data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name _publ_author_address 'Salem, Geoffrey ' ; Department of Chemistry, The Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_contact_author_name 'Salem, Geoffrey ' _publ_contact_author_email geoff.salem@anu.edu.au _publ_section_title ; Manuscript Title: Chiral Birch reduced tertiary phosphines: precursors to asymmetric 1,2-cyclohexenebis(tertiary phosphines) ; _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 '- sal0801a1.cif' data_sal0801a _database_code_depnum_ccdc_archive 'CCDC 781096' #TrackingRef '- sal0801a1.cif' _audit_creation_date 08-10-22 _audit_creation_method CRYSTALS_ver_12.85 _audit_update_record ; 2008-10-22 - Report on 'C29 H41 Cl N O0.5 P Pd by Anthony C. Willis for Geoff Salem and Minghui Chu 2008-10-22 - passes checkcif tests with minor warnings 2008-10-23 - fix up error ; _oxford_structure_analysis_title '10211636 sal0801' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 11.5899(2) _cell_length_b 11.5899(2) _cell_length_c 42.4182(8) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5697.86(18) _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P 43 21 2 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -y+1/2,x+1/2,z+3/4 -x,-y,z+1/2 y+1/2,-x+1/2,z+1/4 -x+1/2,y+1/2,-z+3/4 y,x,-z x+1/2,-y+1/2,-z+1/4 -y,-x,-z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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 8 # Given Formula = C28 H39 Cl1 N1 O0.25 P1 Pd1 # Dc = 1.32 Fooo = 2432.00 Mu = 8.17 M = 566.45 # Found Formula = C29 H41 Cl1 N1 O0.50 P1 Pd1 # Dc = 1.36 FOOO = 2432.00 Mu = 8.20 M = 584.48 _chemical_formula_sum 'C29 H41 Cl N O0.50 P Pd' _chemical_formula_moiety ' C27 H37 Cl N P Pd, 0.5(C4 H8 O)' _chemical_compound_source local _chemical_formula_weight 584.48 _cell_measurement_reflns_used 101202 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 200 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_min 0.06 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_max 0.22 _exptl_crystal_density_diffrn 1.363 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2432 _exptl_absorpt_coefficient_mu 0.820 # Sheldrick geometric approximatio 0.83 0.95 # Absorption correction _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.790 _exptl_absorpt_correction_T_max 0.952 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995,1997) implemented in maxus (2000) ; # 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 'Nonius KappaCCD' _diffrn_measurement_device_type Area _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 0.5 deg at rate 55 sec/frame, crystal-detector distance 60mm, multiple scan sets so over 90 percent of data collected with 2-fold redundancy or more [not assuming Friedel's Law]. ; # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics ; 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 51750 _reflns_number_total 6487 _diffrn_reflns_av_R_equivalents 0.064 # Number of reflections with Friedels Law is 3813 # Number of reflections without Friedels Law is 6487 # Theoretical number of reflections is about 3252 _diffrn_reflns_theta_min 2.664 _diffrn_reflns_theta_max 27.439 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.439 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -54 _diffrn_reflns_limit_l_max 54 _reflns_limit_h_min -10 _reflns_limit_h_max 10 _reflns_limit_k_min 0 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 54 _oxford_diffrn_Wilson_B_factor 2.30 _oxford_diffrn_Wilson_scale 55.89 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.69 _refine_diff_density_max 0.49 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 6487 _refine_ls_number_restraints 40 _refine_ls_number_parameters 326 _oxford_refine_ls_R_factor_ref 0.0446 _refine_ls_wR_factor_ref 0.0879 _refine_ls_goodness_of_fit_ref 0.8527 _refine_ls_shift/su_max 0.047563 # The values computed from all data _oxford_reflns_number_all 6487 _refine_ls_R_factor_all 0.0446 _refine_ls_wR_factor_all 0.0879 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4703 _refine_ls_R_factor_gt 0.0265 _refine_ls_wR_factor_gt 0.0684 _refine_ls_abs_structure_Flack 0.02(3) _refine_ls_abs_structure_details 'Flack (1983), 2674 Friedel-pairs' # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration ad _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # 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: 13.8 20.4 10.8 3.28 ; #============================================================================== # 4. TEXT _publ_section_abstract #Text of the abstract ; The crystal structure of [Pd(C~10~H~14~N)(C~17~H~23~P)Cl].0.5C~4~H~8~O is reported. ; _publ_section_comment #Text of the paper ; The crystallographic asymmetric unit consists of one [Pd(C~10~H~14~N)(C~17~H~23~P)Cl] molecule, and one tetrahydrofuran molecule of crystallization disordered across a crystallographic two-fold axis. The compound is enantiometrically pure. Its absolute configuration has been determined by refinement of the Flack parameter and is in agreement with the configuration expected on the basis of the synthetic precursors. ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions #Captions to figures ; ? ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen for refinement keywords. ; The tetrahydrofuran molecule is located about a two-fold crystallographic axis. An ordered model of this molecule lead to large displacement parameters and some unsatisfactory bond lengths and angles. Sites of half-occupancy were therefore introduced and refinement proceeded with restraints on bonded distances and angles and on adjacent displacement parameters. All hydrogen atoms were included at calculated positions (C---H 1.00\%A, U~iso~(H) = 1.2\\timesU~eq~(C)) and ride on the atom to which they are attached. The biggest peaks in the final difference electron density map were located near the Pd atom or within the solvate molecule. ; _publ_section_exptl_prep ; The compound was recrystallized from tetrahydrofuran and water. The sample ID is MH01. ; #========================================================================== ## -------------------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. Blessing, R. H. (1995). Acta Crystallogr., Section A, 51, 33-37. Blessing, R. H. (1997). J. Appl. Crystallogr., 30, 421-426. 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. Flack, H.D. (1983) Acta Cryst., A39, 876-881. 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 _oxford_atom_site_special_shape _atom_site_attached_hydrogens Pd1 Pd 0.524491(19) 1.012163(19) 0.416529(6) 0.0276 1.0000 Uani . . . . . . . Cl1 Cl 0.60134(10) 0.83254(9) 0.39758(3) 0.0523 1.0000 Uani . . . . . . . P1 P 0.36820(7) 0.92331(7) 0.43722(2) 0.0252 1.0000 Uani . . . . . . . O51 O 0.9073(17) 0.9311(13) 0.4932(5) 0.1460 0.5000 Uani D U . . . . . N1 N 0.6699(3) 1.1047(3) 0.39715(8) 0.0363 1.0000 Uani . . . . . . . C1 C 0.4768(3) 1.1757(3) 0.42882(8) 0.0281 1.0000 Uani . . . . . . . C2 C 0.3960(3) 1.2159(3) 0.45060(9) 0.0286 1.0000 Uani . . . . . . . C3 C 0.3794(3) 1.3341(3) 0.45580(9) 0.0321 1.0000 Uani . . . . . . . C4 C 0.4455(3) 1.4151(3) 0.43999(9) 0.0338 1.0000 Uani . . . . . . . C5 C 0.5272(3) 1.3768(3) 0.41860(9) 0.0347 1.0000 Uani . . . . . . . C6 C 0.5419(3) 1.2590(3) 0.41279(9) 0.0300 1.0000 Uani . . . . . . . C7 C 0.6231(4) 1.2203(3) 0.38729(11) 0.0392 1.0000 Uani . . . . . . . C8 C 0.5604(5) 1.2144(5) 0.35577(11) 0.0603 1.0000 Uani . . . . . . . C9 C 0.7521(4) 1.1227(4) 0.42368(13) 0.0514 1.0000 Uani . . . . . . . C10 C 0.7362(4) 1.0491(4) 0.37143(14) 0.0577 1.0000 Uani . . . . . . . C11 C 0.3333(3) 0.9604(3) 0.47779(8) 0.0289 1.0000 Uani . . . . . . . C12 C 0.2213(3) 0.9625(3) 0.48996(9) 0.0349 1.0000 Uani . . . . . . . C13 C 0.2032(4) 0.9838(4) 0.52194(10) 0.0466 1.0000 Uani . . . . . . . C14 C 0.2955(4) 1.0029(4) 0.54168(10) 0.0526 1.0000 Uani . . . . . . . C15 C 0.4069(4) 1.0028(4) 0.52984(10) 0.0487 1.0000 Uani . . . . . . . C16 C 0.4247(3) 0.9826(4) 0.49827(9) 0.0377 1.0000 Uani . . . . . . . C17 C 0.3825(3) 0.7613(3) 0.44140(9) 0.0318 1.0000 Uani . . . . . . . C18 C 0.4752(4) 0.7328(3) 0.46463(10) 0.0382 1.0000 Uani . . . . . . . C19 C 0.4520(4) 0.6919(4) 0.49332(11) 0.0482 1.0000 Uani . . . . . . . C20 C 0.3321(5) 0.6726(5) 0.50489(12) 0.0596 1.0000 Uani . . . . . . . C21 C 0.2466(4) 0.6683(4) 0.47885(12) 0.0516 1.0000 Uani . . . . . . . C22 C 0.2687(4) 0.7066(3) 0.44992(10) 0.0385 1.0000 Uani . . . . . . . C23 C 0.2340(3) 0.9396(3) 0.41351(9) 0.0288 1.0000 Uani . . . . . . . C24 C 0.1956(3) 1.0658(3) 0.41072(10) 0.0349 1.0000 Uani . . . . . . . C25 C 0.0799(4) 1.0778(4) 0.39364(11) 0.0454 1.0000 Uani . . . . . . . C26 C 0.2463(4) 0.8774(4) 0.38128(9) 0.0365 1.0000 Uani . . . . . . . C27 C 0.3184(4) 0.9393(5) 0.35695(10) 0.0541 1.0000 Uani . . . . . . . C52 C 0.809(2) 0.9301(14) 0.5115(6) 0.1413 0.5000 Uani D U . . . . . C53 C 0.782(2) 0.8048(14) 0.5177(6) 0.1437 0.5000 Uani D U . . . . . C54 C 0.845(2) 0.7459(14) 0.4915(7) 0.1469 0.5000 Uani D U . . . . . C55 C 0.916(2) 0.8358(17) 0.4760(6) 0.1477 0.5000 Uani D U . . . . . H21 H 0.3489 1.1591 0.4628 0.0343 1.0000 Uiso R . . . . . . H31 H 0.3192 1.3602 0.4711 0.0384 1.0000 Uiso R . . . . . . H41 H 0.4343 1.4995 0.4439 0.0405 1.0000 Uiso R . . . . . . H51 H 0.5764 1.4341 0.4072 0.0416 1.0000 Uiso R . . . . . . H71 H 0.6882 1.2765 0.3857 0.0469 1.0000 Uiso R . . . . . . H81 H 0.5308 1.2927 0.3501 0.0723 1.0000 Uiso R . . . . . . H82 H 0.6151 1.1872 0.3391 0.0723 1.0000 Uiso R . . . . . . H83 H 0.4943 1.1593 0.3574 0.0723 1.0000 Uiso R . . . . . . H91 H 0.7841 1.0466 0.4305 0.0616 1.0000 Uiso R . . . . . . H92 H 0.7108 1.1598 0.4417 0.0616 1.0000 Uiso R . . . . . . H93 H 0.8165 1.1738 0.4166 0.0616 1.0000 Uiso R . . . . . . H101 H 0.7658 0.9727 0.3788 0.0690 1.0000 Uiso R . . . . . . H102 H 0.8026 1.0996 0.3654 0.0690 1.0000 Uiso R . . . . . . H103 H 0.6849 1.0375 0.3527 0.0690 1.0000 Uiso R . . . . . . H121 H 0.1539 0.9487 0.4757 0.0419 1.0000 Uiso R . . . . . . H131 H 0.1229 0.9852 0.5306 0.0559 1.0000 Uiso R . . . . . . H141 H 0.2821 1.0168 0.5646 0.0632 1.0000 Uiso R . . . . . . H151 H 0.4739 1.0173 0.5441 0.0585 1.0000 Uiso R . . . . . . H161 H 0.5052 0.9838 0.4898 0.0453 1.0000 Uiso R . . . . . . H171 H 0.4066 0.7298 0.4205 0.0381 1.0000 Uiso R . . . . . . H181 H 0.5576 0.7447 0.4584 0.0457 1.0000 Uiso R . . . . . . H191 H 0.5178 0.6734 0.5077 0.0576 1.0000 Uiso R . . . . . . H201 H 0.3109 0.7370 0.5195 0.0716 1.0000 Uiso R . . . . . . H202 H 0.3296 0.5977 0.5166 0.0716 1.0000 Uiso R . . . . . . H211 H 0.1686 0.6349 0.4833 0.0619 1.0000 Uiso R . . . . . . H221 H 0.2079 0.6989 0.4333 0.0462 1.0000 Uiso R . . . . . . H231 H 0.1717 0.8983 0.4253 0.0345 1.0000 Uiso R . . . . . . H241 H 0.1879 1.0990 0.4324 0.0417 1.0000 Uiso R . . . . . . H242 H 0.2555 1.1096 0.3987 0.0417 1.0000 Uiso R . . . . . . H251 H 0.0582 1.1612 0.3924 0.0544 1.0000 Uiso R . . . . . . H252 H 0.0191 1.0347 0.4055 0.0544 1.0000 Uiso R . . . . . . H253 H 0.0867 1.0453 0.3719 0.0544 1.0000 Uiso R . . . . . . H261 H 0.2823 0.8003 0.3852 0.0439 1.0000 Uiso R . . . . . . H262 H 0.1672 0.8667 0.3723 0.0439 1.0000 Uiso R . . . . . . H271 H 0.3210 0.8925 0.3372 0.0648 1.0000 Uiso R . . . . . . H272 H 0.3985 0.9500 0.3652 0.0648 1.0000 Uiso R . . . . . . H273 H 0.2835 1.0163 0.3524 0.0648 1.0000 Uiso R . . . . . . H521 H 0.8211 0.9728 0.5317 0.1660 0.5000 Uiso R . . . . . . H522 H 0.7434 0.9663 0.4996 0.1660 0.5000 Uiso R . . . . . . H531 H 0.8129 0.7807 0.5387 0.1690 0.5000 Uiso R . . . . . . H532 H 0.6974 0.7888 0.5168 0.1690 0.5000 Uiso R . . . . . . H541 H 0.8953 0.6834 0.5000 0.1729 0.5000 Uiso R . . . . . . H542 H 0.7884 0.7119 0.4762 0.1729 0.5000 Uiso R . . . . . . H551 H 0.9979 0.8104 0.4748 0.1733 0.5000 Uiso R . . . . . . H552 H 0.8856 0.8508 0.4543 0.1733 0.5000 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 Pd1 0.02350(12) 0.02338(12) 0.03587(12) -0.00445(9) 0.00713(10) -0.00049(10) Cl1 0.0472(6) 0.0287(5) 0.0809(8) -0.0105(5) 0.0319(6) 0.0016(4) P1 0.0241(4) 0.0223(4) 0.0293(4) -0.0011(3) 0.0032(3) -0.0009(3) O51 0.188(14) 0.057(5) 0.193(14) -0.003(7) 0.076(10) -0.049(7) N1 0.0266(15) 0.0281(15) 0.054(2) -0.0051(14) 0.0179(14) -0.0019(12) C1 0.0270(16) 0.0229(14) 0.0344(17) -0.0012(12) 0.0003(15) -0.0005(14) C2 0.0281(18) 0.0248(17) 0.0330(19) -0.0018(13) 0.0046(15) 0.0032(14) C3 0.036(2) 0.0278(17) 0.0322(19) -0.0026(14) 0.0002(15) 0.0038(15) C4 0.0370(19) 0.0257(17) 0.039(2) -0.0018(14) -0.0037(16) 0.0031(14) C5 0.0325(18) 0.0265(16) 0.045(2) 0.0028(15) -0.0016(18) -0.0023(15) C6 0.0268(18) 0.0279(16) 0.0353(19) -0.0017(14) 0.0045(15) -0.0009(13) C7 0.033(2) 0.0289(19) 0.056(3) 0.0019(18) 0.0167(18) -0.0015(16) C8 0.074(4) 0.070(3) 0.037(3) 0.004(2) 0.016(2) 0.011(3) C9 0.0234(19) 0.046(2) 0.084(4) -0.005(2) -0.003(2) -0.0010(18) C10 0.049(3) 0.039(2) 0.085(4) -0.006(2) 0.042(3) -0.0022(19) C11 0.0308(17) 0.0233(17) 0.0326(17) 0.0003(14) 0.0037(14) -0.0005(13) C12 0.0366(19) 0.033(2) 0.035(2) 0.0001(16) 0.0103(15) -0.0046(16) C13 0.049(2) 0.048(2) 0.043(2) -0.009(2) 0.0171(18) -0.003(2) C14 0.066(3) 0.057(3) 0.035(2) -0.0092(19) 0.014(2) -0.011(2) C15 0.056(2) 0.054(3) 0.036(2) -0.0118(18) 0.0007(17) -0.007(2) C16 0.0384(18) 0.0374(19) 0.0374(18) -0.0039(17) 0.0010(14) -0.0035(16) C17 0.036(2) 0.0247(17) 0.035(2) -0.0027(15) -0.0005(16) 0.0011(15) C18 0.037(2) 0.0274(16) 0.050(2) -0.0017(15) -0.0030(19) 0.0083(17) C19 0.058(3) 0.033(2) 0.054(3) 0.0061(19) -0.010(2) 0.010(2) C20 0.077(4) 0.049(3) 0.053(3) 0.021(2) 0.009(3) 0.001(3) C21 0.055(3) 0.034(2) 0.066(3) 0.011(2) 0.013(2) -0.0046(19) C22 0.037(2) 0.0236(17) 0.054(2) -0.0002(16) 0.0007(18) -0.0033(15) C23 0.0273(17) 0.0310(17) 0.0281(18) -0.0023(15) 0.0012(14) -0.0014(14) C24 0.032(2) 0.0339(19) 0.038(2) -0.0027(16) -0.0010(16) 0.0052(15) C25 0.040(2) 0.045(2) 0.051(3) -0.007(2) -0.0075(19) 0.0140(18) C26 0.040(2) 0.0345(19) 0.035(2) -0.0119(16) -0.0049(16) 0.0062(17) C27 0.042(2) 0.086(4) 0.034(2) -0.008(2) 0.0068(18) -0.001(2) C52 0.182(14) 0.055(6) 0.187(14) -0.021(8) 0.081(11) -0.037(8) C53 0.189(14) 0.063(7) 0.180(13) -0.014(8) 0.078(11) -0.043(8) C54 0.189(14) 0.067(7) 0.184(13) -0.020(8) 0.073(12) -0.039(8) C55 0.189(14) 0.076(7) 0.179(14) -0.030(8) 0.074(11) -0.044(8) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.14540(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pd1 . Cl1 . 2.4027(10) yes Pd1 . P1 . 2.2609(9) yes Pd1 . N1 . 2.160(3) yes Pd1 . C1 . 2.042(3) yes P1 . C11 . 1.819(4) yes P1 . C17 . 1.893(4) yes P1 . C23 . 1.861(4) yes O51 . C52 . 1.383(15) yes O51 . C55 . 1.326(15) yes N1 . C7 . 1.505(5) yes N1 . C9 . 1.489(6) yes N1 . C10 . 1.481(5) yes C1 . C2 . 1.396(5) yes C1 . C6 . 1.402(5) yes C2 . C3 . 1.400(5) yes C2 . H21 . 1.000 no C3 . C4 . 1.385(5) yes C3 . H31 . 1.000 no C4 . C5 . 1.385(5) yes C4 . H41 . 1.000 no C5 . C6 . 1.397(5) yes C5 . H51 . 1.000 no C6 . C7 . 1.502(5) yes C7 . C8 . 1.523(7) yes C7 . H71 . 1.000 no C8 . H81 . 1.000 no C8 . H82 . 1.000 no C8 . H83 . 1.000 no C9 . H91 . 1.000 no C9 . H92 . 1.000 no C9 . H93 . 1.000 no C10 . H101 . 1.000 no C10 . H102 . 1.000 no C10 . H103 . 1.000 no C11 . C12 . 1.397(5) yes C11 . C16 . 1.394(5) yes C12 . C13 . 1.395(6) yes C12 . H121 . 1.000 no C13 . C14 . 1.376(7) yes C13 . H131 . 1.000 no C14 . C15 . 1.385(6) yes C14 . H141 . 1.000 no C15 . C16 . 1.375(6) yes C15 . H151 . 1.000 no C16 . H161 . 1.000 no C17 . C18 . 1.495(5) yes C17 . C22 . 1.508(5) yes C17 . H171 . 1.000 no C18 . C19 . 1.333(6) yes C18 . H181 . 1.000 no C19 . C20 . 1.490(7) yes C19 . H191 . 1.000 no C20 . C21 . 1.485(7) yes C20 . H201 . 1.000 no C20 . H202 . 1.000 no C21 . C22 . 1.330(6) yes C21 . H211 . 1.000 no C22 . H221 . 1.000 no C23 . C24 . 1.533(5) yes C23 . C26 . 1.552(5) yes C23 . H231 . 1.000 no C24 . C25 . 1.530(5) yes C24 . H241 . 1.000 no C24 . H242 . 1.000 no C25 . H251 . 1.000 no C25 . H252 . 1.000 no C25 . H253 . 1.000 no C26 . C27 . 1.509(6) yes C26 . H261 . 1.000 no C26 . H262 . 1.000 no C27 . H271 . 1.000 no C27 . H272 . 1.000 no C27 . H273 . 1.000 no C52 . C53 . 1.508(16) yes C52 . H521 . 1.000 no C52 . H522 . 1.000 no C53 . C54 . 1.492(14) yes C53 . H531 . 1.000 no C53 . H532 . 1.000 no C54 . C55 . 1.483(17) yes C54 . H541 . 1.000 no C54 . H542 . 1.000 no C55 . H551 . 1.000 no C55 . H552 . 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 . Pd1 . P1 . 91.84(3) yes Cl1 . Pd1 . N1 . 90.77(9) yes P1 . Pd1 . N1 . 177.33(9) yes Cl1 . Pd1 . C1 . 171.87(10) yes P1 . Pd1 . C1 . 96.13(10) yes N1 . Pd1 . C1 . 81.23(13) yes Pd1 . P1 . C11 . 115.97(12) yes Pd1 . P1 . C17 . 114.71(13) yes C11 . P1 . C17 . 99.50(17) yes Pd1 . P1 . C23 . 114.42(12) yes C11 . P1 . C23 . 107.52(16) yes C17 . P1 . C23 . 102.96(17) yes C52 . O51 . C55 . 111.2(10) yes Pd1 . N1 . C7 . 105.4(2) yes Pd1 . N1 . C9 . 106.3(3) yes C7 . N1 . C9 . 108.4(3) yes Pd1 . N1 . C10 . 118.0(3) yes C7 . N1 . C10 . 111.7(4) yes C9 . N1 . C10 . 106.6(4) yes Pd1 . C1 . C2 . 131.4(3) yes Pd1 . C1 . C6 . 111.7(3) yes C2 . C1 . C6 . 116.9(3) yes C1 . C2 . C3 . 121.6(3) yes C1 . C2 . H21 . 119.2 no C3 . C2 . H21 . 119.2 no C2 . C3 . C4 . 120.7(4) yes C2 . C3 . H31 . 119.6 no C4 . C3 . H31 . 119.6 no C3 . C4 . C5 . 118.5(3) yes C3 . C4 . H41 . 120.7 no C5 . C4 . H41 . 120.7 no C4 . C5 . C6 . 120.8(3) yes C4 . C5 . H51 . 119.6 no C6 . C5 . H51 . 119.6 no C1 . C6 . C5 . 121.5(3) yes C1 . C6 . C7 . 118.7(3) yes C5 . C6 . C7 . 119.7(3) yes N1 . C7 . C6 . 107.0(3) yes N1 . C7 . C8 . 112.1(4) yes C6 . C7 . C8 . 110.3(4) yes N1 . C7 . H71 . 109.1 no C6 . C7 . H71 . 109.1 no C8 . C7 . H71 . 109.1 no C7 . C8 . H81 . 109.5 no C7 . C8 . H82 . 109.5 no H81 . C8 . H82 . 109.5 no C7 . C8 . H83 . 109.5 no H81 . C8 . H83 . 109.5 no H82 . C8 . H83 . 109.5 no N1 . C9 . H91 . 109.5 no N1 . C9 . H92 . 109.5 no H91 . C9 . H92 . 109.5 no N1 . C9 . H93 . 109.5 no H91 . C9 . H93 . 109.5 no H92 . C9 . H93 . 109.5 no N1 . C10 . H101 . 109.4 no N1 . C10 . H102 . 109.4 no H101 . C10 . H102 . 109.5 no N1 . C10 . H103 . 109.5 no H101 . C10 . H103 . 109.5 no H102 . C10 . H103 . 109.5 no P1 . C11 . C12 . 124.1(3) yes P1 . C11 . C16 . 117.6(3) yes C12 . C11 . C16 . 118.2(3) yes C11 . C12 . C13 . 120.1(4) yes C11 . C12 . H121 . 119.9 no C13 . C12 . H121 . 119.9 no C12 . C13 . C14 . 120.2(4) yes C12 . C13 . H131 . 119.9 no C14 . C13 . H131 . 119.9 no C13 . C14 . C15 . 120.3(4) yes C13 . C14 . H141 . 119.9 no C15 . C14 . H141 . 119.9 no C14 . C15 . C16 . 119.5(4) yes C14 . C15 . H151 . 120.3 no C16 . C15 . H151 . 120.2 no C11 . C16 . C15 . 121.7(4) yes C11 . C16 . H161 . 119.2 no C15 . C16 . H161 . 119.2 no P1 . C17 . C18 . 110.1(3) yes P1 . C17 . C22 . 111.3(3) yes C18 . C17 . C22 . 112.2(3) yes P1 . C17 . H171 . 107.7 no C18 . C17 . H171 . 107.7 no C22 . C17 . H171 . 107.7 no C17 . C18 . C19 . 122.4(4) yes C17 . C18 . H181 . 118.8 no C19 . C18 . H181 . 118.8 no C18 . C19 . C20 . 122.8(4) yes C18 . C19 . H191 . 118.6 no C20 . C19 . H191 . 118.6 no C19 . C20 . C21 . 112.5(4) yes C19 . C20 . H201 . 108.7 no C21 . C20 . H201 . 108.7 no C19 . C20 . H202 . 108.7 no C21 . C20 . H202 . 108.7 no H201 . C20 . H202 . 109.5 no C20 . C21 . C22 . 123.1(4) yes C20 . C21 . H211 . 118.4 no C22 . C21 . H211 . 118.4 no C17 . C22 . C21 . 122.0(4) yes C17 . C22 . H221 . 119.0 no C21 . C22 . H221 . 119.0 no P1 . C23 . C24 . 112.4(2) yes P1 . C23 . C26 . 110.6(3) yes C24 . C23 . C26 . 113.7(3) yes P1 . C23 . H231 . 106.6 no C24 . C23 . H231 . 106.6 no C26 . C23 . H231 . 106.5 no C23 . C24 . C25 . 112.2(3) yes C23 . C24 . H241 . 108.8 no C25 . C24 . H241 . 108.8 no C23 . C24 . H242 . 108.8 no C25 . C24 . H242 . 108.8 no H241 . C24 . H242 . 109.5 no C24 . C25 . H251 . 109.5 no C24 . C25 . H252 . 109.5 no H251 . C25 . H252 . 109.5 no C24 . C25 . H253 . 109.5 no H251 . C25 . H253 . 109.5 no H252 . C25 . H253 . 109.5 no C23 . C26 . C27 . 115.7(4) yes C23 . C26 . H261 . 107.9 no C27 . C26 . H261 . 107.9 no C23 . C26 . H262 . 107.9 no C27 . C26 . H262 . 107.9 no H261 . C26 . H262 . 109.5 no C26 . C27 . H271 . 109.5 no C26 . C27 . H272 . 109.5 no H271 . C27 . H272 . 109.5 no C26 . C27 . H273 . 109.5 no H271 . C27 . H273 . 109.5 no H272 . C27 . H273 . 109.5 no O51 . C52 . C53 . 105.9(13) yes O51 . C52 . H521 . 111.0 no C53 . C52 . H521 . 110.9 no O51 . C52 . H522 . 109.8 no C53 . C52 . H522 . 109.8 no H521 . C52 . H522 . 109.5 no C52 . C53 . C54 . 102.2(14) yes C52 . C53 . H531 . 110.6 no C54 . C53 . H531 . 111.3 no C52 . C53 . H532 . 111.8 no C54 . C53 . H532 . 111.3 no H531 . C53 . H532 . 109.5 no C53 . C54 . C55 . 106.1(14) yes C53 . C54 . H541 . 110.3 no C55 . C54 . H541 . 110.0 no C53 . C54 . H542 . 110.3 no C55 . C54 . H542 . 110.5 no H541 . C54 . H542 . 109.5 no C54 . C55 . O51 . 107.6(13) yes C54 . C55 . H551 . 110.2 no O51 . C55 . H551 . 110.1 no C54 . C55 . H552 . 109.8 no O51 . C55 . H552 . 109.7 no H551 . C55 . H552 . 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 O51 C13 3.34(2) . 6_566 no O51 C12 3.50(2) . 6_566 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 C11 C12 . . . . 148.4(3) no Pd1 P1 C11 C16 . . . . -34.8(3) no Pd1 P1 C17 C18 . . . . 64.8(3) no Pd1 P1 C17 C22 . . . . -170.1(2) no Pd1 P1 C23 C24 . . . . -62.5(3) no Pd1 P1 C23 C26 . . . . 65.8(3) no Pd1 N1 C7 C6 . . . . 41.3(3) no Pd1 N1 C7 C8 . . . . -79.6(4) no Pd1 C1 C2 C3 . . . . 178.3(3) no Pd1 C1 C6 C5 . . . . -177.2(3) no Pd1 C1 C6 C7 . . . . 7.0(4) no Cl1 Pd1 P1 C11 . . . . 131.0(1) no Cl1 Pd1 P1 C17 . . . . 15.8(1) no Cl1 Pd1 P1 C23 . . . . -102.9(1) no Cl1 Pd1 N1 C7 . . . . 147.0(2) no Cl1 Pd1 N1 C9 . . . . -98.0(3) no Cl1 Pd1 N1 C10 . . . . 21.5(3) no P1 Pd1 C1 C2 . . . . 17.2(3) no P1 Pd1 C1 C6 . . . . -165.4(2) no P1 C11 C12 C13 . . . . 175.3(3) no P1 C11 C16 C15 . . . . -175.1(4) no P1 C17 C18 C19 . . . . 107.3(4) no P1 C17 C22 C21 . . . . -105.3(4) no P1 C23 C24 C25 . . . . -175.1(3) no P1 C23 C26 C27 . . . . -76.5(4) no O51 C52 C53 C54 . . . . -21(3) no O51 C55 C54 C53 . . . . 7(3) no N1 Pd1 C1 C2 . . . . -163.2(4) no N1 Pd1 C1 C6 . . . . 14.1(3) no N1 C7 C6 C1 . . . . -34.1(5) no N1 C7 C6 C5 . . . . 150.1(3) no C1 Pd1 P1 C11 . . . . -50.6(2) no C1 Pd1 P1 C17 . . . . -165.8(2) no C1 Pd1 P1 C23 . . . . 75.5(2) no C1 Pd1 N1 C7 . . . . -31.5(3) no C1 Pd1 N1 C9 . . . . 83.5(3) no C1 Pd1 N1 C10 . . . . -157.0(3) no C1 C2 C3 C4 . . . . -1.8(6) no C1 C6 C5 C4 . . . . -1.5(6) no C1 C6 C7 C8 . . . . 88.0(4) no C2 C1 C6 C5 . . . . 0.6(5) no C2 C1 C6 C7 . . . . -175.2(3) no C2 C3 C4 C5 . . . . 0.9(5) no C3 C2 C1 C6 . . . . 1.1(5) no C3 C4 C5 C6 . . . . 0.7(5) no C4 C5 C6 C7 . . . . 174.2(4) no C5 C6 C7 C8 . . . . -87.8(4) no C6 C7 N1 C9 . . . . -72.2(4) no C6 C7 N1 C10 . . . . 170.6(3) no C8 C7 N1 C9 . . . . 166.8(4) no C8 C7 N1 C10 . . . . 49.7(5) no C11 P1 C17 C18 . . . . -59.6(3) no C11 P1 C17 C22 . . . . 65.4(3) no C11 P1 C23 C24 . . . . 67.9(3) no C11 P1 C23 C26 . . . . -163.8(3) no C11 C12 C13 C14 . . . . 0.0(6) no C11 C16 C15 C14 . . . . -1.0(7) no C12 C11 P1 C17 . . . . -88.0(3) no C12 C11 P1 C23 . . . . 18.9(4) no C12 C11 C16 C15 . . . . 1.9(6) no C12 C13 C14 C15 . . . . 1.0(7) no C13 C12 C11 C16 . . . . -1.4(6) no C13 C14 C15 C16 . . . . -0.5(7) no C16 C11 P1 C17 . . . . 88.8(3) no C16 C11 P1 C23 . . . . -164.3(3) no C17 P1 C23 C24 . . . . 172.4(3) no C17 P1 C23 C26 . . . . -59.3(3) no C17 C18 C19 C20 . . . . -0.9(7) no C17 C22 C21 C20 . . . . -1.9(7) no C18 C17 P1 C23 . . . . -170.2(3) no C18 C17 C22 C21 . . . . 18.6(5) no C18 C19 C20 C21 . . . . 17.8(7) no C19 C18 C17 C22 . . . . -17.2(5) no C19 C20 C21 C22 . . . . -16.3(7) no C22 C17 P1 C23 . . . . -45.2(3) no C24 C23 C26 C27 . . . . 51.0(5) no C25 C24 C23 C26 . . . . 58.3(4) no C52 O51 C55 C54 . . . . -22(3) no C52 C53 C54 C55 . . . . 9(3) no C53 C52 O51 C55 . . . . 28(3) no #------------------------------------------------------------------------------ #===END # Attachment '- sal1001.cif' data_sal1001 _database_code_depnum_ccdc_archive 'CCDC 781097' #TrackingRef '- sal1001.cif' _audit_creation_date 10-05-18 _audit_creation_method CRYSTALS_ver_12.87 _audit_update_record ; 2010-05-18 - Report on C29 H36 P2 Pt by Anthony C. Willis for Geoff Salem and Roy Doylen 2010-05-18 - passes checkcif tests with minor warnings ; _oxford_structure_analysis_title '4121217 sal1001' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 10.2514(1) _cell_length_b 16.8489(2) _cell_length_c 15.6183(2) _cell_angle_alpha 90 _cell_angle_beta 97.5919(7) _cell_angle_gamma 90 _cell_volume 2674.02(5) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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' 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' _cell_formula_units_Z 4 # Given Formula = C29 H36 P2 Pt1 # Dc = 1.59 Fooo = 1272.00 Mu = 53.82 M = 641.64 # Found Formula = C29 H36.00 P2 Pt1 # Dc = 1.59 FOOO = 1272.00 Mu = 53.82 M = 641.64 _chemical_formula_sum 'C29 H36 P2 Pt' _chemical_formula_moiety 'C29 H36 P2 Pt' _chemical_compound_source local _chemical_formula_weight 641.64 _cell_measurement_reflns_used 71654 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 30 _cell_measurement_temperature 200 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_min 0.120 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_max 0.220 _exptl_crystal_density_diffrn 1.594 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1272.000 _exptl_absorpt_coefficient_mu 5.382 # Sheldrick geometric approximatio 0.34 0.52 # Absorption correction loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -3 3 0 0.120 1 -1 0 0.110 -1 -1 0 0.120 1 1 0 0.080 0 0 1 0.040 0 0 -1 0.075 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.277 _exptl_absorpt_correction_T_max 0.576 _exptl_absorpt_process_details ; via Gaussian method (Coppens, 1970) implemented in maXus (2000) ; #_diffrn_reflns_av_R_equivalents 0.038 # 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 'Nonius KappaCCD' _diffrn_measurement_device_type Area _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 48 sec/frame, crystal-detector distance 28mm, 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, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics ; 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 69946 _reflns_number_total 7853 _diffrn_reflns_av_R_equivalents 0.052 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 7853 # Theoretical number of reflections is about 15721 _diffrn_reflns_theta_min 2.552 _diffrn_reflns_theta_max 30.086 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.086 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _reflns_limit_h_min -14 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 23 _reflns_limit_l_min 0 _reflns_limit_l_max 22 _oxford_diffrn_Wilson_B_factor 2.80 _oxford_diffrn_Wilson_scale 18.60 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.79 _refine_diff_density_max 4.26 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 7847 _refine_ls_number_restraints 31 _refine_ls_number_parameters 335 _oxford_refine_ls_R_factor_ref 0.0453 _refine_ls_wR_factor_ref 0.0874 _refine_ls_goodness_of_fit_ref 0.9906 _refine_ls_shift/su_max 0.0242266 _refine_ls_shift/su_mean 0.0066263 # The values computed from all data _oxford_reflns_number_all 7847 _refine_ls_R_factor_all 0.0453 _refine_ls_wR_factor_all 0.0874 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 6546 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_gt 0.0820 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 8.39P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; #============================================================================== # 4. TEXT _publ_section_abstract #Text of the abstract ; The crystal structure of [Pt(CH~3~)~2~(C~27~H~30~P~2~)] is reported. ; _publ_section_comment #Text of the paper ; The crystallographic asymmetric unit consists of one [Pt(CH~3~)~2~(C~27~H~30~P~2~)] molecule. There is disorder in the cyclohexene ring, with there being alternative sites for atoms C14, C15 and C16. Restraints were imposed on distances and angles involving the minor sites so they would tend to be equal to values obtained for the major sites and restraints were imposed on their displacement parameters. The relative occupancies of major- and minor-sites were refined. ; _publ_section_acknowledgements # Acknowledgments ; ; _publ_section_figure_captions #Captions to figures ; ? ; _refine_special_details #_publ_section_exptl_refinement # see also _refine_ls_hydrogen for refinement keywords. ; The H atoms were included at calculated positions and ride on the atoms to which they are attached. The H atoms of methyl C1 and C2 were oriented to match peaks in a difference map and then allowed to refine positionally while tight restraints were imposed on distances and angles involving them. The largest peaks in the final difference electron density map are located near the Pt atom and C1 and C2. ; _publ_section_exptl_prep ; The compound was prepared by RD and recrystallised from 2-propanol/dichloromethane. The sample ID is RD-3-PtMe2. ; # Insert your own references if required - in alphabetical 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, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. 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 _oxford_atom_site_special_shape _atom_site_attached_hydrogens Pt1 Pt 0.343163(14) 0.334808(9) 0.182383(10) 0.0357 1.0000 Uani D . . . . . . P1 P 0.33662(10) 0.22757(6) 0.26849(7) 0.0369 1.0000 Uani . . . . . . . P2 P 0.17544(10) 0.38061(6) 0.24733(7) 0.0355 1.0000 Uani . . . . . . . C1 C 0.4902(5) 0.2902(3) 0.1136(4) 0.0628 1.0000 Uani D . . . . . . C2 C 0.3609(4) 0.4414(2) 0.1058(3) 0.0442 1.0000 Uani D . . . . . . C11 C 0.1994(4) 0.2397(2) 0.3328(3) 0.0404 1.0000 Uani D U . . . . . C12 C 0.1321(4) 0.3073(2) 0.3264(3) 0.0390 1.0000 Uani . . . . . . . C13 C 0.0210(5) 0.3257(3) 0.3782(3) 0.0490 1.0000 Uani D U . . . . . C14 C -0.0280(10) 0.2508(6) 0.4166(7) 0.0584 0.711(16) Uani . U P . . . . C15 C 0.0814(9) 0.1978(5) 0.4577(6) 0.0551 0.711(16) Uani . U P . . . . C16 C 0.1741(14) 0.1721(6) 0.3926(9) 0.0499 0.711(16) Uani . U P . . . . C111 C 0.3110(4) 0.1295(2) 0.2187(3) 0.0399 1.0000 Uani . . . . . . . C112 C 0.2696(5) 0.1257(3) 0.1312(3) 0.0494 1.0000 Uani . . . . . . . C113 C 0.2502(5) 0.0532(3) 0.0883(4) 0.0603 1.0000 Uani . . . . . . . C114 C 0.2726(5) -0.0170(3) 0.1338(4) 0.0612 1.0000 Uani . . . . . . . C115 C 0.3152(5) -0.0137(3) 0.2219(4) 0.0581 1.0000 Uani . . . . . . . C116 C 0.3342(5) 0.0583(3) 0.2645(3) 0.0497 1.0000 Uani . . . . . . . C121 C 0.4802(5) 0.2148(3) 0.3527(3) 0.0517 1.0000 Uani . . . . . . . C122 C 0.5068(7) 0.2929(4) 0.4016(4) 0.0734 1.0000 Uani . . . . . . . C123 C 0.6024(6) 0.1867(4) 0.3143(4) 0.0742 1.0000 Uani . . . . . . . C211 C 0.0216(4) 0.3923(2) 0.1758(3) 0.0380 1.0000 Uani . . . . . . . C212 C -0.0627(5) 0.3283(2) 0.1596(3) 0.0445 1.0000 Uani . . . . . . . C213 C -0.1760(5) 0.3353(3) 0.1003(4) 0.0511 1.0000 Uani . . . . . . . C214 C -0.2045(5) 0.4052(3) 0.0558(3) 0.0518 1.0000 Uani . . . . . . . C215 C -0.1184(5) 0.4685(3) 0.0694(3) 0.0481 1.0000 Uani . . . . . . . C216 C -0.0068(4) 0.4623(2) 0.1290(3) 0.0421 1.0000 Uani . . . . . . . C221 C 0.1955(4) 0.4732(2) 0.3084(3) 0.0392 1.0000 Uani . . . . . . . C222 C 0.3240(5) 0.4963(3) 0.3388(3) 0.0477 1.0000 Uani . . . . . . . C223 C 0.3472(5) 0.5635(3) 0.3898(4) 0.0596 1.0000 Uani . . . . . . . C224 C 0.2430(6) 0.6079(3) 0.4100(4) 0.0600 1.0000 Uani . . . . . . . C225 C 0.1157(5) 0.5867(3) 0.3801(4) 0.0566 1.0000 Uani . . . . . . . C226 C 0.0907(5) 0.5192(3) 0.3294(3) 0.0470 1.0000 Uani . . . . . . . C314 C 0.012(3) 0.2675(9) 0.4503(13) 0.0592 0.289(16) Uani D U P . . . . C315 C 0.021(2) 0.1842(8) 0.4145(14) 0.0461 0.289(16) Uani D U P . . . . C316 C 0.156(3) 0.1752(12) 0.390(2) 0.0508 0.289(16) Uani D U P . . . . H11 H 0.512(3) 0.2370(10) 0.130(2) 0.0754 1.0000 Uiso D . . . . . . H12 H 0.565(2) 0.3234(17) 0.123(2) 0.0754 1.0000 Uiso D . . . . . . H13 H 0.460(3) 0.29037(10) 0.0539(8) 0.0754 1.0000 Uiso D . . . . . . H21 H 0.302(3) 0.4798(13) 0.121(2) 0.0531 1.0000 Uiso D . . . . . . H22 H 0.4459(16) 0.4617(17) 0.116(2) 0.0531 1.0000 Uiso D . . . . . . H23 H 0.345(4) 0.4298(16) 0.0470(8) 0.0531 1.0000 Uiso D . . . . . . H131 H 0.0518 0.3613 0.4236 0.0587 0.711 Uiso R . . . . . . H132 H -0.0494 0.3496 0.3415 0.0587 0.711 Uiso R . . . . . . H133 H 0.0346 0.3772 0.4025 0.0587 0.289 Uiso R . . . . . . H134 H -0.0596 0.3247 0.3404 0.0587 0.289 Uiso R . . . . . . H141 H -0.0815 0.2652 0.4594 0.0702 0.711 Uiso R . . . . . . H142 H -0.0793 0.2219 0.3719 0.0702 0.711 Uiso R . . . . . . H151 H 0.1312 0.2258 0.5037 0.0662 0.711 Uiso R . . . . . . H152 H 0.0440 0.1518 0.4798 0.0662 0.711 Uiso R . . . . . . H161 H 0.2555 0.1552 0.4234 0.0593 0.711 Uiso R . . . . . . H162 H 0.1348 0.1292 0.3590 0.0593 0.711 Uiso R . . . . . . H1121 H 0.2539 0.1736 0.0993 0.0592 1.0000 Uiso R . . . . . . H1131 H 0.2217 0.0519 0.0279 0.0723 1.0000 Uiso R . . . . . . H1141 H 0.2590 -0.0667 0.1053 0.0734 1.0000 Uiso R . . . . . . H1151 H 0.3315 -0.0617 0.2535 0.0698 1.0000 Uiso R . . . . . . H1161 H 0.3631 0.0595 0.3249 0.0597 1.0000 Uiso R . . . . . . H1211 H 0.4587 0.1757 0.3924 0.0621 1.0000 Uiso R . . . . . . H1221 H 0.5804 0.2868 0.4449 0.0882 1.0000 Uiso R . . . . . . H1222 H 0.5248 0.3334 0.3624 0.0882 1.0000 Uiso R . . . . . . H1223 H 0.4316 0.3072 0.4279 0.0882 1.0000 Uiso R . . . . . . H1231 H 0.6738 0.1808 0.3592 0.0890 1.0000 Uiso R . . . . . . H1232 H 0.6247 0.2247 0.2737 0.0890 1.0000 Uiso R . . . . . . H1233 H 0.5844 0.1371 0.2862 0.0890 1.0000 Uiso R . . . . . . H2121 H -0.0432 0.2795 0.1891 0.0534 1.0000 Uiso R . . . . . . H2131 H -0.2343 0.2915 0.0903 0.0613 1.0000 Uiso R . . . . . . H2141 H -0.2827 0.4098 0.0160 0.0622 1.0000 Uiso R . . . . . . H2151 H -0.1361 0.5163 0.0378 0.0577 1.0000 Uiso R . . . . . . H2161 H 0.0516 0.5062 0.1383 0.0505 1.0000 Uiso R . . . . . . H2221 H 0.3960 0.4657 0.3245 0.0572 1.0000 Uiso R . . . . . . H2231 H 0.4349 0.5788 0.4106 0.0715 1.0000 Uiso R . . . . . . H2241 H 0.2591 0.6538 0.4451 0.0720 1.0000 Uiso R . . . . . . H2251 H 0.0447 0.6182 0.3940 0.0679 1.0000 Uiso R . . . . . . H2261 H 0.0026 0.5043 0.3092 0.0564 1.0000 Uiso R . . . . . . H3141 H 0.0819 0.2762 0.4954 0.0710 0.289 Uiso R . . . . . . H3142 H -0.0699 0.2741 0.4720 0.0710 0.289 Uiso R . . . . . . H3151 H 0.0017 0.1463 0.4561 0.0553 0.289 Uiso R . . . . . . H3152 H -0.0397 0.1782 0.3633 0.0553 0.289 Uiso R . . . . . . H3161 H 0.2161 0.1739 0.4416 0.0624 0.289 Uiso R . . . . . . H3162 H 0.1588 0.1262 0.3603 0.0624 0.289 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 0.03615(8) 0.03425(8) 0.03830(8) 0.00231(6) 0.01125(6) -0.00153(6) P1 0.0383(5) 0.0320(5) 0.0419(5) 0.0027(4) 0.0109(4) 0.0015(4) P2 0.0403(5) 0.0277(4) 0.0405(5) 0.0011(4) 0.0128(4) -0.0011(4) C1 0.056(3) 0.061(3) 0.079(4) 0.014(3) 0.037(3) 0.016(2) C2 0.044(2) 0.0334(19) 0.051(2) -0.0024(17) -0.0101(18) 0.0070(16) C11 0.048(2) 0.0329(18) 0.043(2) 0.0023(16) 0.0166(17) -0.0035(16) C12 0.044(2) 0.0332(18) 0.043(2) -0.0003(16) 0.0175(17) -0.0031(16) C13 0.059(3) 0.037(2) 0.056(3) 0.0012(18) 0.026(2) 0.0010(19) C14 0.053(5) 0.059(5) 0.071(6) 0.014(5) 0.033(5) -0.001(4) C15 0.069(5) 0.049(4) 0.052(4) 0.014(3) 0.025(4) 0.001(4) C16 0.055(4) 0.045(7) 0.054(4) 0.011(5) 0.022(4) -0.008(5) C111 0.038(2) 0.0322(19) 0.051(2) -0.0011(17) 0.0118(17) 0.0033(15) C112 0.049(2) 0.045(2) 0.054(3) -0.003(2) 0.005(2) 0.0054(19) C113 0.060(3) 0.057(3) 0.062(3) -0.012(2) 0.003(2) 0.002(2) C114 0.052(3) 0.049(3) 0.084(4) -0.022(3) 0.010(3) 0.000(2) C115 0.061(3) 0.038(2) 0.076(4) -0.001(2) 0.015(3) 0.005(2) C116 0.057(3) 0.039(2) 0.055(3) 0.0039(19) 0.015(2) 0.0081(19) C121 0.050(3) 0.051(3) 0.051(3) 0.007(2) -0.003(2) -0.005(2) C122 0.090(4) 0.064(3) 0.060(3) 0.003(3) -0.016(3) -0.023(3) C123 0.046(3) 0.093(4) 0.081(4) 0.015(3) -0.002(3) 0.007(3) C211 0.0390(19) 0.0316(18) 0.045(2) -0.0025(16) 0.0122(16) -0.0002(15) C212 0.051(2) 0.0291(18) 0.057(3) -0.0018(17) 0.020(2) 0.0003(16) C213 0.040(2) 0.045(2) 0.069(3) -0.010(2) 0.009(2) -0.0050(18) C214 0.044(2) 0.051(3) 0.060(3) -0.012(2) 0.007(2) 0.004(2) C215 0.052(2) 0.041(2) 0.052(2) -0.0042(19) 0.008(2) 0.0054(19) C216 0.046(2) 0.0311(18) 0.050(2) -0.0009(17) 0.0087(18) 0.0004(16) C221 0.046(2) 0.0304(18) 0.042(2) -0.0011(15) 0.0110(17) -0.0042(16) C222 0.049(2) 0.038(2) 0.058(3) -0.0019(19) 0.011(2) -0.0052(18) C223 0.061(3) 0.045(3) 0.072(3) -0.007(2) 0.006(3) -0.019(2) C224 0.077(4) 0.036(2) 0.068(3) -0.014(2) 0.010(3) -0.009(2) C225 0.067(3) 0.038(2) 0.067(3) -0.014(2) 0.015(3) 0.003(2) C226 0.048(2) 0.038(2) 0.056(3) -0.0080(18) 0.010(2) -0.0005(17) C314 0.083(18) 0.036(8) 0.070(12) -0.003(7) 0.051(10) 0.001(9) C315 0.060(9) 0.025(6) 0.060(10) 0.008(6) 0.034(6) -0.004(6) C316 0.071(16) 0.019(11) 0.07112(10) 0.016(10) 0.044(13) 0.023(11) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.3397(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 . P1 . 2.2587(10) yes Pt1 . P2 . 2.2454(10) yes Pt1 . C1 . 2.102(5) yes Pt1 . C2 . 2.179(4) yes P1 . C11 . 1.845(4) yes P1 . C111 . 1.830(4) yes P1 . C121 . 1.853(5) yes P2 . C12 . 1.841(4) yes P2 . C211 . 1.819(4) yes P2 . C221 . 1.826(4) yes C1 . H11 . 0.948(10) no C1 . H12 . 0.947(10) no C1 . H13 . 0.942(10) no C2 . H21 . 0.937(10) no C2 . H22 . 0.930(10) no C2 . H23 . 0.933(10) no C11 . C12 . 1.328(6) yes C11 . C16 . 1.517(11) yes C11 . C316 . 1.512(18) yes C12 . C13 . 1.515(6) yes C13 . C14 . 1.511(10) yes C13 . C314 . 1.504(16) yes C13 . H131 . 0.950 no C13 . H132 . 0.950 no C13 . H133 . 0.950 no C13 . H134 . 0.950 no C14 . C15 . 1.510(13) yes C14 . H141 . 0.950 no C14 . H142 . 0.950 no C15 . C16 . 1.543(12) yes C15 . H151 . 0.950 no C15 . H152 . 0.950 no C16 . H161 . 0.950 no C16 . H162 . 0.950 no C111 . C112 . 1.379(7) yes C111 . C116 . 1.400(6) yes C112 . C113 . 1.395(7) yes C112 . H1121 . 0.950 no C113 . C114 . 1.383(8) yes C113 . H1131 . 0.950 no C114 . C115 . 1.389(8) yes C114 . H1141 . 0.950 no C115 . C116 . 1.386(7) yes C115 . H1151 . 0.950 no C116 . H1161 . 0.950 no C121 . C122 . 1.529(8) yes C121 . C123 . 1.533(8) yes C121 . H1211 . 0.950 no C122 . H1221 . 0.950 no C122 . H1222 . 0.950 no C122 . H1223 . 0.950 no C123 . H1231 . 0.950 no C123 . H1232 . 0.950 no C123 . H1233 . 0.950 no C211 . C212 . 1.385(6) yes C211 . C216 . 1.397(6) yes C212 . C213 . 1.392(7) yes C212 . H2121 . 0.950 no C213 . C214 . 1.379(7) yes C213 . H2131 . 0.950 no C214 . C215 . 1.383(7) yes C214 . H2141 . 0.950 no C215 . C216 . 1.380(6) yes C215 . H2151 . 0.950 no C216 . H2161 . 0.950 no C221 . C222 . 1.395(6) yes C221 . C226 . 1.399(6) yes C222 . C223 . 1.387(7) yes C222 . H2221 . 0.950 no C223 . C224 . 1.376(8) yes C223 . H2231 . 0.950 no C224 . C225 . 1.374(8) yes C224 . H2241 . 0.950 no C225 . C226 . 1.389(6) yes C225 . H2251 . 0.950 no C226 . H2261 . 0.950 no C314 . C315 . 1.519(16) yes C314 . H3141 . 0.950 no C314 . H3142 . 0.950 no C315 . C316 . 1.491(18) yes C315 . H3151 . 0.950 no C315 . H3152 . 0.950 no C316 . H3161 . 0.950 no C316 . H3162 . 0.950 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag P1 . Pt1 . P2 . 85.48(4) yes P1 . Pt1 . C1 . 95.61(15) yes P2 . Pt1 . C1 . 175.81(18) yes P1 . Pt1 . C2 . 175.96(11) yes P2 . Pt1 . C2 . 95.10(13) yes C1 . Pt1 . C2 . 84.09(19) yes Pt1 . P1 . C11 . 108.66(14) yes Pt1 . P1 . C111 . 118.90(15) yes C11 . P1 . C111 . 104.74(19) yes Pt1 . P1 . C121 . 115.63(16) yes C11 . P1 . C121 . 102.6(2) yes C111 . P1 . C121 . 104.6(2) yes Pt1 . P2 . C12 . 109.83(14) yes Pt1 . P2 . C211 . 114.41(13) yes C12 . P2 . C211 . 102.62(19) yes Pt1 . P2 . C221 . 119.30(14) yes C12 . P2 . C221 . 104.07(19) yes C211 . P2 . C221 . 104.90(19) yes Pt1 . C1 . H11 . 111.2(17) no Pt1 . C1 . H12 . 109.5(17) no H11 . C1 . H12 . 111(2) no Pt1 . C1 . H13 . 109.8(16) no H11 . C1 . H13 . 107(2) no H12 . C1 . H13 . 108(2) no Pt1 . C2 . H21 . 108.9(16) no Pt1 . C2 . H22 . 110.6(16) no H21 . C2 . H22 . 109(2) no Pt1 . C2 . H23 . 110.6(16) no H21 . C2 . H23 . 111(2) no H22 . C2 . H23 . 107(2) no P1 . C11 . C12 . 118.7(3) yes P1 . C11 . C16 . 117.1(5) yes C12 . C11 . C16 . 124.2(5) yes P1 . C11 . C316 . 123.3(9) yes C12 . C11 . C316 . 118.0(10) yes P2 . C12 . C11 . 117.2(3) yes P2 . C12 . C13 . 119.1(3) yes C11 . C12 . C13 . 123.6(4) yes C12 . C13 . C14 . 110.8(5) yes C12 . C13 . C314 . 113.2(11) yes C12 . C13 . H131 . 109.1 no C14 . C13 . H131 . 109.1 no C12 . C13 . H132 . 109.1 no C14 . C13 . H132 . 109.1 no H131 . C13 . H132 . 109.5 no C12 . C13 . H133 . 108.5 no C314 . C13 . H133 . 108.5 no C12 . C13 . H134 . 108.5 no C314 . C13 . H134 . 108.5 no H133 . C13 . H134 . 109.5 no C13 . C14 . C15 . 113.3(8) yes C13 . C14 . H141 . 108.5 no C15 . C14 . H141 . 108.5 no C13 . C14 . H142 . 108.5 no C15 . C14 . H142 . 108.5 no H141 . C14 . H142 . 109.5 no C14 . C15 . C16 . 111.9(9) yes C14 . C15 . H151 . 108.8 no C16 . C15 . H151 . 108.8 no C14 . C15 . H152 . 108.9 no C16 . C15 . H152 . 108.9 no C15 . C16 . C11 . 111.4(8) yes C15 . C16 . H161 . 109.0 no C11 . C16 . H161 . 109.0 no C15 . C16 . H162 . 109.0 no C11 . C16 . H162 . 109.0 no H161 . C16 . H162 . 109.5 no P1 . C111 . C112 . 118.1(3) yes P1 . C111 . C116 . 123.4(4) yes C112 . C111 . C116 . 118.5(4) yes C111 . C112 . C113 . 121.5(5) yes C111 . C112 . H1121 . 119.3 no C113 . C112 . H1121 . 119.3 no C112 . C113 . C114 . 119.9(5) yes C112 . C113 . H1131 . 120.1 no C114 . C113 . H1131 . 120.1 no C113 . C114 . C115 . 119.0(5) yes C113 . C114 . H1141 . 120.5 no C115 . C114 . H1141 . 120.5 no C114 . C115 . C116 . 121.1(5) yes C114 . C115 . H1151 . 119.5 no C116 . C115 . H1151 . 119.5 no C111 . C116 . C115 . 120.1(5) yes C111 . C116 . H1161 . 120.0 no C115 . C116 . H1161 . 120.0 no P1 . C121 . C122 . 109.1(4) yes P1 . C121 . C123 . 111.8(4) yes C122 . C121 . C123 . 111.1(5) yes P1 . C121 . H1211 . 108.2 no C122 . C121 . H1211 . 108.2 no C123 . C121 . H1211 . 108.2 no C121 . C122 . H1221 . 109.5 no C121 . C122 . H1222 . 109.5 no H1221 . C122 . H1222 . 109.5 no C121 . C122 . H1223 . 109.5 no H1221 . C122 . H1223 . 109.5 no H1222 . C122 . H1223 . 109.5 no C121 . C123 . H1231 . 109.5 no C121 . C123 . H1232 . 109.5 no H1231 . C123 . H1232 . 109.5 no C121 . C123 . H1233 . 109.5 no H1231 . C123 . H1233 . 109.5 no H1232 . C123 . H1233 . 109.5 no P2 . C211 . C212 . 119.8(3) yes P2 . C211 . C216 . 121.1(3) yes C212 . C211 . C216 . 118.7(4) yes C211 . C212 . C213 . 120.1(4) yes C211 . C212 . H2121 . 120.0 no C213 . C212 . H2121 . 120.0 no C212 . C213 . C214 . 120.8(4) yes C212 . C213 . H2131 . 119.6 no C214 . C213 . H2131 . 119.6 no C213 . C214 . C215 . 119.5(5) yes C213 . C214 . H2141 . 120.3 no C215 . C214 . H2141 . 120.3 no C214 . C215 . C216 . 120.1(4) yes C214 . C215 . H2151 . 120.0 no C216 . C215 . H2151 . 120.0 no C211 . C216 . C215 . 120.9(4) yes C211 . C216 . H2161 . 119.6 no C215 . C216 . H2161 . 119.6 no P2 . C221 . C222 . 116.9(3) yes P2 . C221 . C226 . 124.0(3) yes C222 . C221 . C226 . 119.1(4) yes C221 . C222 . C223 . 120.3(4) yes C221 . C222 . H2221 . 119.8 no C223 . C222 . H2221 . 119.8 no C222 . C223 . C224 . 119.8(5) yes C222 . C223 . H2231 . 120.1 no C224 . C223 . H2231 . 120.1 no C223 . C224 . C225 . 120.8(4) yes C223 . C224 . H2241 . 119.6 no C225 . C224 . H2241 . 119.6 no C224 . C225 . C226 . 120.2(5) yes C224 . C225 . H2251 . 119.9 no C226 . C225 . H2251 . 119.9 no C221 . C226 . C225 . 119.8(4) yes C221 . C226 . H2261 . 120.1 no C225 . C226 . H2261 . 120.1 no C13 . C314 . C315 . 108.3(13) yes C13 . C314 . H3141 . 109.8 no C315 . C314 . H3141 . 109.8 no C13 . C314 . H3142 . 109.8 no C315 . C314 . H3142 . 109.8 no H3141 . C314 . H3142 . 109.5 no C314 . C315 . C316 . 107.0(19) yes C314 . C315 . H3151 . 110.0 no C316 . C315 . H3151 . 112.9 no C314 . C315 . H3152 . 110.0 no C316 . C315 . H3152 . 107.3 no H3151 . C315 . H3152 . 109.5 no C11 . C316 . C315 . 115.8(17) yes C11 . C316 . C15 . 118.2(15) yes C11 . C316 . H3161 . 107.9 no C315 . C316 . H3161 . 107.9 no C11 . C316 . H3162 . 107.8 no C315 . C316 . H3162 . 107.8 no H3161 . C316 . H3162 . 109.5 no #===END