9.24 M = 703.66 _chemical_formula_sum 'C27.66 H29.32 Cl2 N2 O5 P2 Pd' #'C27.66 H24 Cl2 N2 O5.00 P2 Pd1' _chemical_formula_moiety 'C26 H20 Cl2 N2 O2 P2 Pd, 1.66(C H4 O), 1.34(H2 O)' _chemical_compound_source local _chemical_formula_weight 709.02 # 703.66 _cell_measurement_reflns_used 46880 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 200 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_min 0.03 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 1.528 _exptl_crystal_density_meas 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 718.55 # 707.906 _exptl_absorpt_coefficient_mu 0.924 # Sheldrick geometric approximatio 0.93 0.97 # 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 0.200 -1 0 0 0.200 0 1 0 0.015 0 -1 0 0.020 0 0 1 0.040 0 0 -1 0.040 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.794 _exptl_absorpt_correction_T_max 0.969 _exptl_absorpt_process_details ; via Gaussian method (Coppens, 1970) implemented in maXus (2000) ; #_diffrn_reflns_av_R_equivalents 0.041 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method ' \f and \w scans with CCD ' _diffrn_special_details ; CCD data collecting conditions- phi and omega scans of width 1.6 deg at rate 192 sec/frame, crystal-detector distance 30mm, multiple scan sets so over 90 percent of data collected with 2-fold redundancy or more. ; # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius BV, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'CRYSTALS (Watkin et al 2003)' _computing_publication_material 'CRYSTALS (Watkin et al 2003)' _computing_molecular_graphics ; ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997) ; _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 200 _diffrn_reflns_number 34432 _reflns_number_total 7035 _diffrn_reflns_av_R_equivalents 0.043 # Number of reflections with Friedels Law is 7035 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 7049 _diffrn_reflns_theta_min 2.642 _diffrn_reflns_theta_max 27.529 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.529 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min -11 _reflns_limit_h_max 11 _reflns_limit_k_min -14 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _oxford_diffrn_Wilson_B_factor 2.21 _oxford_diffrn_Wilson_scale 8.07 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.58 _refine_diff_density_max 0.69 _refine_ls_number_reflns 4819 _refine_ls_number_restraints 38 _refine_ls_number_parameters 400 #_refine_ls_R_factor_ref 0.0284 _refine_ls_wR_factor_ref 0.0334 _refine_ls_goodness_of_fit_ref 1.1131 #_reflns_number_all 7015 _refine_ls_R_factor_all 0.0489 _refine_ls_wR_factor_all 0.0411 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 4819 _refine_ls_R_factor_gt 0.0284 _refine_ls_wR_factor_gt 0.0334 _refine_ls_shift/su_max 0.027645 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.873 0.175 0.655 ; #============================================================================== # 4. TEXT _publ_section_abstract #Text of the abstract ; The crystal structure of cis-[Pd(C~13~H~10~NOP)~2~Cl~2~].1.66(CH~3~OH).1.34(H~2~O) is reported. ; _publ_section_comment #Text of the paper ; The crystallographic asymmetric unit consists of one cis-[Pd(C~13~H~10~NOP)~2~Cl~2~] molecule and solvate methanol and water molecules. ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions #Captions to figures ; ? ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen for refinement keywords. ; One methanol solvate molecule and one water solvate molecule are clearly observed. There is, however, a region of disordered solvate molecules about the inversion symmetry position (0,1/2,1) where identification of the species present is not so clear. There appear to be one methanol molecule and two sites for water molecules, but they are so close together that they are mutually exclusive. Their populations have therefore been restrained to sum to 1.0. Restraints were imposed on the C---O distance of the methanol and on the atomic displacement parameters so that they would tend to be similar for adjacent sites. Hydrogen atoms attached to C of the organometallic species were included at idealized positions and ride on the atoms to which they were bonded. H atoms attached to N were included at calculated positions and were refined positionally with restraints on distances and angles involving them. The H atoms of the full-occupied methanol solvate molecule were observed in a difference electron density map and were included at these positions. They were then refined positionally with restraints on distances and angles involving them. H atoms of the full-occupied water solvate were not located, nor were those of the partially-occupied methanol and water solvate molecules. The biggest peaks in the final difference electron density map were located within the disordered solvate region of the structure. ; _publ_section_exptl_prep ; The compound was recrystallized from acetone/methanol. The sample ID is R/07/Pd1. ; #========================================================================== ## -------------------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. 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 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius BV, COLLECT Software, 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. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994), Acta Cryst, A50, 411-437 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 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Pd1 Pd 0.78291(2) 0.093485(19) 0.751712(12) 0.0248 1.0000 Uani . . . . . . Cl1 Cl 0.93489(8) -0.06799(6) 0.83500(4) 0.0339 1.0000 Uani . . . . . . Cl2 Cl 0.81582(9) -0.02557(7) 0.64299(4) 0.0388 1.0000 Uani . . . . . . P1 P 0.76477(8) 0.20923(6) 0.85383(4) 0.0261 1.0000 Uani . . . . . . P2 P 0.62313(8) 0.23116(6) 0.67021(4) 0.0283 1.0000 Uani . . . . . . O1 O 1.0792(2) 0.1628(2) 0.89491(13) 0.0414 1.0000 Uani . . . . . . O2 O 0.4168(3) 0.3875(2) 0.76797(15) 0.0507 1.0000 Uani . . . . . . O51 O 0.4260(3) 0.7177(2) 0.63882(19) 0.0620 1.0000 Uani D . . . . . O61 O 0.1346(5) 0.7347(4) 0.7234(4) 0.1355 1.0000 Uani . . . . . . O71 O 0.2348(10) 0.6010(10) 0.8462(6) 0.1504 0.658(12) Uani D U P . . . O73 O 0.147(4) 0.459(4) 0.929(2) 0.1419 0.181(13) Uani . U P . . . O74 O 0.049(4) 0.413(3) 0.9811(18) 0.1172 0.161(11) Uani . U P . . . N1 N 0.8806(3) 0.1309(2) 0.99770(14) 0.0333 1.0000 Uani D . . . . . N2 N 0.5497(3) 0.4700(2) 0.64891(19) 0.0471 1.0000 Uani D . . . . . C10 C 0.9406(3) 0.1619(2) 0.91880(16) 0.0309 1.0000 Uani D . . . . . C11 C 0.6287(3) 0.1822(2) 0.94251(16) 0.0283 1.0000 Uani . . . . . . C12 C 0.7145(3) 0.1376(2) 1.01242(16) 0.0293 1.0000 Uani D . . . . . C13 C 0.6391(3) 0.1024(3) 1.08861(17) 0.0357 1.0000 Uani . . . . . . C14 C 0.4745(4) 0.1106(3) 1.09423(19) 0.0392 1.0000 Uani . . . . . . C15 C 0.3882(3) 0.1532(3) 1.02557(19) 0.0385 1.0000 Uani . . . . . . C16 C 0.4638(3) 0.1889(3) 0.94921(17) 0.0334 1.0000 Uani . . . . . . C21 C 0.7638(3) 0.3707(2) 0.83058(17) 0.0337 1.0000 Uani . . . . . . C22 C 0.8825(5) 0.4053(3) 0.7726(2) 0.0498 1.0000 Uani . . . . . . C23 C 0.8959(6) 0.5270(4) 0.7589(3) 0.0674 1.0000 Uani . . . . . . C24 C 0.7911(6) 0.6118(4) 0.8024(3) 0.0686 1.0000 Uani . . . . . . C25 C 0.6717(5) 0.5776(3) 0.8577(3) 0.0625 1.0000 Uani . . . . . . C26 C 0.6583(4) 0.4556(3) 0.8730(2) 0.0445 1.0000 Uani . . . . . . C30 C 0.5106(4) 0.3789(3) 0.70614(19) 0.0391 1.0000 Uani D . . . . . C31 C 0.7153(4) 0.3113(3) 0.58125(19) 0.0389 1.0000 Uani . . . . . . C32 C 0.6611(4) 0.4362(3) 0.5824(2) 0.0447 1.0000 Uani D . . . . . C33 C 0.7201(6) 0.5194(4) 0.5202(3) 0.0657 1.0000 Uani . . . . . . C34 C 0.8313(6) 0.4731(5) 0.4598(3) 0.0728 1.0000 Uani . . . . . . C35 C 0.8860(5) 0.3508(4) 0.4577(3) 0.0662 1.0000 Uani . . . . . . C36 C 0.8295(4) 0.2681(4) 0.5184(2) 0.0477 1.0000 Uani . . . . . . C41 C 0.4589(3) 0.1743(2) 0.64223(16) 0.0298 1.0000 Uani . . . . . . C42 C 0.3415(4) 0.1479(3) 0.7049(2) 0.0464 1.0000 Uani . . . . . . C43 C 0.2150(4) 0.1043(4) 0.6857(2) 0.0550 1.0000 Uani . . . . . . C44 C 0.2055(4) 0.0862(3) 0.6046(3) 0.0553 1.0000 Uani . . . . . . C45 C 0.3210(4) 0.1116(3) 0.5424(2) 0.0457 1.0000 Uani . . . . . . C46 C 0.4497(3) 0.1555(3) 0.56110(17) 0.0358 1.0000 Uani . . . . . . C52 C 0.5043(7) 0.7931(4) 0.6732(3) 0.0780 1.0000 Uani D . . . . . C72 C 0.1397(18) 0.572(2) 0.9261(8) 0.1646 0.658(12) Uani D U P . . . H1 H 0.939(2) 0.111(3) 1.0380(9) 0.0404 1.0000 Uiso D . . . . . H2 H 0.512(4) 0.5448(10) 0.6546(17) 0.0575 1.0000 Uiso D . . . . . H131 H 0.7008 0.0720 1.13829 0.0430 1.0000 Uiso R . . . . . H141 H 0.4173 0.0853 1.14880 0.0475 1.0000 Uiso R . . . . . H151 H 0.2700 0.1582 1.03135 0.0473 1.0000 Uiso R . . . . . H161 H 0.4014 0.2188 0.89971 0.0411 1.0000 Uiso R . . . . . H221 H 0.9577 0.3434 0.7410 0.0609 1.0000 Uiso R . . . . . H231 H 0.9813 0.5529 0.7176 0.0828 1.0000 Uiso R . . . . . H241 H 0.8024 0.6989 0.7934 0.0858 1.0000 Uiso R . . . . . H251 H 0.5936 0.6404 0.8873 0.0757 1.0000 Uiso R . . . . . H261 H 0.5727 0.4303 0.9145 0.0540 1.0000 Uiso R . . . . . H331 H 0.6818 0.6094 0.5203 0.0802 1.0000 Uiso R . . . . . H341 H 0.8744 0.5313 0.4154 0.0866 1.0000 Uiso R . . . . . H351 H 0.9671 0.3210 0.4121 0.0785 1.0000 Uiso R . . . . . H361 H 0.8700 0.1784 0.5174 0.0582 1.0000 Uiso R . . . . . H421 H 0.3493 0.1605 0.7634 0.0572 1.0000 Uiso R . . . . . H431 H 0.1302 0.0858 0.7302 0.0673 1.0000 Uiso R . . . . . H441 H 0.1136 0.0543 0.5911 0.0688 1.0000 Uiso R . . . . . H451 H 0.3126 0.0984 0.4841 0.0575 1.0000 Uiso R . . . . . H461 H 0.5346 0.1734 0.51645 0.0436 1.0000 Uiso R . . . . . H511 H 0.337(3) 0.725(4) 0.663(2) 0.08 1.0000 Uiso D . . . . . H521 H 0.472(4) 0.8813(12) 0.650(2) 0.10 1.0000 Uiso D . . . . . H522 H 0.6230(15) 0.766(3) 0.661(2) 0.10 1.0000 Uiso D . . . . . H523 H 0.479(4) 0.784(3) 0.7350(8) 0.10 1.0000 Uiso D . . . . . 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 Pd1 0.02375(10) 0.02911(10) 0.02301(9) -0.00228(6) -0.00589(6) -0.00726(7) Cl1 0.0357(3) 0.0355(3) 0.0290(3) -0.0017(3) -0.0102(3) -0.0019(3) Cl2 0.0405(4) 0.0443(4) 0.0359(3) -0.0145(3) -0.0118(3) -0.0070(3) P1 0.0279(3) 0.0280(3) 0.0235(3) -0.0024(2) -0.0071(2) -0.0063(2) P2 0.0295(3) 0.0310(3) 0.0261(3) -0.0001(3) -0.0101(3) -0.0081(3) O1 0.0295(10) 0.0586(13) 0.0387(11) -0.0058(9) -0.0085(8) -0.0118(9) O2 0.0525(13) 0.0497(13) 0.0487(13) -0.0131(11) -0.0106(11) -0.0004(10) O51 0.0600(16) 0.0499(14) 0.0755(18) -0.0094(13) -0.0014(14) -0.0122(12) O61 0.100(3) 0.095(3) 0.218(6) -0.084(3) 0.068(3) -0.036(2) O71 0.121(6) 0.207(9) 0.151(7) -0.107(7) 0.026(5) -0.057(6) O73 0.123(15) 0.210(18) 0.098(13) -0.066(15) -0.039(11) -0.001(15) O74 0.110(17) 0.17(2) 0.077(15) -0.043(15) -0.056(12) -0.003(15) N1 0.0314(11) 0.0427(13) 0.0269(10) -0.0040(9) -0.0112(9) -0.0056(10) N2 0.0535(16) 0.0289(12) 0.0614(17) 0.0005(12) -0.0237(14) -0.0078(11) C10 0.0293(12) 0.0351(13) 0.0308(13) -0.0053(10) -0.0091(10) -0.0079(10) C11 0.0293(12) 0.0266(12) 0.0297(12) -0.0055(10) -0.0046(10) -0.0049(9) C12 0.0301(12) 0.0284(12) 0.0306(12) -0.0053(10) -0.0051(10) -0.0063(10) C13 0.0400(15) 0.0355(14) 0.0321(13) -0.0026(11) -0.0062(11) -0.0082(11) C14 0.0446(16) 0.0374(15) 0.0367(14) -0.0077(12) 0.0058(12) -0.0139(12) C15 0.0320(13) 0.0427(15) 0.0436(15) -0.0132(13) 0.0039(11) -0.0130(12) C16 0.0313(13) 0.0361(14) 0.0353(13) -0.0089(11) -0.0071(11) -0.0076(11) C21 0.0425(15) 0.0318(13) 0.0292(12) -0.0017(10) -0.0121(11) -0.0092(11) C22 0.066(2) 0.0425(17) 0.0441(17) -0.0010(14) -0.0007(15) -0.0224(16) C23 0.098(3) 0.051(2) 0.058(2) 0.0085(18) -0.004(2) -0.038(2) C24 0.101(3) 0.0376(18) 0.076(3) 0.0031(18) -0.025(2) -0.030(2) C25 0.078(3) 0.0343(17) 0.077(3) -0.0098(17) -0.015(2) -0.0097(17) C26 0.0534(18) 0.0356(15) 0.0460(17) -0.0048(13) -0.0107(14) -0.0097(13) C30 0.0407(15) 0.0373(15) 0.0415(16) -0.0066(12) -0.0166(13) -0.0048(12) C31 0.0397(15) 0.0443(16) 0.0378(14) 0.0062(12) -0.0171(12) -0.0193(12) C32 0.0467(17) 0.0456(17) 0.0457(17) 0.0055(13) -0.0188(14) -0.0177(14) C33 0.075(3) 0.049(2) 0.076(3) 0.0178(19) -0.026(2) -0.0272(19) C34 0.073(3) 0.082(3) 0.062(2) 0.024(2) -0.003(2) -0.036(2) C35 0.060(2) 0.080(3) 0.055(2) 0.015(2) 0.0002(18) -0.029(2) C36 0.0442(17) 0.065(2) 0.0366(15) 0.0075(14) -0.0071(13) -0.0240(15) C41 0.0289(12) 0.0304(12) 0.0313(12) -0.0010(10) -0.0086(10) -0.0075(10) C42 0.0413(16) 0.062(2) 0.0397(16) -0.0068(14) -0.0005(13) -0.0201(15) C43 0.0336(16) 0.076(2) 0.059(2) -0.0080(18) 0.0013(14) -0.0214(16) C44 0.0339(16) 0.058(2) 0.080(3) -0.0040(18) -0.0179(16) -0.0186(15) C45 0.0457(17) 0.0519(18) 0.0463(17) -0.0066(14) -0.0214(14) -0.0150(14) C46 0.0333(13) 0.0432(15) 0.0323(13) -0.0012(11) -0.0082(11) -0.0105(11) C52 0.093(3) 0.065(3) 0.082(3) -0.002(2) -0.029(3) -0.022(2) C72 0.156(10) 0.235(14) 0.117(8) -0.069(10) -0.069(7) -0.010(10) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.3725(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pd1 . Cl1 . 2.3516(7) yes Pd1 . Cl2 . 2.3404(7) yes Pd1 . P1 . 2.2420(7) yes Pd1 . P2 . 2.2282(7) yes P1 . C10 . 1.888(3) yes P1 . C11 . 1.783(3) yes P1 . C21 . 1.811(3) yes P2 . C30 . 1.874(3) yes P2 . C31 . 1.794(3) yes P2 . C41 . 1.810(3) yes O1 . C10 . 1.211(3) yes O2 . C30 . 1.216(4) yes O51 . C52 . 1.412(5) yes O51 . H511 . 0.812(10) no O71 . C72 . 1.488(14) yes N1 . C10 . 1.355(3) yes N1 . C12 . 1.408(3) yes N1 . H1 . 0.849(10) no N2 . C30 . 1.358(4) yes N2 . C32 . 1.398(5) yes N2 . H2 . 0.851(10) no C11 . C12 . 1.404(4) yes C11 . C16 . 1.397(4) yes C12 . C13 . 1.379(4) yes C13 . C14 . 1.392(4) yes C13 . H131 . 1.000 no C14 . C15 . 1.387(5) yes C14 . H141 . 1.000 no C15 . C16 . 1.383(4) yes C15 . H151 . 1.000 no C16 . H161 . 1.000 no C21 . C22 . 1.389(4) yes C21 . C26 . 1.373(4) yes C22 . C23 . 1.392(5) yes C22 . H221 . 1.000 no C23 . C24 . 1.378(7) yes C23 . H231 . 1.000 no C24 . C25 . 1.368(6) yes C24 . H241 . 1.000 no C25 . C26 . 1.396(5) yes C25 . H251 . 1.000 no C26 . H261 . 1.000 no C31 . C32 . 1.390(5) yes C31 . C36 . 1.396(5) yes C32 . C33 . 1.408(5) yes C33 . C34 . 1.366(7) yes C33 . H331 . 1.000 no C34 . C35 . 1.364(7) yes C34 . H341 . 1.000 no C35 . C36 . 1.382(5) yes C35 . H351 . 1.000 no C36 . H361 . 1.000 no C41 . C42 . 1.397(4) yes C41 . C46 . 1.388(4) yes C42 . C43 . 1.379(5) yes C42 . H421 . 1.000 no C43 . C44 . 1.385(6) yes C43 . H431 . 1.000 no C44 . C45 . 1.378(5) yes C44 . H441 . 1.000 no C45 . C46 . 1.394(4) yes C45 . H451 . 1.000 no C46 . H461 . 1.000 no C52 . H521 . 1.003(10) no C52 . H522 . 1.004(10) no C52 . H523 . 1.003(10) 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 . Pd1 . Cl2 . 91.22(3) yes Cl1 . Pd1 . P1 . 88.17(2) yes Cl2 . Pd1 . P1 . 176.91(3) yes Cl1 . Pd1 . P2 . 173.46(3) yes Cl2 . Pd1 . P2 . 84.56(3) yes P1 . Pd1 . P2 . 96.30(3) yes Pd1 . P1 . C10 . 113.06(9) yes Pd1 . P1 . C11 . 116.88(8) yes C10 . P1 . C11 . 91.38(12) yes Pd1 . P1 . C21 . 120.93(9) yes C10 . P1 . C21 . 98.87(12) yes C11 . P1 . C21 . 110.21(13) yes Pd1 . P2 . C30 . 121.30(9) yes Pd1 . P2 . C31 . 117.67(10) yes C30 . P2 . C31 . 90.96(15) yes Pd1 . P2 . C41 . 113.08(9) yes C30 . P2 . C41 . 99.95(13) yes C31 . P2 . C41 . 110.94(12) yes C52 . O51 . H511 . 106.3(18) no C10 . N1 . C12 . 117.8(2) yes C10 . N1 . H1 . 122.3(12) no C12 . N1 . H1 . 119.9(12) no C30 . N2 . C32 . 117.3(3) yes C30 . N2 . H2 . 121.6(13) no C32 . N2 . H2 . 121.0(13) no P1 . C10 . N1 . 106.60(18) yes P1 . C10 . O1 . 126.5(2) yes N1 . C10 . O1 . 126.8(2) yes P1 . C11 . C12 . 109.46(19) yes P1 . C11 . C16 . 130.6(2) yes C12 . C11 . C16 . 119.7(2) yes N1 . C12 . C11 . 114.7(2) yes N1 . C12 . C13 . 123.7(2) yes C11 . C12 . C13 . 121.5(2) yes C12 . C13 . C14 . 118.0(3) yes C12 . C13 . H131 . 121.0 no C14 . C13 . H131 . 121.0 no C13 . C14 . C15 . 121.3(3) yes C13 . C14 . H141 . 119.4 no C15 . C14 . H141 . 119.4 no C14 . C15 . C16 . 120.8(3) yes C14 . C15 . H151 . 119.6 no C16 . C15 . H151 . 119.6 no C11 . C16 . C15 . 118.8(3) yes C11 . C16 . H161 . 120.6 no C15 . C16 . H161 . 120.6 no P1 . C21 . C22 . 117.5(2) yes P1 . C21 . C26 . 121.7(2) yes C22 . C21 . C26 . 120.7(3) yes C21 . C22 . C23 . 119.3(4) yes C21 . C22 . H221 . 120.3 no C23 . C22 . H221 . 120.3 no C22 . C23 . C24 . 119.9(4) yes C22 . C23 . H231 . 120.1 no C24 . C23 . H231 . 120.1 no C23 . C24 . C25 . 120.4(3) yes C23 . C24 . H241 . 119.8 no C25 . C24 . H241 . 119.8 no C24 . C25 . C26 . 120.3(4) yes C24 . C25 . H251 . 119.8 no C26 . C25 . H251 . 119.8 no C25 . C26 . C21 . 119.3(3) yes C25 . C26 . H261 . 120.3 no C21 . C26 . H261 . 120.3 no P2 . C30 . N2 . 107.1(2) yes P2 . C30 . O2 . 124.7(2) yes N2 . C30 . O2 . 128.2(3) yes P2 . C31 . C32 . 109.3(2) yes P2 . C31 . C36 . 130.8(3) yes C32 . C31 . C36 . 119.8(3) yes N2 . C32 . C31 . 115.4(3) yes N2 . C32 . C33 . 124.3(3) yes C31 . C32 . C33 . 120.3(4) yes C32 . C33 . C34 . 117.9(4) yes C32 . C33 . H331 . 121.0 no C34 . C33 . H331 . 121.0 no C33 . C34 . C35 . 122.6(4) yes C33 . C34 . H341 . 118.7 no C35 . C34 . H341 . 118.7 no C34 . C35 . C36 . 120.2(4) yes C34 . C35 . H351 . 119.9 no C36 . C35 . H351 . 119.9 no C31 . C36 . C35 . 119.2(4) yes C31 . C36 . H361 . 120.4 no C35 . C36 . H361 . 120.4 no P2 . C41 . C42 . 118.2(2) yes P2 . C41 . C46 . 121.4(2) yes C42 . C41 . C46 . 120.4(3) yes C41 . C42 . C43 . 119.7(3) yes C41 . C42 . H421 . 120.2 no C43 . C42 . H421 . 120.1 no C42 . C43 . C44 . 119.9(3) yes C42 . C43 . H431 . 120.1 no C44 . C43 . H431 . 120.1 no C43 . C44 . C45 . 120.9(3) yes C43 . C44 . H441 . 119.6 no C45 . C44 . H441 . 119.6 no C44 . C45 . C46 . 119.8(3) yes C44 . C45 . H451 . 120.1 no C46 . C45 . H451 . 120.1 no C45 . C46 . C41 . 119.4(3) yes C45 . C46 . H461 . 120.3 no C41 . C46 . H461 . 120.3 no O51 . C52 . H521 . 112.1(16) no O51 . C52 . H522 . 109.1(16) no H521 . C52 . H522 . 108.5(17) no O51 . C52 . H523 . 109.1(16) no H521 . C52 . H523 . 109.3(17) no H522 . C52 . H523 . 108.7(17) 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 O61 3.164(5) . 1_645 no Cl1 N1 3.237(2) . 2_757 no Cl1 C15 3.587(3) . 2_657 no O1 O74 3.30(4) . 1_655 no O1 C13 3.411(3) . 2_757 no O1 N1 3.488(3) . 2_757 no O1 C15 3.582(4) . 1_655 no O1 C43 3.585(4) . 1_655 no O2 O71 2.95(1) . . no O2 O73 3.36(3) . . no O51 O61 2.694(5) . . no O51 N2 2.757(3) . . no O51 C46 3.510(4) . 2_666 no O51 C36 3.544(5) . 2_666 no O51 C35 3.555(6) . 2_666 no O51 C32 3.556(4) . . no O51 C33 3.573(5) . . no O61 O71 2.45(1) . . no O61 C35 3.285(8) . 2_666 no O61 C52 3.375(7) . . no O61 C23 3.401(7) . 1_455 no O61 C72 3.54(2) . . no O61 C24 3.568(7) . 1_455 no O71 O74 3.51(3) . 2_567 no O73 O74 1.26(5) . . no O73 C72 1.26(5) . . no O73 O74 2.46(5) . 2_567 no O73 C72 3.25(4) . 2_567 no O73 O73 3.29(6) . 2_567 no O74 C72 2.08(3) . 2_567 no O74 O74 2.11(7) . 2_567 no O74 C10 3.51(4) . 1_455 no N1 N1 3.204(4) . 2_757 no N1 C10 3.480(3) . 2_757 no C14 C16 3.481(5) . 2_657 no C24 C52 3.533(7) . . no C34 C34 3.54(1) . 2_766 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 Pd1 P1 C10 O1 . . . . 62.4(3) no Pd1 P1 C10 N1 . . . . -119.7(2) no Pd1 P1 C11 C12 . . . . 114.9(2) no Pd1 P1 C11 C16 . . . . -59.1(3) no Pd1 P1 C21 C22 . . . . -49.5(3) no Pd1 P1 C21 C26 . . . . 135.6(2) no Pd1 P2 C30 O2 . . . . -57.6(4) no Pd1 P2 C30 N2 . . . . 124.8(2) no Pd1 P2 C31 C32 . . . . -126.7(2) no Pd1 P2 C31 C36 . . . . 50.5(4) no Pd1 P2 C41 C42 . . . . 66.9(2) no Pd1 P2 C41 C46 . . . . -112.2(2) no Cl1 Pd1 P1 C10 . . . . 28.29(9) no Cl1 Pd1 P1 C11 . . . . -75.92(9) no Cl1 Pd1 P1 C21 . . . . 145.0(1) no Cl2 Pd1 P2 C30 . . . . 176.5(1) no Cl2 Pd1 P2 C31 . . . . -73.6(1) no Cl2 Pd1 P2 C41 . . . . 57.88(9) no P1 Pd1 P2 C30 . . . . -6.5(1) no P1 Pd1 P2 C31 . . . . 103.4(1) no P1 Pd1 P2 C41 . . . . -125.10(9) no P1 C10 N1 C12 . . . . 1.3(3) no P1 C11 C12 N1 . . . . 3.0(3) no P1 C11 C12 C13 . . . . -176.2(2) no P1 C11 C16 C15 . . . . 174.7(2) no P1 C21 C22 C23 . . . . -173.7(3) no P1 C21 C26 C25 . . . . 174.4(3) no P2 Pd1 P1 C10 . . . . -156.49(9) no P2 Pd1 P1 C11 . . . . 99.31(9) no P2 Pd1 P1 C21 . . . . -39.7(1) no P2 C30 N2 C32 . . . . -2.0(4) no P2 C31 C32 N2 . . . . -1.0(4) no P2 C31 C32 C33 . . . . 177.9(3) no P2 C31 C36 C35 . . . . -177.5(3) no P2 C41 C42 C43 . . . . -179.9(3) no P2 C41 C46 C45 . . . . -180.0(2) no O1 C10 P1 C11 . . . . -177.5(2) no O1 C10 P1 C21 . . . . -66.8(3) no O1 C10 N1 C12 . . . . 179.2(3) no O2 C30 P2 C31 . . . . 178.8(3) no O2 C30 P2 C41 . . . . 67.3(3) no O2 C30 N2 C32 . . . . -179.6(4) no O71 C72 O73 O74 . . . . -165(3) no N1 C10 P1 C11 . . . . 0.4(2) no N1 C10 P1 C21 . . . . 111.1(2) no N1 C12 C11 C16 . . . . 177.8(2) no N1 C12 C13 C14 . . . . -178.3(3) no N2 C30 P2 C31 . . . . 1.2(3) no N2 C30 P2 C41 . . . . -110.3(2) no N2 C32 C31 C36 . . . . -178.6(3) no N2 C32 C33 C34 . . . . 178.7(4) no C10 P1 C11 C12 . . . . -1.9(2) no C10 P1 C11 C16 . . . . -176.0(3) no C10 P1 C21 C22 . . . . 74.3(3) no C10 P1 C21 C26 . . . . -100.6(3) no C10 N1 C12 C11 . . . . -3.0(3) no C10 N1 C12 C13 . . . . 176.3(3) no C11 P1 C21 C22 . . . . 169.1(3) no C11 P1 C21 C26 . . . . -5.8(3) no C11 C12 C13 C14 . . . . 0.9(4) no C11 C16 C15 C14 . . . . -0.5(5) no C12 C11 P1 C21 . . . . -101.9(2) no C12 C11 C16 C15 . . . . 1.2(4) no C12 C13 C14 C15 . . . . -0.2(5) no C13 C12 C11 C16 . . . . -1.4(4) no C13 C14 C15 C16 . . . . -0.0(5) no C16 C11 P1 C21 . . . . 84.1(3) no C21 C22 C23 C24 . . . . -0.4(7) no C21 C26 C25 C24 . . . . -1.5(6) no C22 C21 C26 C25 . . . . -0.3(5) no C22 C23 C24 C25 . . . . -1.4(8) no C23 C22 C21 C26 . . . . 1.3(6) no C23 C24 C25 C26 . . . . 2.4(8) no C30 P2 C31 C32 . . . . -0.1(3) no C30 P2 C31 C36 . . . . 177.1(4) no C30 P2 C41 C42 . . . . -63.5(2) no C30 P2 C41 C46 . . . . 117.4(2) no C30 N2 C32 C31 . . . . 2.1(5) no C30 N2 C32 C33 . . . . -176.8(4) no C31 P2 C41 C42 . . . . -158.4(2) no C31 P2 C41 C46 . . . . 22.5(2) no C31 C32 C33 C34 . . . . -0.2(7) no C31 C36 C35 C34 . . . . 0.5(7) no C32 C31 P2 C41 . . . . 100.9(3) no C32 C31 C36 C35 . . . . -0.5(6) no C32 C33 C34 C35 . . . . 0.1(8) no C33 C32 C31 C36 . . . . 0.4(6) no C33 C34 C35 C36 . . . . -0.3(8) no C36 C31 P2 C41 . . . . -81.9(4) no C41 C42 C43 C44 . . . . 0.4(5) no C41 C46 C45 C44 . . . . -0.7(4) no C42 C41 C46 C45 . . . . 0.9(4) no C42 C43 C44 C45 . . . . -0.2(5) no C43 C42 C41 C46 . . . . -0.8(4) no C43 C44 C45 C46 . . . . 0.3(5) no #------------------------------------------------------------------------------ loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O51 H511 O61 0.81(3) 1.88(3) 2.694(5) 177(4) . no N1 H1 Cl1 0.85(2) 2.39(2) 3.237(2) 171(2) 2_757 no N2 H2 O51 0.85(1) 1.92(1) 2.757(3) 166(3) . no # start Validation Reply Form _vrf_PLAT306_sal0701 ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O61 RESPONSE: ... Yes, these H atoms are missing. O61 is adjacent to a disordered region in the structure, and is, itself, probably disordered to some degree. The fact that the H atoms are not observed in a difference map is therefore not surprising. ; _vrf_PLAT430_sal0701 ; PROBLEM: Short Inter D...A Contact O61 .. O71 .. 2.45 Ang. RESPONSE: ... For O61....O71: O61 is adjacent to a disordered region in the structure, and is, itself, probably disordered to some degree. The coordinates indicate the average position. When O71 is present then O61 will adjust to this. In this situation they are probably H-bonded so this distance will tend to be short anyway (ca. 2.7 Ang). For O74....O74: these atom sites (occ < .5) need not be occupied simultaneously. ; _vrf_PLAT432_sal0701 ; PROBLEM: Short Inter X...Y Contact C72 .. O74 .. 2.08 Ang. RESPONSE: ... Disordered region of the structure. These atom sites need not be occupied simultaneously. ; # end Validation Reply Form #===END # Attachment 'sal0702.cif' data_sal0702 _database_code_depnum_ccdc_archive 'CCDC 744589' _audit_creation_date 07-09-12 _audit_creation_method CRYSTALS_ver_12.18 _audit_update_record ; 2007-09-17 - Report on C71 H83 C33 H39 Cl N2 O4 P2 Pt by Anthony C. Willis for Geoff Salem, Roy Doyle and Justine Bennett 2007-09-17 - passes checkcif tests with minor warnings ; _oxford_structure_analysis_title '9111430 sal0702' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 15.4641(2) _cell_length_b 12.9680(2) _cell_length_c 18.4124(3) _cell_angle_alpha 90 _cell_angle_beta 113.4788(9) _cell_angle_gamma 90 _cell_volume 3386.69(9) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/a 1 ' _symmetry_space_group_name_Hall ? 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 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Pt -1.7033 8.3905 27.0059 1.5129 17.7639 8.8117 15.7131 0.4246 5.7837 38.6103 11.6883 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C32 H36 Cl2 N2 O4 P2 Pt1 # Dc = 1.65 Fooo = 1620.00 Mu = 44.33 M = 840.59 # Found Formula = C33 H36 Cl1 N2 O4 P2 Pt1 # Dc = 1.60 FOOO = 1620.00 Mu = 43.55 M = 817.15 _chemical_formula_sum 'C33 H36 Cl N2 O4 P2 Pt' _chemical_formula_moiety 'C33 H39 Cl N2 O4 P2 Pt' _chemical_compound_source local _chemical_formula_weight 820.17 # 817.15 _cell_measurement_reflns_used 52649 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 200 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_min 0.05 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_max 0.36 _exptl_crystal_density_diffrn 1.609 # 1.603 _exptl_crystal_density_meas ' not measured ' # Non-dispersive F(000): _exptl_crystal_F_000 1626 # 1620 _exptl_absorpt_coefficient_mu 4.37 # 4.355 # Sheldrick geometric approximatio 0.57 0.80 # Absorption correction loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 1 0 0.070 0 -1 0 0.060 0 0 1 0.020 0 0 -1 0.030 -2 0 1 0.204 2 0 -1 0.153 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.347 _exptl_absorpt_correction_T_max 0.803 _exptl_absorpt_process_details ; via Gaussian method (Coppens, 1970) implemented in maXus (2000) ; #_diffrn_reflns_av_R_equivalents 0.030 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _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 133 sec/frame, crystal-detector distance 35mm, multiple scan sets so over 90 percent of data collected with 4-fold redundancy or more. ; # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius BV, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'CRYSTALS (Watkin et al 2003)' _computing_publication_material 'CRYSTALS (Watkin et al 2003)' _computing_molecular_graphics ; ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997) ; _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 200 _diffrn_reflns_number 69517 _reflns_number_total 7756 _diffrn_reflns_av_R_equivalents 0.041 # Number of reflections with Friedels Law is 7756 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 7765 _diffrn_reflns_theta_min 2.635 _diffrn_reflns_theta_max 27.481 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.481 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _reflns_limit_h_min -20 _reflns_limit_h_max 18 _reflns_limit_k_min 0 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 23 _oxford_diffrn_Wilson_B_factor 3.09 _oxford_diffrn_Wilson_scale 32.32 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.83 _refine_diff_density_max 0.93 _refine_ls_number_reflns 5069 _refine_ls_number_restraints 5 _refine_ls_number_parameters 395 #_refine_ls_R_factor_ref 0.0256 _refine_ls_wR_factor_ref 0.0296 _refine_ls_goodness_of_fit_ref 1.0991 #_reflns_number_all 7733 _refine_ls_R_factor_all 0.0435 _refine_ls_wR_factor_all 0.0342 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 5069 _refine_ls_R_factor_gt 0.0256 _refine_ls_wR_factor_gt 0.0296 _refine_ls_shift/su_max 0.010060 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.29 0.298 1.09 ; #============================================================================== # 4. TEXT _publ_section_abstract #Text of the abstract ; The crystal structure of [Pt(C~13~H~10~NOP)~2~(CH~3~)Cl].2C~3~H~8~O is reported. ; _publ_section_comment #Text of the paper ; The crystallographic asymmetric unit consists of one [Pt(C~13~H~10~NOP)~2~(CH~3~)Cl] molecule and two solvate isopropanol molecules. There is disorder of the methyl and chloro ligands. Distances and angles listed here involving these atoms are presumably for the weighted averaged positions. ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions #Captions to figures ; ? ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen for refinement keywords. ; Initial solution of the structure revealed that the two non-phosphine sites on the Pt atom were of very similar size. When incorporated as two Cl atoms their displacement parameters were much larger than those of adjacent atoms; when assigned to be two C atoms their displacement parameters were very small. This suggested that chloro and methyl groups were disordered on the two sites. Cl and C atoms of occupancy 0.5 were placed at each site and constraints were imposed on their positional and anisotropic displacement parameters so they would remain identical during further refinement. The relative occupancies of Cl versus C were refined. Hydrogen atoms attached to O were included at positions indicated in difference electron density maps and then were refined positionally, with restraints being imposed on distances and angles involving them. H atoms attached to C and N were included at idealized positions and ride on the atoms to which they were bonded. The methyl H atoms were not located. Attempts to get the disordered Cl and methyl groups to refine to separate positions were not successful. The biggest peaks in the final difference electron density map were located near the Cl and Pt atoms. ; _publ_section_exptl_prep ; The compound was recrystallized from dichloromethane/isopropanol. The sample ID is Ro7/Pt1. ; #========================================================================== ## -------------------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. 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 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius BV, COLLECT Software, 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. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994), Acta Cryst, A50, 411-437 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 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Pt1 Pt 0.233085(10) 0.172478(10) 0.258456(8) 0.0392 1.0000 Uani . . . . . . Cl1 Cl 0.24857(11) 0.00445(10) 0.29948(9) 0.0449 0.481(5) Uani . . P . . . Cl2 Cl 0.12625(12) 0.10655(13) 0.14074(9) 0.0526 0.519(5) Uani . . P . . . P1 P 0.34391(6) 0.22044(7) 0.37565(5) 0.0367 1.0000 Uani . . . . . . P2 P 0.19695(6) 0.32851(7) 0.20305(5) 0.0367 1.0000 Uani . . . . . . O1 O 0.4791(2) 0.0677(2) 0.40965(17) 0.0503 1.0000 Uani . . . . . . O2 O 0.2495(2) 0.4727(2) 0.32391(18) 0.0547 1.0000 Uani . . . . . . O50 O 0.1805(2) 0.8375(3) 0.1575(2) 0.0662 1.0000 Uani D . . . . . O60 O 0.3251(3) 0.7117(3) 0.2443(4) 0.1337 1.0000 Uani D . . . . . N1 N 0.4066(2) 0.0910(3) 0.4958(2) 0.0459 1.0000 Uani . . . . . . N2 N 0.2841(2) 0.5055(3) 0.2160(2) 0.0505 1.0000 Uani . . . . . . C1 C 0.24857(11) 0.00445(10) 0.29948(9) 0.0449 0.519(5) Uani . . P . . . C2 C 0.12625(12) 0.10655(13) 0.14074(9) 0.0526 0.481(5) Uani . . P . . . C10 C 0.4225(3) 0.1108(3) 0.4302(2) 0.0427 1.0000 Uani . . . . . . C11 C 0.3064(2) 0.2378(3) 0.4556(2) 0.0386 1.0000 Uani . . . . . . C12 C 0.3431(2) 0.1576(3) 0.5106(2) 0.0420 1.0000 Uani . . . . . . C13 C 0.3182(3) 0.1466(4) 0.5750(3) 0.0529 1.0000 Uani . . . . . . C14 C 0.2580(3) 0.2197(4) 0.5848(3) 0.0566 1.0000 Uani . . . . . . C15 C 0.2237(3) 0.3010(4) 0.5323(3) 0.0585 1.0000 Uani . . . . . . C16 C 0.2459(3) 0.3099(3) 0.4660(3) 0.0489 1.0000 Uani . . . . . . C20 C 0.4337(3) 0.3139(3) 0.3821(2) 0.0416 1.0000 Uani . . . . . . C21 C 0.4552(3) 0.3297(3) 0.3167(3) 0.0475 1.0000 Uani . . . . . . C22 C 0.5328(3) 0.3901(4) 0.3249(3) 0.0606 1.0000 Uani . . . . . . C23 C 0.5869(3) 0.4340(4) 0.3962(4) 0.0650 1.0000 Uani . . . . . . C24 C 0.5649(3) 0.4199(4) 0.4610(3) 0.0595 1.0000 Uani . . . . . . C25 C 0.4883(3) 0.3593(3) 0.4541(3) 0.0532 1.0000 Uani . . . . . . C30 C 0.2488(3) 0.4525(3) 0.2603(2) 0.0451 1.0000 Uani . . . . . . C31 C 0.2364(3) 0.3646(3) 0.1272(2) 0.0450 1.0000 Uani . . . . . . C32 C 0.2809(3) 0.4604(3) 0.1461(3) 0.0508 1.0000 Uani . . . . . . C33 C 0.3199(3) 0.5047(4) 0.0975(3) 0.0674 1.0000 Uani . . . . . . C34 C 0.3154(4) 0.4512(5) 0.0315(4) 0.0793 1.0000 Uani . . . . . . C35 C 0.2733(4) 0.3554(6) 0.0127(3) 0.0753 1.0000 Uani . . . . . . C36 C 0.2337(3) 0.3109(4) 0.0611(3) 0.0551 1.0000 Uani . . . . . . C41 C 0.0740(3) 0.3660(3) 0.1698(2) 0.0418 1.0000 Uani . . . . . . C42 C 0.0357(3) 0.3692(4) 0.2261(3) 0.0537 1.0000 Uani . . . . . . C43 C -0.0571(3) 0.4011(4) 0.2045(3) 0.0599 1.0000 Uani . . . . . . C44 C -0.1109(3) 0.4282(4) 0.1272(3) 0.0610 1.0000 Uani . . . . . . C45 C -0.0725(3) 0.4252(5) 0.0714(3) 0.0685 1.0000 Uani . . . . . . C46 C 0.0200(3) 0.3946(4) 0.0924(3) 0.0568 1.0000 Uani . . . . . . C51 C 0.0894(4) 0.7966(4) 0.1441(4) 0.0726 1.0000 Uani D . . . . . C52 C 0.0946(5) 0.6815(5) 0.1419(6) 0.0944 1.0000 Uani . . . . . . C53 C 0.0181(5) 0.8412(6) 0.0695(6) 0.1077 1.0000 Uani . . . . . . C61 C 0.4100(4) 0.7570(5) 0.2935(5) 0.0880 1.0000 Uani D . . . . . C62 C 0.4800(5) 0.6714(5) 0.3230(5) 0.1038 1.0000 Uani . . . . . . C63 C 0.4361(5) 0.8398(6) 0.2538(6) 0.1059 1.0000 Uani . . . . . . H1 H 0.4349 0.0382 0.5284 0.0559 1.0000 Uiso R . . . . . H2 H 0.3091 0.5686 0.2309 0.0598 1.0000 Uiso R . . . . . H50 H 0.184(2) 0.900(2) 0.174(3) 0.0790 1.0000 Uiso D . . . . . H60 H 0.286(2) 0.7589(19) 0.22004(10) 0.1560 1.0000 Uiso D . . . . . H131 H 0.3429 0.0880 0.6129 0.0641 1.0000 Uiso R . . . . . H141 H 0.2392 0.2134 0.6307 0.0711 1.0000 Uiso R . . . . . H151 H 0.1825 0.3541 0.5419 0.0741 1.0000 Uiso R . . . . . H161 H 0.2188 0.3669 0.4269 0.0599 1.0000 Uiso R . . . . . H211 H 0.4155 0.2982 0.2645 0.0593 1.0000 Uiso R . . . . . H221 H 0.5493 0.4017 0.2782 0.0770 1.0000 Uiso R . . . . . H231 H 0.6430 0.4766 0.4014 0.0795 1.0000 Uiso R . . . . . H241 H 0.6040 0.4532 0.5127 0.0686 1.0000 Uiso R . . . . . H251 H 0.4723 0.3483 0.5010 0.0632 1.0000 Uiso R . . . . . H331 H 0.3506 0.5741 0.1101 0.0816 1.0000 Uiso R . . . . . H341 H 0.3435 0.4825 -0.0038 0.0993 1.0000 Uiso R . . . . . H351 H 0.2712 0.3182 -0.0355 0.0955 1.0000 Uiso R . . . . . H361 H 0.2037 0.2413 0.0484 0.0681 1.0000 Uiso R . . . . . H421 H 0.0746 0.3488 0.2821 0.0666 1.0000 Uiso R . . . . . H431 H -0.0848 0.4044 0.2451 0.0774 1.0000 Uiso R . . . . . H441 H -0.1779 0.4500 0.1116 0.0739 1.0000 Uiso R . . . . . H451 H -0.1117 0.4454 0.0155 0.0791 1.0000 Uiso R . . . . . H461 H 0.0478 0.3931 0.0518 0.0680 1.0000 Uiso R . . . . . H511 H 0.0727 0.8171 0.1893 0.0907 1.0000 Uiso R . . . . . H521 H 0.0314 0.6516 0.1326 0.1123 1.0000 Uiso R . . . . . H522 H 0.1422 0.6559 0.1935 0.1123 1.0000 Uiso R . . . . . H523 H 0.1134 0.6602 0.0981 0.1123 1.0000 Uiso R . . . . . H531 H -0.0456 0.8127 0.0601 0.1196 1.0000 Uiso R . . . . . H532 H 0.0171 0.9179 0.0745 0.1196 1.0000 Uiso R . . . . . H533 H 0.0349 0.8227 0.0240 0.1196 1.0000 Uiso R . . . . . H611 H 0.4010 0.7871 0.3400 0.0970 1.0000 Uiso R . . . . . H621 H 0.5425 0.7001 0.3589 0.1065 1.0000 Uiso R . . . . . H622 H 0.4579 0.6207 0.3528 0.1065 1.0000 Uiso R . . . . . H623 H 0.4863 0.6362 0.2771 0.1065 1.0000 Uiso R . . . . . H631 H 0.4971 0.8707 0.2907 0.1279 1.0000 Uiso R . . . . . H632 H 0.3859 0.8939 0.2374 0.1279 1.0000 Uiso R . . . . . H633 H 0.4435 0.8121 0.2060 0.1279 1.0000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.04367(8) 0.03475(7) 0.04585(8) -0.00507(7) 0.02474(6) -0.00217(6) Cl1 0.0607(10) 0.0250(7) 0.0537(10) 0.0045(5) 0.0279(7) 0.0034(6) Cl2 0.0547(9) 0.0546(9) 0.0427(9) -0.0125(6) 0.0133(7) -0.0124(7) P1 0.0384(4) 0.0350(4) 0.0383(4) 0.0015(3) 0.0170(4) 0.0056(4) P2 0.0381(4) 0.0336(4) 0.0402(4) 0.0025(4) 0.0177(3) 0.0001(4) O1 0.0546(16) 0.0510(15) 0.0499(15) 0.0119(12) 0.0258(13) 0.0201(13) O2 0.0654(18) 0.0478(15) 0.0492(16) -0.0095(13) 0.0211(14) 0.0003(13) O50 0.0631(19) 0.0593(19) 0.076(2) -0.0192(17) 0.0269(17) -0.0087(15) O60 0.079(3) 0.049(2) 0.196(6) 0.015(3) -0.026(3) -0.016(2) N1 0.0456(17) 0.0465(17) 0.0477(18) 0.0097(14) 0.0209(14) 0.0089(14) N2 0.0531(18) 0.0373(17) 0.0591(19) 0.0001(15) 0.0204(15) -0.0102(14) C1 0.0607(10) 0.0250(7) 0.0537(10) 0.0045(5) 0.0279(7) 0.0034(6) C2 0.0547(9) 0.0546(9) 0.0427(9) -0.0125(6) 0.0133(7) -0.0124(7) C10 0.0428(18) 0.0404(18) 0.044(2) 0.0032(15) 0.0166(16) 0.0063(15) C11 0.0378(17) 0.0405(18) 0.0374(17) -0.0025(14) 0.0150(14) 0.0017(14) C12 0.0356(16) 0.049(2) 0.0408(18) 0.0015(15) 0.0148(14) -0.0001(15) C13 0.049(2) 0.068(3) 0.043(2) 0.0064(18) 0.0201(17) -0.0019(19) C14 0.052(2) 0.078(3) 0.047(2) -0.003(2) 0.0283(19) -0.002(2) C15 0.053(2) 0.071(3) 0.062(3) -0.010(2) 0.034(2) 0.005(2) C16 0.049(2) 0.051(2) 0.049(2) -0.0035(17) 0.0230(17) 0.0038(17) C20 0.0377(17) 0.0400(18) 0.0467(19) 0.0009(15) 0.0163(15) 0.0057(14) C21 0.0429(18) 0.049(2) 0.056(2) -0.0009(18) 0.0256(17) 0.0001(17) C22 0.049(2) 0.062(3) 0.082(3) 0.006(2) 0.038(2) 0.002(2) C23 0.043(2) 0.054(2) 0.103(4) -0.006(3) 0.033(2) -0.0028(19) C24 0.042(2) 0.054(2) 0.075(3) -0.014(2) 0.016(2) -0.0004(18) C25 0.047(2) 0.049(2) 0.062(3) -0.0069(19) 0.0201(19) -0.0014(17) C30 0.0379(19) 0.050(2) 0.0433(19) 0.0054(17) 0.0117(16) -0.0063(15) C31 0.0375(18) 0.0498(19) 0.051(2) 0.0123(17) 0.0206(16) 0.0075(15) C32 0.0426(19) 0.050(2) 0.060(2) 0.0147(18) 0.0208(18) 0.0010(16) C33 0.053(2) 0.077(3) 0.075(3) 0.025(3) 0.028(2) -0.006(2) C34 0.062(3) 0.108(5) 0.078(3) 0.038(3) 0.039(3) 0.004(3) C35 0.067(3) 0.112(5) 0.060(3) 0.014(3) 0.039(3) 0.018(3) C36 0.057(2) 0.066(3) 0.047(2) 0.0046(19) 0.0259(19) 0.007(2) C41 0.0400(18) 0.0360(16) 0.052(2) 0.0013(16) 0.0214(16) -0.0011(14) C42 0.050(2) 0.060(2) 0.057(2) 0.017(2) 0.0269(19) 0.0081(19) C43 0.052(2) 0.068(3) 0.074(3) 0.016(2) 0.040(2) 0.010(2) C44 0.044(2) 0.064(3) 0.077(3) 0.008(2) 0.026(2) 0.006(2) C45 0.045(2) 0.091(4) 0.062(3) 0.004(3) 0.013(2) 0.008(2) C46 0.047(2) 0.073(3) 0.050(2) -0.002(2) 0.0188(18) 0.004(2) C51 0.073(3) 0.072(3) 0.082(4) -0.026(3) 0.040(3) -0.016(3) C52 0.077(4) 0.072(4) 0.132(6) -0.015(4) 0.039(4) -0.012(3) C53 0.061(3) 0.094(5) 0.143(7) -0.002(4) 0.015(4) 0.001(3) C61 0.075(3) 0.060(3) 0.107(5) 0.007(3) 0.013(3) -0.018(3) C62 0.096(5) 0.074(4) 0.096(5) 0.020(3) -0.010(4) -0.020(3) C63 0.078(4) 0.084(4) 0.156(7) 0.028(4) 0.048(4) 0.001(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2170(2) 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 . 2.2873(13) yes Pt1 . Cl2 . 2.3032(15) yes Pt1 . P1 . 2.2435(9) yes Pt1 . P2 . 2.2345(9) yes Pt1 . C1 . 2.2873(13) yes Pt1 . C2 . 2.3032(15) yes P1 . C10 . 1.880(4) yes P1 . C11 . 1.798(4) yes P1 . C20 . 1.811(4) yes P2 . C30 . 1.915(4) yes P2 . C31 . 1.794(4) yes P2 . C41 . 1.816(4) yes O1 . C10 . 1.219(5) yes O2 . C30 . 1.196(5) yes O50 . C51 . 1.431(6) yes O50 . H50 . 0.853(19) no O60 . C61 . 1.394(7) yes O60 . H60 . 0.85(2) no N1 . C10 . 1.351(5) yes N1 . C12 . 1.413(5) yes N1 . H1 . 0.900 no N2 . C30 . 1.337(5) yes N2 . C32 . 1.398(6) yes N2 . H2 . 0.900 no C11 . C12 . 1.404(5) yes C11 . C16 . 1.389(5) yes C12 . C13 . 1.391(5) yes C13 . C14 . 1.390(7) yes C13 . H131 . 1.000 no C14 . C15 . 1.387(7) yes C14 . H141 . 1.000 no C15 . C16 . 1.399(6) yes C15 . H151 . 1.000 no C16 . H161 . 1.000 no C20 . C21 . 1.385(6) yes C20 . C25 . 1.387(6) yes C21 . C22 . 1.390(6) yes C21 . H211 . 1.000 no C22 . C23 . 1.368(8) yes C22 . H221 . 1.000 no C23 . C24 . 1.376(8) yes C23 . H231 . 1.000 no C24 . C25 . 1.384(6) yes C24 . H241 . 1.000 no C25 . H251 . 1.000 no C31 . C32 . 1.395(6) yes C31 . C36 . 1.389(6) yes C32 . C33 . 1.387(6) yes C33 . C34 . 1.377(9) yes C33 . H331 . 1.000 no C34 . C35 . 1.381(9) yes C34 . H341 . 1.000 no C35 . C36 . 1.391(7) yes C35 . H351 . 1.000 no C36 . H361 . 1.000 no C41 . C42 . 1.385(6) yes C41 . C46 . 1.385(6) yes C42 . C43 . 1.391(6) yes C42 . H421 . 1.000 no C43 . C44 . 1.377(7) yes C43 . H431 . 1.000 no C44 . C45 . 1.376(7) yes C44 . H441 . 1.000 no C45 . C46 . 1.384(6) yes C45 . H451 . 1.000 no C46 . H461 . 1.000 no C51 . C52 . 1.496(9) yes C51 . C53 . 1.493(10) yes C51 . H511 . 1.000 no C52 . H521 . 1.000 no C52 . H522 . 1.000 no C52 . H523 . 1.000 no C53 . H531 . 1.000 no C53 . H532 . 1.000 no C53 . H533 . 1.000 no C61 . C62 . 1.493(10) yes C61 . C63 . 1.444(9) yes C61 . H611 . 1.000 no C62 . H621 . 1.000 no C62 . H622 . 1.000 no C62 . H623 . 1.000 no C63 . H631 . 1.000 no C63 . H632 . 1.000 no C63 . H633 . 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 . P1 . 90.41(5) yes Cl2 . Pt1 . P1 . 174.08(5) yes Cl1 . Pt1 . P2 . 170.99(5) yes Cl2 . Pt1 . P2 . 87.21(5) yes P1 . Pt1 . P2 . 98.30(3) yes Cl2 . Pt1 . C1 . 84.18(6) yes P1 . Pt1 . C1 . 90.41(5) yes P2 . Pt1 . C1 . 170.99(5) yes Cl1 . Pt1 . C2 . 84.18(6) yes P1 . Pt1 . C2 . 174.08(5) yes P2 . Pt1 . C2 . 87.21(5) yes Pt1 . P1 . C10 . 112.79(12) yes Pt1 . P1 . C11 . 116.75(12) yes C10 . P1 . C11 . 90.46(17) yes Pt1 . P1 . C20 . 121.35(13) yes C10 . P1 . C20 . 98.94(17) yes C11 . P1 . C20 . 110.61(18) yes Pt1 . P2 . C30 . 122.37(12) yes Pt1 . P2 . C31 . 119.40(13) yes C30 . P2 . C31 . 90.66(19) yes Pt1 . P2 . C41 . 115.75(13) yes C30 . P2 . C41 . 96.50(17) yes C31 . P2 . C41 . 107.60(18) yes C51 . O50 . H50 . 109.7(18) no C61 . O60 . H60 . 109.1(19) no C10 . N1 . C12 . 116.4(3) yes C10 . N1 . H1 . 121.8 no C12 . N1 . H1 . 121.8 no C30 . N2 . C32 . 118.3(3) yes C30 . N2 . H2 . 120.9 no C32 . N2 . H2 . 120.9 no P1 . C10 . N1 . 108.2(3) yes P1 . C10 . O1 . 124.9(3) yes N1 . C10 . O1 . 126.8(3) yes P1 . C11 . C12 . 109.2(3) yes P1 . C11 . C16 . 130.6(3) yes C12 . C11 . C16 . 120.0(3) yes N1 . C12 . C11 . 115.2(3) yes N1 . C12 . C13 . 123.4(4) yes C11 . C12 . C13 . 121.4(4) yes C12 . C13 . C14 . 117.9(4) yes C12 . C13 . H131 . 121.0 no C14 . C13 . H131 . 121.0 no C13 . C14 . C15 . 121.2(4) yes C13 . C14 . H141 . 119.4 no C15 . C14 . H141 . 119.4 no C14 . C15 . C16 . 120.8(4) yes C14 . C15 . H151 . 119.6 no C16 . C15 . H151 . 119.6 no C15 . C16 . C11 . 118.5(4) yes C15 . C16 . H161 . 120.7 no C11 . C16 . H161 . 120.7 no P1 . C20 . C21 . 119.0(3) yes P1 . C20 . C25 . 120.4(3) yes C21 . C20 . C25 . 120.1(4) yes C20 . C21 . C22 . 119.0(4) yes C20 . C21 . H211 . 120.5 no C22 . C21 . H211 . 120.5 no C21 . C22 . C23 . 120.6(5) yes C21 . C22 . H221 . 119.7 no C23 . C22 . H221 . 119.7 no C22 . C23 . C24 . 120.6(4) yes C22 . C23 . H231 . 119.7 no C24 . C23 . H231 . 119.7 no C23 . C24 . C25 . 119.6(5) yes C23 . C24 . H241 . 120.2 no C25 . C24 . H241 . 120.2 no C20 . C25 . C24 . 120.1(4) yes C20 . C25 . H251 . 120.0 no C24 . C25 . H251 . 119.9 no P2 . C30 . N2 . 106.2(3) yes P2 . C30 . O2 . 124.1(3) yes N2 . C30 . O2 . 129.7(4) yes P2 . C31 . C32 . 109.0(3) yes P2 . C31 . C36 . 130.6(3) yes C32 . C31 . C36 . 120.2(4) yes N2 . C32 . C31 . 115.7(3) yes N2 . C32 . C33 . 123.8(4) yes C31 . C32 . C33 . 120.5(5) yes C32 . C33 . C34 . 118.6(5) yes C32 . C33 . H331 . 120.7 no C34 . C33 . H331 . 120.7 no C33 . C34 . C35 . 121.8(4) yes C33 . C34 . H341 . 119.1 no C35 . C34 . H341 . 119.1 no C34 . C35 . C36 . 119.8(5) yes C34 . C35 . H351 . 120.1 no C36 . C35 . H351 . 120.1 no C35 . C36 . C31 . 119.1(5) yes C35 . C36 . H361 . 120.4 no C31 . C36 . H361 . 120.5 no P2 . C41 . C42 . 117.2(3) yes P2 . C41 . C46 . 122.7(3) yes C42 . C41 . C46 . 120.0(4) yes C41 . C42 . C43 . 119.7(4) yes C41 . C42 . H421 . 120.2 no C43 . C42 . H421 . 120.2 no C42 . C43 . C44 . 120.1(4) yes C42 . C43 . H431 . 120.0 no C44 . C43 . H431 . 120.0 no C43 . C44 . C45 . 120.1(4) yes C43 . C44 . H441 . 119.9 no C45 . C44 . H441 . 119.9 no C44 . C45 . C46 . 120.4(5) yes C44 . C45 . H451 . 119.8 no C46 . C45 . H451 . 119.8 no C41 . C46 . C45 . 119.8(4) yes C41 . C46 . H461 . 120.1 no C45 . C46 . H461 . 120.1 no O50 . C51 . C52 . 108.3(5) yes O50 . C51 . C53 . 109.3(5) yes C52 . C51 . C53 . 112.9(6) yes O50 . C51 . H511 . 108.7 no C52 . C51 . H511 . 108.8 no C53 . C51 . H511 . 108.7 no C51 . C52 . H521 . 109.4 no C51 . C52 . H522 . 109.5 no H521 . C52 . H522 . 109.5 no C51 . C52 . H523 . 109.5 no H521 . C52 . H523 . 109.5 no H522 . C52 . H523 . 109.5 no C51 . C53 . H531 . 109.4 no C51 . C53 . H532 . 109.5 no H531 . C53 . H532 . 109.5 no C51 . C53 . H533 . 109.5 no H531 . C53 . H533 . 109.5 no H532 . C53 . H533 . 109.5 no O60 . C61 . C62 . 106.3(5) yes O60 . C61 . C63 . 111.5(7) yes C62 . C61 . C63 . 115.4(7) yes O60 . C61 . H611 . 107.8 no C62 . C61 . H611 . 107.8 no C63 . C61 . H611 . 107.8 no C61 . C62 . H621 . 109.5 no C61 . C62 . H622 . 109.5 no H621 . C62 . H622 . 109.5 no C61 . C62 . H623 . 109.5 no H621 . C62 . H623 . 109.5 no H622 . C62 . H623 . 109.5 no C61 . C63 . H631 . 109.5 no C61 . C63 . H632 . 109.5 no H631 . C63 . H632 . 109.5 no C61 . C63 . H633 . 109.4 no H631 . C63 . H633 . 109.5 no H632 . C63 . H633 . 109.5 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 O50 3.231(4) . 1_545 no Cl2 O50 3.573(4) . 1_545 no O1 N1 2.818(4) . 2_656 no O1 C10 3.577(4) . 2_656 no O1 O1 3.586(6) . 2_656 no O2 C13 3.346(7) . 3_556 no O50 O60 2.714(5) . . no O50 C1 3.231(4) . 1_565 no O50 C35 3.488(8) . 3 no O50 C2 3.573(4) . 1_565 no O50 C61 3.588(6) . . no O60 N2 2.750(5) . . no O60 C52 3.326(8) . . no O60 C51 3.542(7) . . no N1 C10 3.580(5) . 2_656 no N2 C52 3.532(7) . . no N2 C62 3.596(7) . . no C14 C24 3.459(6) . 4_455 no C21 C42 3.555(8) . 4 no C21 C43 3.599(7) . 4 no C23 C62 3.500(8) . . no C24 C25 3.513(7) . 2_666 no C24 C24 3.56(1) . 2_666 no C43 C63 3.49(1) . 4_465 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 C10 O1 . . . . 68.3(4) no Pt1 P1 C10 N1 . . . . -113.2(2) no Pt1 P1 C11 C12 . . . . 109.0(2) no Pt1 P1 C11 C16 . . . . -66.3(4) no Pt1 P1 C20 C21 . . . . -22.2(4) no Pt1 P1 C20 C25 . . . . 165.8(3) no Pt1 P2 C30 O2 . . . . -49.7(4) no Pt1 P2 C30 N2 . . . . 128.6(2) no Pt1 P2 C31 C32 . . . . -129.5(3) no Pt1 P2 C31 C36 . . . . 46.1(4) no Pt1 P2 C41 C42 . . . . 59.2(4) no Pt1 P2 C41 C46 . . . . -123.3(4) no Cl1 Pt1 P1 C10 . . . . 21.1(2) no Cl1 Pt1 P1 C11 . . . . -81.7(2) no Cl1 Pt1 P1 C20 . . . . 138.1(2) no Cl2 Pt1 P2 C30 . . . . 176.4(2) no Cl2 Pt1 P2 C31 . . . . -71.7(1) no Cl2 Pt1 P2 C41 . . . . 59.3(1) no P1 Pt1 P2 C30 . . . . -5.8(2) no P1 Pt1 P2 C31 . . . . 106.1(1) no P1 Pt1 P2 C41 . . . . -122.8(1) no P1 C10 N1 C12 . . . . -3.9(4) no P1 C11 C12 N1 . . . . 6.4(3) no P1 C11 C12 C13 . . . . -174.1(3) no P1 C11 C16 C15 . . . . 175.5(3) no P1 C20 C21 C22 . . . . -170.9(3) no P1 C20 C25 C24 . . . . 171.3(3) no P2 Pt1 P1 C10 . . . . -161.2(2) no P2 Pt1 P1 C11 . . . . 96.0(1) no P2 Pt1 P1 C20 . . . . -44.2(2) no P2 C30 N2 C32 . . . . -3.4(4) no P2 C31 C32 N2 . . . . -0.6(4) no P2 C31 C32 C33 . . . . 178.5(3) no P2 C31 C36 C35 . . . . -177.2(4) no P2 C41 C42 C43 . . . . 177.6(4) no P2 C41 C46 C45 . . . . -178.1(4) no O1 C10 P1 C11 . . . . -172.3(3) no O1 C10 P1 C20 . . . . -61.3(4) no O1 C10 N1 C12 . . . . 174.5(3) no O2 C30 P2 C31 . . . . -175.7(4) no O2 C30 P2 C41 . . . . 76.5(4) no O2 C30 N2 C32 . . . . 174.6(4) no N1 C10 P1 C11 . . . . 6.2(3) no N1 C10 P1 C20 . . . . 117.2(3) no N1 C12 C11 C16 . . . . -177.7(3) no N1 C12 C13 C14 . . . . 177.4(4) no N2 C30 P2 C31 . . . . 2.5(3) no N2 C30 P2 C41 . . . . -105.3(3) no N2 C32 C31 C36 . . . . -176.7(4) no N2 C32 C33 C34 . . . . 177.6(4) no C1 Pt1 P1 C10 . . . . 21.1(2) no C1 Pt1 P1 C11 . . . . -81.7(2) no C1 Pt1 P1 C20 . . . . 138.1(2) no C2 Pt1 P2 C30 . . . . 176.4(2) no C2 Pt1 P2 C31 . . . . -71.7(1) no C2 Pt1 P2 C41 . . . . 59.3(1) no C10 P1 C11 C12 . . . . -7.0(2) no C10 P1 C11 C16 . . . . 177.7(4) no C10 P1 C20 C21 . . . . 101.5(3) no C10 P1 C20 C25 . . . . -70.4(4) no C10 N1 C12 C11 . . . . -1.5(4) no C10 N1 C12 C13 . . . . 179.0(4) no C11 P1 C20 C21 . . . . -164.6(3) no C11 P1 C20 C25 . . . . 23.5(4) no C11 C12 C13 C14 . . . . -2.1(6) no C11 C16 C15 C14 . . . . -2.7(6) no C12 C11 P1 C20 . . . . -106.7(3) no C12 C11 C16 C15 . . . . 0.6(5) no C12 C13 C14 C15 . . . . 0.0(6) no C13 C12 C11 C16 . . . . 1.8(5) no C13 C14 C15 C16 . . . . 2.4(7) no C16 C11 P1 C20 . . . . 78.0(4) no C20 C21 C22 C23 . . . . -0.5(7) no C20 C25 C24 C23 . . . . -0.6(7) no C21 C20 C25 C24 . . . . -0.5(6) no C21 C22 C23 C24 . . . . -0.6(7) no C22 C21 C20 C25 . . . . 1.0(6) no C22 C23 C24 C25 . . . . 1.1(7) no C30 P2 C31 C32 . . . . -1.1(3) no C30 P2 C31 C36 . . . . 174.5(4) no C30 P2 C41 C42 . . . . -71.6(4) no C30 P2 C41 C46 . . . . 105.9(4) no C30 N2 C32 C31 . . . . 2.9(5) no C30 N2 C32 C33 . . . . -176.1(4) no C31 P2 C41 C42 . . . . -164.4(3) no C31 P2 C41 C46 . . . . 13.1(4) no C31 C32 C33 C34 . . . . -1.3(6) no C31 C36 C35 C34 . . . . 0.7(7) no C32 C31 P2 C41 . . . . 95.9(3) no C32 C31 C36 C35 . . . . -2.0(6) no C32 C33 C34 C35 . . . . 0.0(7) no C33 C32 C31 C36 . . . . 2.3(6) no C33 C34 C35 C36 . . . . 0.3(8) no C36 C31 P2 C41 . . . . -88.4(4) no C41 C42 C43 C44 . . . . 0.8(7) no C41 C46 C45 C44 . . . . 0.6(8) no C42 C41 C46 C45 . . . . -0.7(7) no C42 C43 C44 C45 . . . . -0.9(8) no C43 C42 C41 C46 . . . . 0.1(7) no C43 C44 C45 C46 . . . . 0.3(9) no #------------------------------------------------------------------------------ loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O50 H50 Cl1 0.86(3) 2.52(4) 3.231(4) 141(4) 1_565 no O60 H60 O50 0.85(2) 1.88(2) 2.714(5) 167(3) . no N1 H1 O1 0.90 1.936 2.818(4) 166 2_656 no N2 H2 O60 0.90 1.875 2.750(5) 163 . no O50 H50 Cl2 0.86(3) 2.81(3) 3.573(4) 148(4) 1_565 no #===END