# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 #=============================================================================== _audit_creation_date 2012-05-16 # 1. SUBMISSION DETAILS _publ_contact_author_name 'Nicolas Mezailles' _publ_contact_author_address ;Laboratoire DCPH Ecole Polytechnique Route de Saclay F91128 Palaiseau France ; _publ_contact_author_email nicolas.mezailles@polytechnique.edu _publ_contact_author_phone 330169334402 _publ_contact_author_fax 330169334440 _publ_contact_letter ; Please consider this CIF submission for publication as a new structure paper in Chemical Communications. The figures, chemical structure diagram (scheme), Transfert of Copyright Agreement form and structure factors will be sent on receipt of your acknowledgement letter ; #=============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #=============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Room Temperature Reversible CH Activation Mediated by a Pt(0) center, and Stoichiometric Biphenyl Formation via Solvent Activation ; _publ_author_address ; a) Laboratoire Heteroelements et Coordination, Ecole Polytechnique, CNRS F-91128 Palaiseau Cedex France b) Laboratoire Mecanismes Reactionnels, Ecole Polytechnique, CNRS F-91128 Palaiseau Cedex France ; #=============================================================================== # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ; _publ_section_exptl_prep ;All structures were solved using SIR97 (Altomare et al.) and refined with SHELXL97 (Sheldrick). Figures were drawn with Platon (Spek, 1990). ; _publ_section_references ;Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993) J. Appl. Cryst. 26, 343-350. Sheldrick, G.M. SHELXL97. Program for crystal structure refinement. University of G\\"ottingen, Germany, 1997. Sluis, P. v.d., Spek, A.L. (1990). Acta Cryst. A46, 194-201. Spek, A.L. (1990). Acta Cryst. A46, C-34. Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7 ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; loop_ _publ_author_name 'Nicolas Mezailles' 'Emmanuel Nicolas' 'Xavier Le Goff' 'Stephane Bouchonnet' #=============================================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the ? in the data_? line below # by a unique identifier. #=============================================================================== # Compound 1Cl data_en233 _database_code_depnum_ccdc_archive 'CCDC 882554' #TrackingRef '- 2012_chemcomm_nicolas.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H48 Cl2 P2 Pt, 2 (C H2 CL2)' _chemical_formula_sum 'C29 H52 Cl6 P2 Pt' _chemical_formula_weight 870.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'Cm ' _symmetry_space_group_name_Hall 'C -2y' 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' _cell_length_a 8.959(1) _cell_length_b 17.604(2) _cell_length_c 11.960(1) _cell_angle_alpha 90.00 _cell_angle_beta 110.056(2) _cell_angle_gamma 90.00 _cell_volume 1771.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 1405 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.631 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 4.521 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2650 _exptl_absorpt_correction_T_max 0.5702 _exptl_absorpt_process_details 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3929 _diffrn_reflns_av_R_equivalents 0.0418 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2471 _reflns_number_gt 2470 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT' _computing_data_reduction 'DENZO & COLLECT' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material 'PLATON (Spek, 2009)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Flack parameter was refined to 0.21334. ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.057 0.500 0.479 238 100 ' ' 2 0.013 -0.000 0.479 238 100 ' ' _platon_squeeze_details ; Two highly disordered CH2Cl2 molecule was accounted for using the Platon SQUEEZE function. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0747P)^2^+6.4213P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.21(2) _refine_ls_number_reflns 2471 _refine_ls_number_parameters 149 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0384 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.1020 _refine_ls_wR_factor_gt 0.1020 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.00770(17) 1.0000 0.02603(15) 0.01603(12) Uani 1 2 d S . . Cl1 Cl -0.1854(5) 1.0928(3) 0.0211(4) 0.0252(10) Uani 1 1 d . . . P1 P 0.1774(4) 0.9045(3) 0.0286(3) 0.0162(9) Uani 1 1 d . . . C1 C 0.3780(10) 0.9277(5) 0.0372(9) 0.0215(17) Uani 1 1 d . . . H1A H 0.4442 0.9308 0.1225 0.026 Uiso 1 1 calc R . . H1B H 0.4188 0.8846 0.0030 0.026 Uiso 1 1 calc R . . C2 C 0.4057(19) 1.0000 -0.0228(13) 0.030(3) Uani 1 2 d S . . H2A H 0.3338 1.0000 -0.1068 0.036 Uiso 1 2 calc SR . . H2B H 0.5163 1.0000 -0.0226 0.036 Uiso 1 2 calc SR . . C4 C 0.2239(11) 0.8411(5) 0.1597(8) 0.0198(16) Uani 1 1 d . . . C5 C 0.2501(13) 0.8869(6) 0.2710(8) 0.028(2) Uani 1 1 d . . . H5A H 0.1486 0.9108 0.2677 0.034 Uiso 1 1 calc R . . H5B H 0.3273 0.9279 0.2752 0.034 Uiso 1 1 calc R . . C6 C 0.3120(13) 0.8379(6) 0.3821(9) 0.029(2) Uani 1 1 d . . . H6A H 0.4185 0.8182 0.3894 0.035 Uiso 1 1 calc R . . H6B H 0.3234 0.8695 0.4529 0.035 Uiso 1 1 calc R . . C7 C 0.2035(13) 0.7722(6) 0.3792(9) 0.030(2) Uani 1 1 d . . . H7A H 0.1004 0.7914 0.3809 0.036 Uiso 1 1 calc R . . H7B H 0.2514 0.7398 0.4502 0.036 Uiso 1 1 calc R . . C8 C 0.1769(12) 0.7256(5) 0.2663(9) 0.0269(19) Uani 1 1 d . . . H8A H 0.1031 0.6832 0.2635 0.032 Uiso 1 1 calc R . . H8B H 0.2792 0.7036 0.2674 0.032 Uiso 1 1 calc R . . C9 C 0.1067(12) 0.7761(5) 0.1545(9) 0.0254(18) Uani 1 1 d . . . H9A H 0.0892 0.7455 0.0817 0.030 Uiso 1 1 calc R . . H9B H 0.0032 0.7973 0.1520 0.030 Uiso 1 1 calc R . . C10 C 0.0952(12) 0.8441(5) -0.1044(8) 0.0221(17) Uani 1 1 d . . . H10 H -0.0043 0.8208 -0.0996 0.026 Uiso 1 1 calc R . . C11 C 0.2034(12) 0.7788(5) -0.1103(9) 0.0249(18) Uani 1 1 d . . . H11A H 0.2290 0.7477 -0.0372 0.030 Uiso 1 1 calc R . . H11B H 0.3041 0.7993 -0.1149 0.030 Uiso 1 1 calc R . . C12 C 0.1230(14) 0.7294(5) -0.2190(10) 0.030(2) Uani 1 1 d . . . H12A H 0.1952 0.6875 -0.2217 0.035 Uiso 1 1 calc R . . H12B H 0.0255 0.7067 -0.2119 0.035 Uiso 1 1 calc R . . C13 C 0.0800(15) 0.7745(7) -0.3328(10) 0.036(2) Uani 1 1 d . . . H13A H 0.0257 0.7411 -0.4013 0.043 Uiso 1 1 calc R . . H13B H 0.1780 0.7942 -0.3431 0.043 Uiso 1 1 calc R . . C14 C -0.0307(14) 0.8419(6) -0.3303(8) 0.029(2) Uani 1 1 d . . . H14A H -0.0511 0.8732 -0.4028 0.035 Uiso 1 1 calc R . . H14B H -0.1338 0.8221 -0.3295 0.035 Uiso 1 1 calc R . . C15 C 0.0467(13) 0.8914(5) -0.2189(8) 0.0251(18) Uani 1 1 d . . . H15A H 0.1418 0.9168 -0.2256 0.030 Uiso 1 1 calc R . . H15B H -0.0292 0.9312 -0.2148 0.030 Uiso 1 1 calc 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 0.01640(19) 0.01400(17) 0.01851(18) 0.000 0.00702(13) 0.000 Cl1 0.0245(19) 0.0169(16) 0.0340(19) 0.0000(14) 0.0096(15) 0.0023(13) P1 0.0170(17) 0.0124(16) 0.0208(17) 0.0021(12) 0.0084(13) 0.0033(12) C1 0.013(4) 0.024(4) 0.029(4) -0.006(3) 0.009(3) -0.002(3) C2 0.027(7) 0.031(7) 0.028(7) 0.000 0.005(6) 0.000 C4 0.022(4) 0.017(3) 0.019(4) 0.001(3) 0.005(3) 0.002(3) C5 0.029(5) 0.033(5) 0.016(4) -0.009(4) 0.001(3) -0.002(4) C6 0.033(5) 0.027(4) 0.023(4) -0.005(4) 0.004(4) -0.008(4) C7 0.028(5) 0.040(5) 0.017(4) 0.010(4) 0.002(4) 0.003(4) C8 0.025(5) 0.027(4) 0.030(5) 0.007(4) 0.010(4) -0.002(4) C9 0.028(5) 0.023(4) 0.022(4) 0.008(3) 0.004(4) 0.001(4) C10 0.027(4) 0.018(4) 0.018(4) -0.002(3) 0.004(3) 0.004(3) C11 0.028(5) 0.019(4) 0.026(4) -0.005(3) 0.009(4) 0.004(4) C12 0.041(6) 0.021(4) 0.031(5) -0.006(4) 0.018(4) 0.000(4) C13 0.040(6) 0.039(5) 0.026(5) -0.011(4) 0.009(4) -0.003(5) C14 0.044(6) 0.028(5) 0.011(4) -0.002(3) 0.004(4) -0.002(4) C15 0.036(5) 0.020(4) 0.019(4) 0.002(3) 0.009(4) -0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P1 2.260(6) 2_575 ? Pt1 P1 2.260(6) . ? Pt1 Cl1 2.366(6) . ? Pt1 Cl1 2.366(6) 2_575 ? P1 C1 1.811(10) . ? P1 C10 1.844(11) . ? P1 C4 1.852(10) . ? C1 C2 1.522(12) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C1 1.522(12) 2_575 ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C4 C5 1.504(12) . ? C4 C9 1.540(13) . ? C5 C6 1.520(14) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.503(15) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.527(14) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.549(12) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.520(13) . ? C10 C15 1.533(12) . ? C10 H10 1.0000 . ? C11 C12 1.524(13) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.508(15) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.553(16) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.542(12) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pt1 P1 96.1(3) 2_575 . ? P1 Pt1 Cl1 88.26(10) 2_575 . ? P1 Pt1 Cl1 175.6(2) . . ? P1 Pt1 Cl1 175.6(2) 2_575 2_575 ? P1 Pt1 Cl1 88.26(10) . 2_575 ? Cl1 Pt1 Cl1 87.4(3) . 2_575 ? C1 P1 C10 106.0(5) . . ? C1 P1 C4 99.0(5) . . ? C10 P1 C4 106.8(5) . . ? C1 P1 Pt1 118.9(4) . . ? C10 P1 Pt1 110.5(4) . . ? C4 P1 Pt1 114.5(4) . . ? C2 C1 P1 118.7(8) . . ? C2 C1 H1A 107.6 . . ? P1 C1 H1A 107.6 . . ? C2 C1 H1B 107.6 . . ? P1 C1 H1B 107.6 . . ? H1A C1 H1B 107.1 . . ? C1 C2 C1 113.4(12) . 2_575 ? C1 C2 H2A 108.9 . . ? C1 C2 H2A 108.9 2_575 . ? C1 C2 H2B 108.9 . . ? C1 C2 H2B 108.9 2_575 . ? H2A C2 H2B 107.7 . . ? C5 C4 C9 109.3(8) . . ? C5 C4 P1 110.4(6) . . ? C9 C4 P1 117.5(6) . . ? C4 C5 C6 111.7(8) . . ? C4 C5 H5A 109.3 . . ? C6 C5 H5A 109.3 . . ? C4 C5 H5B 109.3 . . ? C6 C5 H5B 109.3 . . ? H5A C5 H5B 108.0 . . ? C7 C6 C5 112.2(8) . . ? C7 C6 H6A 109.2 . . ? C5 C6 H6A 109.2 . . ? C7 C6 H6B 109.2 . . ? C5 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? C6 C7 C8 109.7(8) . . ? C6 C7 H7A 109.7 . . ? C8 C7 H7A 109.7 . . ? C6 C7 H7B 109.7 . . ? C8 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? C7 C8 C9 110.4(8) . . ? C7 C8 H8A 109.6 . . ? C9 C8 H8A 109.6 . . ? C7 C8 H8B 109.6 . . ? C9 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? C4 C9 C8 108.8(7) . . ? C4 C9 H9A 109.9 . . ? C8 C9 H9A 109.9 . . ? C4 C9 H9B 109.9 . . ? C8 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? C11 C10 C15 111.0(8) . . ? C11 C10 P1 113.8(7) . . ? C15 C10 P1 111.3(6) . . ? C11 C10 H10 106.7 . . ? C15 C10 H10 106.7 . . ? P1 C10 H10 106.7 . . ? C10 C11 C12 110.4(8) . . ? C10 C11 H11A 109.6 . . ? C12 C11 H11A 109.6 . . ? C10 C11 H11B 109.6 . . ? C12 C11 H11B 109.6 . . ? H11A C11 H11B 108.1 . . ? C13 C12 C11 111.6(8) . . ? C13 C12 H12A 109.3 . . ? C11 C12 H12A 109.3 . . ? C13 C12 H12B 109.3 . . ? C11 C12 H12B 109.3 . . ? H12A C12 H12B 108.0 . . ? C12 C13 C14 110.6(8) . . ? C12 C13 H13A 109.5 . . ? C14 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? C15 C14 C13 110.3(8) . . ? C15 C14 H14A 109.6 . . ? C13 C14 H14A 109.6 . . ? C15 C14 H14B 109.6 . . ? C13 C14 H14B 109.6 . . ? H14A C14 H14B 108.1 . . ? C10 C15 C14 111.8(7) . . ? C10 C15 H15A 109.3 . . ? C14 C15 H15A 109.3 . . ? C10 C15 H15B 109.3 . . ? C14 C15 H15B 109.3 . . ? H15A C15 H15B 107.9 . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Pt1 P1 C1 2.3(5) 2_575 . . . ? Cl1 Pt1 P1 C1 175(3) . . . . ? Cl1 Pt1 P1 C1 -178.2(4) 2_575 . . . ? P1 Pt1 P1 C10 -120.4(4) 2_575 . . . ? Cl1 Pt1 P1 C10 52(4) . . . . ? Cl1 Pt1 P1 C10 59.0(5) 2_575 . . . ? P1 Pt1 P1 C4 118.9(4) 2_575 . . . ? Cl1 Pt1 P1 C4 -68(3) . . . . ? Cl1 Pt1 P1 C4 -61.6(5) 2_575 . . . ? C10 P1 C1 C2 91.7(9) . . . . ? C4 P1 C1 C2 -157.8(8) . . . . ? Pt1 P1 C1 C2 -33.2(10) . . . . ? P1 C1 C2 C1 68.6(13) . . . 2_575 ? C1 P1 C4 C5 85.3(8) . . . . ? C10 P1 C4 C5 -164.9(7) . . . . ? Pt1 P1 C4 C5 -42.3(8) . . . . ? C1 P1 C4 C9 -148.5(7) . . . . ? C10 P1 C4 C9 -38.7(9) . . . . ? Pt1 P1 C4 C9 83.9(7) . . . . ? C9 C4 C5 C6 57.7(10) . . . . ? P1 C4 C5 C6 -171.6(7) . . . . ? C4 C5 C6 C7 -56.6(12) . . . . ? C5 C6 C7 C8 55.5(11) . . . . ? C6 C7 C8 C9 -57.7(11) . . . . ? C5 C4 C9 C8 -59.2(10) . . . . ? P1 C4 C9 C8 174.0(7) . . . . ? C7 C8 C9 C4 59.9(10) . . . . ? C1 P1 C10 C11 49.2(9) . . . . ? C4 P1 C10 C11 -55.6(8) . . . . ? Pt1 P1 C10 C11 179.2(6) . . . . ? C1 P1 C10 C15 -77.1(8) . . . . ? C4 P1 C10 C15 178.0(7) . . . . ? Pt1 P1 C10 C15 52.9(8) . . . . ? C15 C10 C11 C12 -56.5(11) . . . . ? P1 C10 C11 C12 176.9(7) . . . . ? C10 C11 C12 C13 58.7(11) . . . . ? C11 C12 C13 C14 -57.8(12) . . . . ? C12 C13 C14 C15 54.9(12) . . . . ? C11 C10 C15 C14 55.2(11) . . . . ? P1 C10 C15 C14 -176.9(7) . . . . ? C13 C14 C15 C10 -53.9(11) . . . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.804 _refine_diff_density_min -1.085 _refine_diff_density_rms 0.186 #===END # Compound 1I data_en52 _database_code_depnum_ccdc_archive 'CCDC 882555' #TrackingRef '- 2012_chemcomm_nicolas.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H50 I2 P2 Pt, 2(C H2 Cl2)' _chemical_formula_sum 'C29 H54 Cl4 I2 P2 Pt' _chemical_formula_weight 1055.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.262(1) _cell_length_b 9.278(1) _cell_length_c 17.617(1) _cell_angle_alpha 90.00 _cell_angle_beta 117.018(1) _cell_angle_gamma 90.00 _cell_volume 3678.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 4131 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description Plate _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.906 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2040 _exptl_absorpt_coefficient_mu 5.889 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4170 _exptl_absorpt_correction_T_max 0.5384 _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15410 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_sigmaI/netI 0.0365 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.27 _diffrn_reflns_theta_max 27.45 _reflns_number_total 4176 _reflns_number_gt 3500 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT' _computing_data_reduction 'DENZO & COLLECT' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material 'PLATON (Spek, 2009)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0622P)^2^+7.2716P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4176 _refine_ls_number_parameters 174 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.1069 _refine_ls_wR_factor_gt 0.1009 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.0000 0.05896(3) 0.2500 0.02950(11) Uani 1 2 d S . . I1 I -0.001396(15) -0.14901(4) 0.14318(2) 0.03681(12) Uani 1 1 d . . . P1 P 0.00029(6) 0.22135(15) 0.34669(9) 0.0314(3) Uani 1 1 d . . . C1 C 0.0092(5) 0.4121(12) 0.3263(10) 0.0300(16) Uani 0.50 1 d P A 1 H1A H -0.0051 0.4724 0.3596 0.036 Uiso 0.50 1 calc PR A 1 H1B H 0.0521 0.4322 0.3474 0.036 Uiso 0.50 1 calc PR A 1 C2 C -0.0230(4) 0.4567(11) 0.2341(7) 0.0300(16) Uani 0.50 1 d P A 1 H2A H -0.0279 0.5627 0.2303 0.036 Uiso 0.50 1 calc PR A 1 H2B H -0.0631 0.4125 0.2073 0.036 Uiso 0.50 1 calc PR A 1 C3 C 0.0120(5) 0.4084(12) 0.1869(10) 0.0300(16) Uani 0.50 1 d P . 1 H3A H 0.0549 0.4231 0.2246 0.036 Uiso 0.50 1 calc PR . 1 H3B H 0.0007 0.4702 0.1361 0.036 Uiso 0.50 1 calc PR . 1 C4 C -0.0660(2) 0.1938(6) 0.3646(4) 0.0369(12) Uani 1 1 d . A . H4 H -0.0573 0.1093 0.4037 0.044 Uiso 1 1 calc R . . C5 C -0.1206(2) 0.1537(6) 0.2806(4) 0.0421(14) Uani 1 1 d . . . H5A H -0.1303 0.2348 0.2399 0.051 Uiso 1 1 calc R A . H5B H -0.1111 0.0687 0.2551 0.051 Uiso 1 1 calc R . . C6 C -0.1745(3) 0.1200(7) 0.2948(4) 0.0466(14) Uani 1 1 d . A . H6A H -0.2091 0.0995 0.2393 0.056 Uiso 1 1 calc R . . H6B H -0.1663 0.0328 0.3308 0.056 Uiso 1 1 calc R . . C7 C -0.1892(3) 0.2435(8) 0.3373(5) 0.0548(17) Uani 1 1 d . . . H7A H -0.2227 0.2158 0.3490 0.066 Uiso 1 1 calc R A . H7B H -0.2019 0.3276 0.2985 0.066 Uiso 1 1 calc R . . C8 C -0.1357(3) 0.2852(8) 0.4206(4) 0.0530(16) Uani 1 1 d . A . H8A H -0.1257 0.2044 0.4616 0.064 Uiso 1 1 calc R . . H8B H -0.1461 0.3697 0.4455 0.064 Uiso 1 1 calc R . . C9 C -0.0812(3) 0.3217(7) 0.4071(4) 0.0461(14) Uani 1 1 d . . . H9A H -0.0469 0.3434 0.4626 0.055 Uiso 1 1 calc R A . H9B H -0.0897 0.4082 0.3705 0.055 Uiso 1 1 calc R . . C10 C 0.0681(2) 0.1987(6) 0.4498(4) 0.0368(12) Uani 1 1 d . A . H10 H 0.0628 0.1089 0.4770 0.044 Uiso 1 1 calc R . . C11 C 0.0804(3) 0.3228(6) 0.5139(4) 0.0431(13) Uani 1 1 d . . . H11A H 0.0461 0.3342 0.5263 0.052 Uiso 1 1 calc R A . H11B H 0.0855 0.4141 0.4889 0.052 Uiso 1 1 calc R . . C12 C 0.1370(3) 0.2906(7) 0.5972(4) 0.0500(15) Uani 1 1 d . A . H12A H 0.1455 0.3730 0.6368 0.060 Uiso 1 1 calc R . . H12B H 0.1302 0.2044 0.6247 0.060 Uiso 1 1 calc R . . C13 C 0.1904(3) 0.2645(7) 0.5811(4) 0.0508(16) Uani 1 1 d . . . H13A H 0.2003 0.3545 0.5601 0.061 Uiso 1 1 calc R A . H13B H 0.2251 0.2379 0.6353 0.061 Uiso 1 1 calc R . . C14 C 0.1787(3) 0.1458(7) 0.5164(4) 0.0473(15) Uani 1 1 d . A . H14A H 0.1745 0.0528 0.5406 0.057 Uiso 1 1 calc R . . H14B H 0.2131 0.1377 0.5039 0.057 Uiso 1 1 calc R . . C15 C 0.1223(2) 0.1751(7) 0.4333(4) 0.0415(13) Uani 1 1 d . . . H15A H 0.1146 0.0925 0.3942 0.050 Uiso 1 1 calc R A . H15B H 0.1285 0.2617 0.4054 0.050 Uiso 1 1 calc R . . Cl1 Cl 0.32274(11) 0.0488(2) 0.1449(2) 0.1042(10) Uani 1 1 d . . . Cl2 Cl 0.30696(12) 0.3502(3) 0.0971(2) 0.1054(9) Uani 1 1 d . . . C16 C 0.3534(4) 0.2185(10) 0.1593(7) 0.088(3) Uani 1 1 d . . . H16A H 0.3678 0.2461 0.2197 0.106 Uiso 1 1 calc R . . H16B H 0.3883 0.2143 0.1480 0.106 Uiso 1 1 calc 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 0.03692(17) 0.02159(15) 0.03087(18) 0.000 0.01618(13) 0.000 I1 0.0490(2) 0.0261(2) 0.0377(2) -0.00255(13) 0.02168(18) -0.00080(13) P1 0.0400(7) 0.0256(7) 0.0303(7) 0.0006(5) 0.0173(6) 0.0012(5) C1 0.039(4) 0.030(3) 0.025(4) -0.004(3) 0.019(4) -0.006(2) C2 0.039(4) 0.030(3) 0.025(4) -0.004(3) 0.019(4) -0.006(2) C3 0.039(4) 0.030(3) 0.025(4) -0.004(3) 0.019(4) -0.006(2) C4 0.044(3) 0.031(3) 0.036(3) 0.001(2) 0.018(2) 0.007(2) C5 0.043(3) 0.039(3) 0.038(3) 0.001(2) 0.014(3) 0.005(2) C6 0.044(3) 0.045(3) 0.047(4) 0.000(3) 0.018(3) 0.002(3) C7 0.044(3) 0.063(4) 0.060(4) 0.001(3) 0.026(3) 0.007(3) C8 0.058(4) 0.053(4) 0.055(4) -0.003(3) 0.032(3) 0.010(3) C9 0.048(3) 0.042(3) 0.050(4) -0.007(3) 0.023(3) 0.007(3) C10 0.044(3) 0.029(3) 0.036(3) 0.000(2) 0.017(2) -0.001(2) C11 0.048(3) 0.038(3) 0.038(3) -0.011(3) 0.015(3) -0.001(2) C12 0.060(4) 0.043(3) 0.039(3) -0.011(3) 0.015(3) 0.000(3) C13 0.048(3) 0.051(4) 0.042(4) -0.013(3) 0.010(3) -0.003(3) C14 0.039(3) 0.049(4) 0.045(4) -0.002(3) 0.012(3) 0.004(2) C15 0.038(3) 0.045(3) 0.039(3) -0.002(3) 0.015(3) 0.000(2) Cl1 0.0687(14) 0.0549(13) 0.169(3) -0.0004(14) 0.0368(16) 0.0013(9) Cl2 0.0978(17) 0.0717(15) 0.154(3) 0.0275(15) 0.0640(18) -0.0121(12) C16 0.068(5) 0.082(6) 0.090(7) 0.012(5) 0.014(5) -0.024(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P1 2.2715(14) 2 ? Pt1 P1 2.2716(14) . ? Pt1 I1 2.6843(4) 2 ? Pt1 I1 2.6843(4) . ? P1 C3 1.814(12) 2 ? P1 C1 1.840(12) . ? P1 C4 1.857(6) . ? P1 C10 1.858(6) . ? C1 C2 1.506(19) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.531(17) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 P1 1.814(12) 2 ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.542(8) . ? C4 C9 1.542(8) . ? C4 H4 1.0000 . ? C5 C6 1.523(9) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.505(9) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.526(10) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.537(9) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C15 1.539(8) . ? C10 C11 1.543(8) . ? C10 H10 1.0000 . ? C11 C12 1.544(8) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.520(9) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.514(9) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.533(8) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? Cl1 C16 1.722(9) . ? Cl2 C16 1.703(10) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pt1 P1 96.90(7) 2 . ? P1 Pt1 I1 175.56(4) 2 2 ? P1 Pt1 I1 87.51(4) . 2 ? P1 Pt1 I1 87.51(4) 2 . ? P1 Pt1 I1 175.56(4) . . ? I1 Pt1 I1 88.085(18) 2 . ? C3 P1 C1 15.0(5) 2 . ? C3 P1 C4 98.9(4) 2 . ? C1 P1 C4 111.5(4) . . ? C3 P1 C10 111.8(5) 2 . ? C1 P1 C10 99.2(5) . . ? C4 P1 C10 108.7(3) . . ? C3 P1 Pt1 116.6(5) 2 . ? C1 P1 Pt1 116.8(5) . . ? C4 P1 Pt1 109.87(18) . . ? C10 P1 Pt1 110.20(18) . . ? C2 C1 P1 114.9(8) . . ? C2 C1 H1A 108.6 . . ? P1 C1 H1A 108.6 . . ? C2 C1 H1B 108.6 . . ? P1 C1 H1B 108.6 . . ? H1A C1 H1B 107.5 . . ? C1 C2 C3 110.0(8) . . ? C1 C2 H2A 109.7 . . ? C3 C2 H2A 109.7 . . ? C1 C2 H2B 109.7 . . ? C3 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C2 C3 P1 113.7(8) . 2 ? C2 C3 H3A 108.8 . . ? P1 C3 H3A 108.8 2 . ? C2 C3 H3B 108.8 . . ? P1 C3 H3B 108.8 2 . ? H3A C3 H3B 107.7 . . ? C5 C4 C9 109.8(5) . . ? C5 C4 P1 110.7(4) . . ? C9 C4 P1 114.8(4) . . ? C5 C4 H4 107.0 . . ? C9 C4 H4 107.0 . . ? P1 C4 H4 107.0 . . ? C6 C5 C4 111.6(5) . . ? C6 C5 H5A 109.3 . . ? C4 C5 H5A 109.3 . . ? C6 C5 H5B 109.3 . . ? C4 C5 H5B 109.3 . . ? H5A C5 H5B 108.0 . . ? C7 C6 C5 111.5(5) . . ? C7 C6 H6A 109.3 . . ? C5 C6 H6A 109.3 . . ? C7 C6 H6B 109.3 . . ? C5 C6 H6B 109.3 . . ? H6A C6 H6B 108.0 . . ? C6 C7 C8 111.1(5) . . ? C6 C7 H7A 109.4 . . ? C8 C7 H7A 109.4 . . ? C6 C7 H7B 109.4 . . ? C8 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? C7 C8 C9 111.7(6) . . ? C7 C8 H8A 109.3 . . ? C9 C8 H8A 109.3 . . ? C7 C8 H8B 109.3 . . ? C9 C8 H8B 109.3 . . ? H8A C8 H8B 107.9 . . ? C8 C9 C4 110.2(5) . . ? C8 C9 H9A 109.6 . . ? C4 C9 H9A 109.6 . . ? C8 C9 H9B 109.6 . . ? C4 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? C15 C10 C11 110.1(5) . . ? C15 C10 P1 109.7(4) . . ? C11 C10 P1 114.9(4) . . ? C15 C10 H10 107.3 . . ? C11 C10 H10 107.3 . . ? P1 C10 H10 107.3 . . ? C10 C11 C12 110.0(5) . . ? C10 C11 H11A 109.7 . . ? C12 C11 H11A 109.7 . . ? C10 C11 H11B 109.7 . . ? C12 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? C13 C12 C11 111.8(5) . . ? C13 C12 H12A 109.3 . . ? C11 C12 H12A 109.3 . . ? C13 C12 H12B 109.3 . . ? C11 C12 H12B 109.3 . . ? H12A C12 H12B 107.9 . . ? C14 C13 C12 111.8(5) . . ? C14 C13 H13A 109.3 . . ? C12 C13 H13A 109.3 . . ? C14 C13 H13B 109.3 . . ? C12 C13 H13B 109.3 . . ? H13A C13 H13B 107.9 . . ? C13 C14 C15 111.6(5) . . ? C13 C14 H14A 109.3 . . ? C15 C14 H14A 109.3 . . ? C13 C14 H14B 109.3 . . ? C15 C14 H14B 109.3 . . ? H14A C14 H14B 108.0 . . ? C14 C15 C10 111.5(5) . . ? C14 C15 H15A 109.3 . . ? C10 C15 H15A 109.3 . . ? C14 C15 H15B 109.3 . . ? C10 C15 H15B 109.3 . . ? H15A C15 H15B 108.0 . . ? Cl2 C16 Cl1 115.4(5) . . ? Cl2 C16 H16A 108.4 . . ? Cl1 C16 H16A 108.4 . . ? Cl2 C16 H16B 108.4 . . ? Cl1 C16 H16B 108.4 . . ? H16A C16 H16B 107.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.268 _refine_diff_density_min -1.643 _refine_diff_density_rms 0.179 #===END # Compound 3H data_en201 _database_code_depnum_ccdc_archive 'CCDC 882556' #TrackingRef '- 2012_chemcomm_nicolas.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H58 P2 Pt, C7 H8' _chemical_formula_sum 'C41 H66 P2 Pt' _chemical_formula_weight 815.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P21/c ' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.772(1) _cell_length_b 13.486(1) _cell_length_c 25.007(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.899(2) _cell_angle_gamma 90.00 _cell_volume 3837(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 7629 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description Plate _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.413 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1680 _exptl_absorpt_coefficient_mu 3.767 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3141 _exptl_absorpt_correction_T_max 0.8639 _exptl_absorpt_process_details 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26816 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8715 _reflns_number_gt 7889 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT' _computing_data_reduction 'DENZO & COLLECT' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material 'PLATON (Spek, 2009)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0086P)^2^+10.6738P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8715 _refine_ls_number_parameters 403 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0319 _refine_ls_R_factor_gt 0.0271 _refine_ls_wR_factor_ref 0.0605 _refine_ls_wR_factor_gt 0.0573 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.485412(10) 0.295034(8) 0.315781(4) 0.01878(4) Uani 1 1 d . . . P1 P 0.58555(7) 0.19848(6) 0.38874(3) 0.01849(15) Uani 1 1 d . . . P2 P 0.52559(6) 0.20540(5) 0.24608(3) 0.01721(14) Uani 1 1 d . . . C3 C 0.6570(3) 0.0870(2) 0.36985(12) 0.0247(6) Uani 1 1 d . . . H35A H 0.7371 0.1055 0.3677 0.030 Uiso 1 1 calc R . . H35B H 0.6656 0.0380 0.4001 0.030 Uiso 1 1 calc R . . C4 C 0.5941(3) 0.0365(2) 0.31546(12) 0.0237(6) Uani 1 1 d . . . H36A H 0.5092 0.0322 0.3135 0.028 Uiso 1 1 calc R . . H36B H 0.6243 -0.0321 0.3156 0.028 Uiso 1 1 calc R . . C5 C 0.6094(3) 0.0898(2) 0.26363(12) 0.0240(6) Uani 1 1 d . . . H37A H 0.5857 0.0439 0.2318 0.029 Uiso 1 1 calc R . . H37B H 0.6938 0.1050 0.2689 0.029 Uiso 1 1 calc R . . C12 C 0.7090(3) 0.2642(2) 0.43586(12) 0.0231(6) Uani 1 1 d . . . H16 H 0.6733 0.3170 0.4545 0.028 Uiso 1 1 calc R . . C17 C 0.7838(3) 0.3178(3) 0.40286(13) 0.0291(7) Uani 1 1 d . . . H39A H 0.8225 0.2684 0.3842 0.035 Uiso 1 1 calc R . . H39B H 0.7326 0.3598 0.3741 0.035 Uiso 1 1 calc R . . C16 C 0.8773(3) 0.3824(3) 0.44097(15) 0.0374(8) Uani 1 1 d . . . H40A H 0.9258 0.4150 0.4190 0.045 Uiso 1 1 calc R . . H40B H 0.8385 0.4348 0.4576 0.045 Uiso 1 1 calc R . . C15 C 0.9562(3) 0.3207(3) 0.48675(15) 0.0394(9) Uani 1 1 d . . . H41A H 1.0135 0.3645 0.5118 0.047 Uiso 1 1 calc R . . H41B H 1.0006 0.2723 0.4703 0.047 Uiso 1 1 calc R . . C14 C 0.8836(3) 0.2654(3) 0.51990(13) 0.0323(8) Uani 1 1 d . . . H42A H 0.8468 0.3140 0.5400 0.039 Uiso 1 1 calc R . . H42B H 0.9361 0.2224 0.5476 0.039 Uiso 1 1 calc R . . C13 C 0.7874(3) 0.2018(2) 0.48220(13) 0.0265(7) Uani 1 1 d . . . H43A H 0.8244 0.1479 0.4657 0.032 Uiso 1 1 calc R . . H43B H 0.7385 0.1710 0.5045 0.032 Uiso 1 1 calc R . . C6 C 0.5003(3) 0.1472(2) 0.43545(12) 0.0230(6) Uani 1 1 d . . . H44 H 0.5485 0.0931 0.4576 0.028 Uiso 1 1 calc R . . C11 C 0.4746(3) 0.2230(3) 0.47653(13) 0.0276(7) Uani 1 1 d . . . H45A H 0.5497 0.2485 0.5001 0.033 Uiso 1 1 calc R . . H45B H 0.4308 0.2797 0.4559 0.033 Uiso 1 1 calc R . . C10 C 0.4027(3) 0.1773(3) 0.51317(14) 0.0337(8) Uani 1 1 d . . . H46A H 0.4501 0.1255 0.5369 0.040 Uiso 1 1 calc R . . H46B H 0.3840 0.2291 0.5376 0.040 Uiso 1 1 calc R . . C9 C 0.2889(3) 0.1315(3) 0.47880(15) 0.0374(8) Uani 1 1 d . . . H47A H 0.2471 0.0989 0.5037 0.045 Uiso 1 1 calc R . . H47B H 0.2374 0.1845 0.4583 0.045 Uiso 1 1 calc R . . C8 C 0.3132(3) 0.0559(3) 0.43810(15) 0.0343(8) Uani 1 1 d . . . H48A H 0.2376 0.0311 0.4146 0.041 Uiso 1 1 calc R . . H48B H 0.3560 -0.0012 0.4588 0.041 Uiso 1 1 calc R . . C7 C 0.3858(3) 0.1002(3) 0.40131(13) 0.0286(7) Uani 1 1 d . . . H49A H 0.3385 0.1512 0.3769 0.034 Uiso 1 1 calc R . . H49B H 0.4049 0.0474 0.3775 0.034 Uiso 1 1 calc R . . C24 C 0.3931(3) 0.1634(2) 0.19336(12) 0.0219(6) Uani 1 1 d . . . H50 H 0.4194 0.1173 0.1676 0.026 Uiso 1 1 calc R . . C25 C 0.3108(3) 0.1051(3) 0.22081(13) 0.0283(7) Uani 1 1 d . . . H51A H 0.3535 0.0472 0.2407 0.034 Uiso 1 1 calc R . . H51B H 0.2873 0.1480 0.2483 0.034 Uiso 1 1 calc R . . C26 C 0.2008(3) 0.0692(3) 0.17819(15) 0.0330(8) Uani 1 1 d . . . H52A H 0.2237 0.0203 0.1533 0.040 Uiso 1 1 calc R . . H52B H 0.1480 0.0356 0.1975 0.040 Uiso 1 1 calc R . . C27 C 0.1354(3) 0.1546(3) 0.14397(15) 0.0345(8) Uani 1 1 d . . . H53A H 0.0653 0.1300 0.1172 0.041 Uiso 1 1 d R . . H53B H 0.1019 0.2022 0.1681 0.041 Uiso 1 1 d R . . C28 C 0.2167(3) 0.2107(3) 0.11571(14) 0.0341(8) Uani 1 1 d . . . H54A H 0.1738 0.2674 0.0946 0.041 Uiso 1 1 calc R . . H54B H 0.2414 0.1662 0.0893 0.041 Uiso 1 1 calc R . . C29 C 0.3258(3) 0.2489(3) 0.15875(13) 0.0268(7) Uani 1 1 d . . . H55A H 0.3782 0.2836 0.1396 0.032 Uiso 1 1 calc R . . H55B H 0.3013 0.2971 0.1835 0.032 Uiso 1 1 calc R . . C18 C 0.6099(3) 0.2762(2) 0.20599(12) 0.0209(6) Uani 1 1 d . . . H56 H 0.5609 0.3350 0.1903 0.025 Uiso 1 1 calc R . . C23 C 0.6332(3) 0.2189(2) 0.15667(12) 0.0260(7) Uani 1 1 d . . . H57A H 0.6795 0.1586 0.1703 0.031 Uiso 1 1 calc R . . H57B H 0.5574 0.1979 0.1317 0.031 Uiso 1 1 calc R . . C22 C 0.7000(3) 0.2828(3) 0.12472(14) 0.0312(7) Uani 1 1 d . . . H58A H 0.7167 0.2432 0.0943 0.037 Uiso 1 1 calc R . . H58B H 0.6501 0.3396 0.1080 0.037 Uiso 1 1 calc R . . C21 C 0.8149(3) 0.3215(3) 0.16161(15) 0.0345(8) Uani 1 1 d . . . H59A H 0.8531 0.3658 0.1399 0.041 Uiso 1 1 calc R . . H59B H 0.8685 0.2651 0.1751 0.041 Uiso 1 1 calc R . . C20 C 0.7931(3) 0.3782(3) 0.21095(14) 0.0318(7) Uani 1 1 d . . . H60A H 0.8696 0.3979 0.2359 0.038 Uiso 1 1 calc R . . H60B H 0.7485 0.4395 0.1975 0.038 Uiso 1 1 calc R . . C19 C 0.7248(3) 0.3167(2) 0.24349(13) 0.0254(6) Uani 1 1 d . . . H61A H 0.7066 0.3584 0.2728 0.030 Uiso 1 1 calc R . . H61B H 0.7743 0.2607 0.2616 0.030 Uiso 1 1 calc R . . C30 C 0.4312(3) 0.3945(2) 0.36684(12) 0.0276(7) Uani 1 1 d . . . C35 C 0.3149(3) 0.3950(3) 0.37055(14) 0.0357(8) Uani 1 1 d . . . H63 H 0.2607 0.3503 0.3481 0.043 Uiso 1 1 calc R . . C34 C 0.2746(4) 0.4589(3) 0.40625(16) 0.0417(9) Uani 1 1 d . . . C33 C 0.3527(4) 0.5254(3) 0.43772(15) 0.0421(9) Uani 1 1 d . . . H65 H 0.3272 0.5690 0.4621 0.051 Uiso 1 1 calc R . . C32 C 0.4672(4) 0.5294(3) 0.43425(14) 0.0376(8) Uani 1 1 d . . . H66 H 0.5200 0.5763 0.4557 0.045 Uiso 1 1 calc R . . C31 C 0.5058(3) 0.4651(2) 0.39949(13) 0.0300(7) Uani 1 1 d . . . H67 H 0.5853 0.4688 0.3977 0.036 Uiso 1 1 calc R . . C999 C 0.1510(5) 0.4512(5) 0.4098(2) 0.0747(16) Uani 1 1 d . . . H68A H 0.1497 0.4395 0.4483 0.112 Uiso 1 1 calc R . . H68B H 0.1122 0.3960 0.3867 0.112 Uiso 1 1 calc R . . H68C H 0.1095 0.5131 0.3967 0.112 Uiso 1 1 calc R . . C38 C 0.0327(4) 0.5293(4) 0.1384(2) 0.0588(13) Uani 1 1 d . . . C43 C -0.0116(5) 0.6108(5) 0.1574(4) 0.087(2) Uani 1 1 d . . . H70 H -0.0548 0.6574 0.1316 0.105 Uiso 1 1 calc R . . C42 C 0.0039(7) 0.6272(8) 0.2114(4) 0.114(3) Uani 1 1 d . . . H71 H -0.0291 0.6846 0.2236 0.137 Uiso 1 1 calc R . . C41 C 0.0676(7) 0.5611(8) 0.2494(3) 0.108(3) Uani 1 1 d . . . H72 H 0.0795 0.5729 0.2879 0.130 Uiso 1 1 calc R . . C40 C 0.1163(6) 0.4736(7) 0.2304(3) 0.102(3) Uani 1 1 d . . . H73 H 0.1601 0.4265 0.2558 0.123 Uiso 1 1 calc R . . C39 C 0.0968(4) 0.4611(4) 0.1741(3) 0.0697(16) Uani 1 1 d . . . H74 H 0.1280 0.4048 0.1600 0.084 Uiso 1 1 calc R . . C37 C 0.0123(5) 0.5095(5) 0.0772(3) 0.0814(17) Uani 1 1 d . . . H75A H 0.0818 0.4773 0.0703 0.122 Uiso 1 1 calc R . . H75B H -0.0022 0.5724 0.0569 0.122 Uiso 1 1 calc R . . H75C H -0.0561 0.4661 0.0647 0.122 Uiso 1 1 calc R . . H H 0.417(3) 0.364(2) 0.2685(13) 0.019(8) Uiso 1 1 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 Pt1 0.02393(6) 0.01711(6) 0.01487(6) -0.00030(4) 0.00419(4) 0.00306(4) P1 0.0207(4) 0.0190(4) 0.0149(3) 0.0004(3) 0.0029(3) 0.0019(3) P2 0.0206(4) 0.0159(3) 0.0153(3) -0.0011(3) 0.0049(3) -0.0002(3) C3 0.0285(16) 0.0232(15) 0.0208(14) 0.0031(12) 0.0031(12) 0.0055(13) C4 0.0300(16) 0.0169(14) 0.0241(15) -0.0008(12) 0.0067(13) 0.0016(12) C5 0.0289(16) 0.0214(15) 0.0224(14) -0.0016(12) 0.0080(12) 0.0040(12) C12 0.0255(15) 0.0248(15) 0.0185(14) -0.0024(12) 0.0045(12) -0.0013(12) C17 0.0280(17) 0.0367(19) 0.0220(15) 0.0047(14) 0.0051(13) -0.0036(14) C16 0.0325(18) 0.044(2) 0.0320(18) 0.0039(16) 0.0018(15) -0.0110(17) C15 0.0274(18) 0.057(2) 0.0294(18) 0.0037(17) -0.0013(14) -0.0118(17) C14 0.0292(17) 0.040(2) 0.0229(16) 0.0035(15) -0.0011(13) -0.0023(15) C13 0.0268(16) 0.0294(17) 0.0214(15) 0.0035(13) 0.0026(12) -0.0013(13) C6 0.0240(15) 0.0231(15) 0.0209(14) 0.0016(12) 0.0043(12) -0.0008(12) C11 0.0317(17) 0.0314(17) 0.0199(14) -0.0012(13) 0.0070(13) -0.0028(14) C10 0.0360(19) 0.045(2) 0.0221(15) -0.0002(15) 0.0109(14) -0.0019(16) C9 0.0286(18) 0.052(2) 0.0351(18) -0.0023(17) 0.0140(15) -0.0025(16) C8 0.0285(17) 0.043(2) 0.0328(18) -0.0034(16) 0.0108(14) -0.0087(15) C7 0.0280(17) 0.0347(18) 0.0232(15) -0.0016(14) 0.0069(13) -0.0053(14) C24 0.0228(15) 0.0234(15) 0.0181(13) -0.0022(12) 0.0029(11) -0.0031(12) C25 0.0279(16) 0.0288(17) 0.0263(16) 0.0040(13) 0.0035(13) -0.0072(14) C26 0.0262(17) 0.0329(18) 0.0365(18) 0.0020(15) 0.0018(14) -0.0082(14) C27 0.0253(17) 0.039(2) 0.0338(18) 0.0039(16) -0.0021(14) -0.0071(15) C28 0.0327(18) 0.037(2) 0.0256(16) 0.0030(14) -0.0050(14) -0.0059(15) C29 0.0271(16) 0.0289(17) 0.0214(15) 0.0034(13) 0.0006(12) -0.0029(13) C18 0.0222(15) 0.0219(15) 0.0188(14) 0.0006(11) 0.0054(11) -0.0004(12) C23 0.0283(16) 0.0309(17) 0.0200(14) -0.0038(13) 0.0087(12) -0.0044(13) C22 0.0356(18) 0.0369(19) 0.0256(16) -0.0015(14) 0.0158(14) -0.0053(15) C21 0.0326(18) 0.041(2) 0.0351(18) 0.0001(16) 0.0175(15) -0.0075(15) C20 0.0285(17) 0.0346(18) 0.0338(17) -0.0039(15) 0.0109(14) -0.0109(15) C19 0.0278(16) 0.0261(16) 0.0224(15) -0.0037(13) 0.0067(12) -0.0064(13) C30 0.0398(19) 0.0235(16) 0.0204(14) 0.0034(13) 0.0095(13) 0.0100(14) C35 0.042(2) 0.036(2) 0.0297(17) 0.0009(15) 0.0103(15) 0.0059(16) C34 0.048(2) 0.041(2) 0.042(2) 0.0087(18) 0.0237(18) 0.0159(18) C33 0.067(3) 0.036(2) 0.0286(18) 0.0022(16) 0.0213(18) 0.0144(19) C32 0.058(2) 0.0273(18) 0.0271(17) -0.0030(14) 0.0109(17) 0.0056(17) C31 0.044(2) 0.0218(16) 0.0241(16) 0.0036(13) 0.0094(14) 0.0047(14) C999 0.069(4) 0.084(4) 0.084(4) -0.004(3) 0.042(3) 0.020(3) C38 0.034(2) 0.069(3) 0.073(3) 0.004(3) 0.011(2) -0.019(2) C43 0.044(3) 0.061(4) 0.154(7) -0.003(4) 0.018(4) -0.009(3) C42 0.076(5) 0.159(8) 0.110(6) -0.061(6) 0.028(5) -0.068(5) C41 0.076(5) 0.182(9) 0.071(4) -0.029(5) 0.025(4) -0.090(6) C40 0.056(4) 0.135(7) 0.104(6) 0.043(5) -0.003(4) -0.049(4) C39 0.033(2) 0.061(3) 0.110(5) 0.014(3) 0.009(3) -0.013(2) C37 0.061(3) 0.086(4) 0.101(5) -0.001(4) 0.028(3) -0.014(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C30 2.063(3) . ? Pt1 P2 2.2687(8) . ? Pt1 P1 2.3039(9) . ? Pt1 H 1.56(3) . ? P1 C3 1.843(3) . ? P1 C12 1.846(3) . ? P1 C6 1.858(3) . ? P2 C5 1.836(3) . ? P2 C18 1.848(3) . ? P2 C24 1.853(3) . ? C3 C4 1.531(4) . ? C3 H35A 0.9900 . ? C3 H35B 0.9900 . ? C4 C5 1.533(4) . ? C4 H36A 0.9900 . ? C4 H36B 0.9900 . ? C5 H37A 0.9900 . ? C5 H37B 0.9900 . ? C12 C17 1.534(4) . ? C12 C13 1.534(4) . ? C12 H16 1.0000 . ? C17 C16 1.529(5) . ? C17 H39A 0.9900 . ? C17 H39B 0.9900 . ? C16 C15 1.522(5) . ? C16 H40A 0.9900 . ? C16 H40B 0.9900 . ? C15 C14 1.528(5) . ? C15 H41A 0.9900 . ? C15 H41B 0.9900 . ? C14 C13 1.536(5) . ? C14 H42A 0.9900 . ? C14 H42B 0.9900 . ? C13 H43A 0.9900 . ? C13 H43B 0.9900 . ? C6 C11 1.533(4) . ? C6 C7 1.535(4) . ? C6 H44 1.0000 . ? C11 C10 1.528(4) . ? C11 H45A 0.9900 . ? C11 H45B 0.9900 . ? C10 C9 1.524(5) . ? C10 H46A 0.9900 . ? C10 H46B 0.9900 . ? C9 C8 1.519(5) . ? C9 H47A 0.9900 . ? C9 H47B 0.9900 . ? C8 C7 1.529(4) . ? C8 H48A 0.9900 . ? C8 H48B 0.9900 . ? C7 H49A 0.9900 . ? C7 H49B 0.9900 . ? C24 C29 1.534(4) . ? C24 C25 1.540(4) . ? C24 H50 1.0000 . ? C25 C26 1.529(4) . ? C25 H51A 0.9900 . ? C25 H51B 0.9900 . ? C26 C27 1.521(5) . ? C26 H52A 0.9900 . ? C26 H52B 0.9900 . ? C27 C28 1.528(5) . ? C27 H53A 0.9769 . ? C27 H53B 1.0269 . ? C28 C29 1.537(4) . ? C28 H54A 0.9900 . ? C28 H54B 0.9900 . ? C29 H55A 0.9900 . ? C29 H55B 0.9900 . ? C18 C19 1.535(4) . ? C18 C23 1.538(4) . ? C18 H56 1.0000 . ? C23 C22 1.524(4) . ? C23 H57A 0.9900 . ? C23 H57B 0.9900 . ? C22 C21 1.520(5) . ? C22 H58A 0.9900 . ? C22 H58B 0.9900 . ? C21 C20 1.529(5) . ? C21 H59A 0.9900 . ? C21 H59B 0.9900 . ? C20 C19 1.527(4) . ? C20 H60A 0.9900 . ? C20 H60B 0.9900 . ? C19 H61A 0.9900 . ? C19 H61B 0.9900 . ? C30 C35 1.396(5) . ? C30 C31 1.405(5) . ? C35 C34 1.408(5) . ? C35 H63 0.9500 . ? C34 C33 1.378(6) . ? C34 C999 1.483(6) . ? C33 C32 1.374(6) . ? C33 H65 0.9500 . ? C32 C31 1.384(5) . ? C32 H66 0.9500 . ? C31 H67 0.9500 . ? C999 H68A 0.9800 . ? C999 H68B 0.9800 . ? C999 H68C 0.9800 . ? C38 C43 1.354(8) . ? C38 C39 1.365(7) . ? C38 C37 1.510(8) . ? C43 C42 1.334(10) . ? C43 H70 0.9500 . ? C42 C41 1.377(12) . ? C42 H71 0.9500 . ? C41 C40 1.443(11) . ? C41 H72 0.9500 . ? C40 C39 1.379(9) . ? C40 H73 0.9500 . ? C39 H74 0.9500 . ? C37 H75A 0.9800 . ? C37 H75B 0.9800 . ? C37 H75C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C30 Pt1 P2 168.73(9) . . ? C30 Pt1 P1 93.11(9) . . ? P2 Pt1 P1 98.16(3) . . ? C30 Pt1 H 84.3(12) . . ? P2 Pt1 H 84.4(12) . . ? P1 Pt1 H 177.4(12) . . ? C3 P1 C12 102.68(15) . . ? C3 P1 C6 102.33(15) . . ? C12 P1 C6 103.96(14) . . ? C3 P1 Pt1 115.62(10) . . ? C12 P1 Pt1 113.11(11) . . ? C6 P1 Pt1 117.32(10) . . ? C5 P2 C18 103.75(14) . . ? C5 P2 C24 102.29(15) . . ? C18 P2 C24 104.08(14) . . ? C5 P2 Pt1 118.28(10) . . ? C18 P2 Pt1 112.87(10) . . ? C24 P2 Pt1 113.94(10) . . ? C4 C3 P1 116.3(2) . . ? C4 C3 H35A 108.2 . . ? P1 C3 H35A 108.2 . . ? C4 C3 H35B 108.2 . . ? P1 C3 H35B 108.2 . . ? H35A C3 H35B 107.4 . . ? C3 C4 C5 114.0(3) . . ? C3 C4 H36A 108.7 . . ? C5 C4 H36A 108.7 . . ? C3 C4 H36B 108.7 . . ? C5 C4 H36B 108.7 . . ? H36A C4 H36B 107.6 . . ? C4 C5 P2 115.4(2) . . ? C4 C5 H37A 108.4 . . ? P2 C5 H37A 108.4 . . ? C4 C5 H37B 108.4 . . ? P2 C5 H37B 108.4 . . ? H37A C5 H37B 107.5 . . ? C17 C12 C13 110.4(3) . . ? C17 C12 P1 110.5(2) . . ? C13 C12 P1 116.1(2) . . ? C17 C12 H16 106.4 . . ? C13 C12 H16 106.4 . . ? P1 C12 H16 106.4 . . ? C16 C17 C12 110.7(3) . . ? C16 C17 H39A 109.5 . . ? C12 C17 H39A 109.5 . . ? C16 C17 H39B 109.5 . . ? C12 C17 H39B 109.5 . . ? H39A C17 H39B 108.1 . . ? C15 C16 C17 111.0(3) . . ? C15 C16 H40A 109.4 . . ? C17 C16 H40A 109.4 . . ? C15 C16 H40B 109.4 . . ? C17 C16 H40B 109.4 . . ? H40A C16 H40B 108.0 . . ? C16 C15 C14 110.9(3) . . ? C16 C15 H41A 109.5 . . ? C14 C15 H41A 109.5 . . ? C16 C15 H41B 109.5 . . ? C14 C15 H41B 109.5 . . ? H41A C15 H41B 108.0 . . ? C15 C14 C13 111.5(3) . . ? C15 C14 H42A 109.3 . . ? C13 C14 H42A 109.3 . . ? C15 C14 H42B 109.3 . . ? C13 C14 H42B 109.3 . . ? H42A C14 H42B 108.0 . . ? C12 C13 C14 111.2(3) . . ? C12 C13 H43A 109.4 . . ? C14 C13 H43A 109.4 . . ? C12 C13 H43B 109.4 . . ? C14 C13 H43B 109.4 . . ? H43A C13 H43B 108.0 . . ? C11 C6 C7 110.6(3) . . ? C11 C6 P1 113.9(2) . . ? C7 C6 P1 110.1(2) . . ? C11 C6 H44 107.3 . . ? C7 C6 H44 107.3 . . ? P1 C6 H44 107.3 . . ? C10 C11 C6 111.6(3) . . ? C10 C11 H45A 109.3 . . ? C6 C11 H45A 109.3 . . ? C10 C11 H45B 109.3 . . ? C6 C11 H45B 109.3 . . ? H45A C11 H45B 108.0 . . ? C9 C10 C11 111.6(3) . . ? C9 C10 H46A 109.3 . . ? C11 C10 H46A 109.3 . . ? C9 C10 H46B 109.3 . . ? C11 C10 H46B 109.3 . . ? H46A C10 H46B 108.0 . . ? C8 C9 C10 111.1(3) . . ? C8 C9 H47A 109.4 . . ? C10 C9 H47A 109.4 . . ? C8 C9 H47B 109.4 . . ? C10 C9 H47B 109.4 . . ? H47A C9 H47B 108.0 . . ? C9 C8 C7 111.8(3) . . ? C9 C8 H48A 109.3 . . ? C7 C8 H48A 109.3 . . ? C9 C8 H48B 109.3 . . ? C7 C8 H48B 109.3 . . ? H48A C8 H48B 107.9 . . ? C8 C7 C6 111.9(3) . . ? C8 C7 H49A 109.2 . . ? C6 C7 H49A 109.2 . . ? C8 C7 H49B 109.2 . . ? C6 C7 H49B 109.2 . . ? H49A C7 H49B 107.9 . . ? C29 C24 C25 110.0(3) . . ? C29 C24 P2 112.9(2) . . ? C25 C24 P2 110.5(2) . . ? C29 C24 H50 107.7 . . ? C25 C24 H50 107.7 . . ? P2 C24 H50 107.7 . . ? C26 C25 C24 111.6(3) . . ? C26 C25 H51A 109.3 . . ? C24 C25 H51A 109.3 . . ? C26 C25 H51B 109.3 . . ? C24 C25 H51B 109.3 . . ? H51A C25 H51B 108.0 . . ? C27 C26 C25 111.6(3) . . ? C27 C26 H52A 109.3 . . ? C25 C26 H52A 109.3 . . ? C27 C26 H52B 109.3 . . ? C25 C26 H52B 109.3 . . ? H52A C26 H52B 108.0 . . ? C26 C27 C28 110.4(3) . . ? C26 C27 H53A 110.2 . . ? C28 C27 H53A 111.7 . . ? C26 C27 H53B 111.0 . . ? C28 C27 H53B 110.1 . . ? H53A C27 H53B 103.3 . . ? C27 C28 C29 110.6(3) . . ? C27 C28 H54A 109.5 . . ? C29 C28 H54A 109.5 . . ? C27 C28 H54B 109.5 . . ? C29 C28 H54B 109.5 . . ? H54A C28 H54B 108.1 . . ? C24 C29 C28 111.1(3) . . ? C24 C29 H55A 109.4 . . ? C28 C29 H55A 109.4 . . ? C24 C29 H55B 109.4 . . ? C28 C29 H55B 109.4 . . ? H55A C29 H55B 108.0 . . ? C19 C18 C23 111.0(3) . . ? C19 C18 P2 111.4(2) . . ? C23 C18 P2 114.0(2) . . ? C19 C18 H56 106.7 . . ? C23 C18 H56 106.7 . . ? P2 C18 H56 106.7 . . ? C22 C23 C18 111.0(3) . . ? C22 C23 H57A 109.4 . . ? C18 C23 H57A 109.4 . . ? C22 C23 H57B 109.4 . . ? C18 C23 H57B 109.4 . . ? H57A C23 H57B 108.0 . . ? C21 C22 C23 112.0(3) . . ? C21 C22 H58A 109.2 . . ? C23 C22 H58A 109.2 . . ? C21 C22 H58B 109.2 . . ? C23 C22 H58B 109.2 . . ? H58A C22 H58B 107.9 . . ? C22 C21 C20 110.7(3) . . ? C22 C21 H59A 109.5 . . ? C20 C21 H59A 109.5 . . ? C22 C21 H59B 109.5 . . ? C20 C21 H59B 109.5 . . ? H59A C21 H59B 108.1 . . ? C19 C20 C21 112.3(3) . . ? C19 C20 H60A 109.1 . . ? C21 C20 H60A 109.1 . . ? C19 C20 H60B 109.1 . . ? C21 C20 H60B 109.1 . . ? H60A C20 H60B 107.9 . . ? C20 C19 C18 111.7(3) . . ? C20 C19 H61A 109.3 . . ? C18 C19 H61A 109.3 . . ? C20 C19 H61B 109.3 . . ? C18 C19 H61B 109.3 . . ? H61A C19 H61B 107.9 . . ? C35 C30 C31 115.8(3) . . ? C35 C30 Pt1 120.6(3) . . ? C31 C30 Pt1 123.6(3) . . ? C30 C35 C34 122.8(4) . . ? C30 C35 H63 118.6 . . ? C34 C35 H63 118.6 . . ? C33 C34 C35 118.4(4) . . ? C33 C34 C999 122.2(4) . . ? C35 C34 C999 119.4(4) . . ? C32 C33 C34 120.7(3) . . ? C32 C33 H65 119.6 . . ? C34 C33 H65 119.6 . . ? C33 C32 C31 120.0(4) . . ? C33 C32 H66 120.0 . . ? C31 C32 H66 120.0 . . ? C32 C31 C30 122.2(4) . . ? C32 C31 H67 118.9 . . ? C30 C31 H67 118.9 . . ? C34 C999 H68A 109.5 . . ? C34 C999 H68B 109.5 . . ? H68A C999 H68B 109.5 . . ? C34 C999 H68C 109.5 . . ? H68A C999 H68C 109.5 . . ? H68B C999 H68C 109.5 . . ? C43 C38 C39 121.0(6) . . ? C43 C38 C37 121.6(6) . . ? C39 C38 C37 117.5(6) . . ? C42 C43 C38 121.7(8) . . ? C42 C43 H70 119.1 . . ? C38 C43 H70 119.1 . . ? C43 C42 C41 119.9(9) . . ? C43 C42 H71 120.0 . . ? C41 C42 H71 120.0 . . ? C42 C41 C40 119.6(7) . . ? C42 C41 H72 120.2 . . ? C40 C41 H72 120.2 . . ? C39 C40 C41 117.4(7) . . ? C39 C40 H73 121.3 . . ? C41 C40 H73 121.3 . . ? C38 C39 C40 120.4(7) . . ? C38 C39 H74 119.8 . . ? C40 C39 H74 119.8 . . ? C38 C37 H75A 109.5 . . ? C38 C37 H75B 109.5 . . ? H75A C37 H75B 109.5 . . ? C38 C37 H75C 109.5 . . ? H75A C37 H75C 109.5 . . ? H75B C37 H75C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.455 _refine_diff_density_min -1.198 _refine_diff_density_rms 0.095 #===END # Compound 6 data_en183bis _database_code_depnum_ccdc_archive 'CCDC 882557' #TrackingRef '- 2012_chemcomm_nicolas.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H102 P4 Pt2, C7 H8' _chemical_formula_sum 'C61 H110 P4 Pt2' _chemical_formula_weight 1357.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4080(10) _cell_length_b 17.2460(10) _cell_length_c 18.4540(10) _cell_angle_alpha 78.3290(10) _cell_angle_beta 72.9210(10) _cell_angle_gamma 85.1860(10) _cell_volume 3397.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 17913 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.327 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 4.239 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4844 _exptl_absorpt_correction_T_max 0.6765 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Kappa APEX II' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58812 _diffrn_reflns_av_R_equivalents 0.0518 _diffrn_reflns_av_sigmaI/netI 0.0374 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 27.48 _reflns_number_total 15501 _reflns_number_gt 13088 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.033 0.289 0.248 503 69 ' ' 2 -0.047 0.711 0.752 502 68 ' ' 3 0.267 0.202 0.960 8 1 ' ' 4 0.474 0.286 0.774 11 1 ' ' 5 0.525 0.714 0.226 11 1 ' ' 6 0.733 0.798 0.040 10 1 ' ' _platon_squeeze_details ; A highly disordered C7H8 molecule was accounted for using the Platon SQUEEZE function. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0202P)^2^+6.3036P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15501 _refine_ls_number_parameters 555 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0434 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0770 _refine_ls_wR_factor_gt 0.0719 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.255020(13) 0.762822(9) 0.177386(8) 0.03401(5) Uani 1 1 d . A . H1PT H 0.210(4) 0.686(3) 0.225(3) 0.051 Uiso 1 1 d . . . Pt2 Pt 0.220100(13) 0.750294(9) 0.325330(8) 0.03620(5) Uani 1 1 d . A . H2PT H 0.359(4) 0.748(3) 0.275(3) 0.054 Uiso 1 1 d . . . P1 P 0.30334(9) 0.71155(6) 0.06921(6) 0.0368(2) Uani 1 1 d . . . P2 P 0.30915(9) 0.88920(6) 0.12352(6) 0.0363(2) Uani 1 1 d . . . P3 P 0.27500(10) 0.70306(7) 0.43384(6) 0.0403(2) Uani 1 1 d . . . P4 P 0.01740(10) 0.77241(7) 0.37827(6) 0.0417(2) Uani 1 1 d . . . C1A C 0.3688(4) 0.7768(3) -0.0249(2) 0.0485(10) Uani 0.593(7) 1 d P A 1 H1A1 H 0.4201 0.7446 -0.0601 0.058 Uiso 0.593(7) 1 calc PR A 1 H1A2 H 0.3020 0.7991 -0.0458 0.058 Uiso 0.593(7) 1 calc PR A 1 C2A C 0.4453(7) 0.8451(5) -0.0226(4) 0.0501(15) Uani 0.593(7) 1 d P A 1 H2A1 H 0.5069 0.8234 0.0031 0.060 Uiso 0.593(7) 1 calc PR A 1 H2A2 H 0.4880 0.8688 -0.0752 0.060 Uiso 0.593(7) 1 calc PR A 1 C3A C 0.3734(4) 0.9087(3) 0.0171(2) 0.0493(11) Uani 0.593(7) 1 d P A 1 H3A1 H 0.3056 0.9246 -0.0048 0.059 Uiso 0.593(7) 1 calc PR A 1 H3A2 H 0.4258 0.9540 0.0034 0.059 Uiso 0.593(7) 1 calc PR A 1 C1B C 0.3688(4) 0.7768(3) -0.0249(2) 0.0485(10) Uani 0.407(7) 1 d P A 2 H1B1 H 0.4575 0.7740 -0.0366 0.058 Uiso 0.407(7) 1 calc PR A 2 H1B2 H 0.3469 0.7569 -0.0646 0.058 Uiso 0.407(7) 1 calc PR A 2 C2B C 0.3257(11) 0.8642(7) -0.0280(6) 0.0501(15) Uani 0.407(7) 1 d P A 2 H2B1 H 0.3493 0.8910 -0.0815 0.060 Uiso 0.407(7) 1 calc PR A 2 H2B2 H 0.2369 0.8661 -0.0099 0.060 Uiso 0.407(7) 1 calc PR A 2 C3B C 0.3734(4) 0.9087(3) 0.0171(2) 0.0493(11) Uani 0.407(7) 1 d P A 2 H3B1 H 0.3610 0.9647 -0.0014 0.059 Uiso 0.407(7) 1 calc PR A 2 H3B2 H 0.4613 0.8985 0.0054 0.059 Uiso 0.407(7) 1 calc PR A 2 C4 C 0.4249(4) 0.6328(3) 0.0678(3) 0.0449(10) Uani 1 1 d . A . H4 H 0.4491 0.6180 0.0168 0.054 Uiso 1 1 calc R . . C5 C 0.5382(4) 0.6645(3) 0.0804(3) 0.0639(14) Uani 1 1 d . . . H5A H 0.5146 0.6828 0.1292 0.077 Uiso 1 1 calc R A . H5B H 0.5687 0.7094 0.0397 0.077 Uiso 1 1 calc R . . C6 C 0.6414(5) 0.6006(4) 0.0807(4) 0.0806(18) Uani 1 1 d . A . H6A H 0.6720 0.5868 0.0299 0.097 Uiso 1 1 calc R . . H6B H 0.7087 0.6215 0.0923 0.097 Uiso 1 1 calc R . . C7 C 0.5945(5) 0.5273(4) 0.1400(4) 0.0773(17) Uani 1 1 d . . . H7A H 0.6593 0.4868 0.1367 0.093 Uiso 1 1 calc R A . H7B H 0.5734 0.5400 0.1912 0.093 Uiso 1 1 calc R . . C8 C 0.4842(5) 0.4953(3) 0.1286(4) 0.0695(15) Uani 1 1 d . A . H8A H 0.4541 0.4507 0.1698 0.083 Uiso 1 1 calc R . . H8B H 0.5076 0.4764 0.0801 0.083 Uiso 1 1 calc R . . C9 C 0.3811(4) 0.5589(3) 0.1281(3) 0.0586(13) Uani 1 1 d . . . H9A H 0.3135 0.5372 0.1175 0.070 Uiso 1 1 calc R A . H9B H 0.3513 0.5732 0.1787 0.070 Uiso 1 1 calc R . . C10 C 0.1780(4) 0.6637(2) 0.0506(2) 0.0406(9) Uani 1 1 d . A . H10 H 0.1460 0.6228 0.0961 0.049 Uiso 1 1 calc R . . C11 C 0.2148(5) 0.6223(3) -0.0185(3) 0.0626(13) Uani 1 1 d . . . H11A H 0.2774 0.5819 -0.0121 0.075 Uiso 1 1 calc R A . H11B H 0.2493 0.6605 -0.0650 0.075 Uiso 1 1 calc R . . C12 C 0.1043(5) 0.5841(4) -0.0270(4) 0.0737(16) Uani 1 1 d . A . H12A H 0.1296 0.5601 -0.0726 0.088 Uiso 1 1 calc R . . H12B H 0.0746 0.5425 0.0174 0.088 Uiso 1 1 calc R . . C13 C 0.0026(5) 0.6441(4) -0.0335(3) 0.0727(16) Uani 1 1 d . . . H13A H -0.0674 0.6178 -0.0364 0.087 Uiso 1 1 calc R A . H13B H 0.0299 0.6829 -0.0806 0.087 Uiso 1 1 calc R . . C14 C -0.0360(5) 0.6859(3) 0.0353(3) 0.0640(14) Uani 1 1 d . A . H14A H -0.0720 0.6480 0.0817 0.077 Uiso 1 1 calc R . . H14B H -0.0980 0.7264 0.0280 0.077 Uiso 1 1 calc R . . C15 C 0.0724(4) 0.7239(3) 0.0456(3) 0.0529(11) Uani 1 1 d . . . H15A H 0.0460 0.7460 0.0923 0.063 Uiso 1 1 calc R A . H15B H 0.1013 0.7669 0.0024 0.063 Uiso 1 1 calc R . . C16 C 0.4299(4) 0.9312(3) 0.1515(3) 0.0442(10) Uani 1 1 d . A . H16 H 0.4533 0.9817 0.1162 0.053 Uiso 1 1 calc R . . C17 C 0.3875(4) 0.9478(3) 0.2334(3) 0.0496(11) Uani 1 1 d . . . H17A H 0.3586 0.8993 0.2692 0.060 Uiso 1 1 calc R A . H17B H 0.3193 0.9859 0.2377 0.060 Uiso 1 1 calc R . . C18 C 0.4903(5) 0.9802(3) 0.2555(3) 0.0646(14) Uani 1 1 d . A . H18A H 0.5125 1.0319 0.2238 0.077 Uiso 1 1 calc R . . H18B H 0.4615 0.9864 0.3090 0.077 Uiso 1 1 calc R . . C19 C 0.6024(5) 0.9251(4) 0.2445(4) 0.0768(17) Uani 1 1 d . . . H19A H 0.5824 0.8755 0.2806 0.092 Uiso 1 1 calc R A . H19B H 0.6676 0.9487 0.2560 0.092 Uiso 1 1 calc R . . C20 C 0.6474(5) 0.9088(4) 0.1627(3) 0.0673(15) Uani 1 1 d . A . H20A H 0.7160 0.8711 0.1588 0.081 Uiso 1 1 calc R . . H20B H 0.6757 0.9574 0.1269 0.081 Uiso 1 1 calc R . . C21 C 0.5448(4) 0.8756(3) 0.1412(3) 0.0554(12) Uani 1 1 d . . . H21A H 0.5230 0.8241 0.1734 0.066 Uiso 1 1 calc R A . H21B H 0.5739 0.8687 0.0879 0.066 Uiso 1 1 calc R . . C22 C 0.1838(4) 0.9652(2) 0.1359(3) 0.0425(9) Uani 1 1 d . A . H22 H 0.1556 0.9662 0.1913 0.051 Uiso 1 1 calc R . . C23 C 0.2174(5) 1.0498(3) 0.0957(3) 0.0615(13) Uani 1 1 d . . . H23A H 0.2828 1.0659 0.1129 0.074 Uiso 1 1 calc R A . H23B H 0.2482 1.0515 0.0406 0.074 Uiso 1 1 calc R . . C24 C 0.1101(6) 1.1082(3) 0.1114(4) 0.0766(17) Uani 1 1 d . A . H24A H 0.0844 1.1111 0.1658 0.092 Uiso 1 1 calc R . . H24B H 0.1353 1.1604 0.0822 0.092 Uiso 1 1 calc R . . C25 C 0.0039(6) 1.0831(4) 0.0891(4) 0.0779(17) Uani 1 1 d . . . H25A H 0.0273 1.0852 0.0338 0.094 Uiso 1 1 calc R A . H25B H -0.0652 1.1196 0.1019 0.094 Uiso 1 1 calc R . . C26 C -0.0344(5) 0.9993(4) 0.1306(4) 0.0725(16) Uani 1 1 d . A . H26A H -0.0999 0.9838 0.1132 0.087 Uiso 1 1 calc R . . H26B H -0.0656 0.9984 0.1857 0.087 Uiso 1 1 calc R . . C27 C 0.0738(4) 0.9401(3) 0.1152(3) 0.0566(12) Uani 1 1 d . . . H27A H 0.0980 0.9361 0.0611 0.068 Uiso 1 1 calc R A . H27B H 0.0483 0.8883 0.1454 0.068 Uiso 1 1 calc R . . C28A C 0.1542(4) 0.6919(3) 0.5268(2) 0.0529(12) Uani 0.485(7) 1 d P B 1 H28A H 0.1184 0.6403 0.5372 0.063 Uiso 0.485(7) 1 calc PR B 1 H28B H 0.1917 0.6933 0.5674 0.063 Uiso 0.485(7) 1 calc PR B 1 C29A C 0.0491(9) 0.7566(7) 0.5304(5) 0.0574(17) Uani 0.485(7) 1 d P B 1 H29A H 0.0026 0.7557 0.5838 0.069 Uiso 0.485(7) 1 calc PR B 1 H29B H 0.0847 0.8085 0.5097 0.069 Uiso 0.485(7) 1 calc PR B 1 C30A C -0.0377(4) 0.7431(3) 0.4844(2) 0.0542(12) Uani 0.485(7) 1 d P B 1 H30A H -0.1142 0.7718 0.5023 0.065 Uiso 0.485(7) 1 calc PR B 1 H30B H -0.0559 0.6872 0.4967 0.065 Uiso 0.485(7) 1 calc PR B 1 C28B C 0.1542(4) 0.6919(3) 0.5268(2) 0.0529(12) Uani 0.515(7) 1 d P B 2 H28C H 0.1798 0.6510 0.5639 0.063 Uiso 0.515(7) 1 calc PR B 2 H28D H 0.1444 0.7412 0.5460 0.063 Uiso 0.515(7) 1 calc PR B 2 C29B C 0.0291(8) 0.6702(6) 0.5206(5) 0.0574(17) Uani 0.515(7) 1 d P B 2 H29C H -0.0223 0.6486 0.5717 0.069 Uiso 0.515(7) 1 calc PR B 2 H29D H 0.0420 0.6297 0.4893 0.069 Uiso 0.515(7) 1 calc PR B 2 C30B C -0.0377(4) 0.7431(3) 0.4844(2) 0.0542(12) Uani 0.515(7) 1 d P B 2 H30C H -0.0299 0.7878 0.5070 0.065 Uiso 0.515(7) 1 calc PR B 2 H30D H -0.1243 0.7320 0.4985 0.065 Uiso 0.515(7) 1 calc PR B 2 C31 C 0.3399(4) 0.6006(3) 0.4365(3) 0.0466(10) Uani 1 1 d . B . H31 H 0.3555 0.5823 0.4867 0.056 Uiso 1 1 calc R . . C32 C 0.4605(4) 0.5961(3) 0.3743(3) 0.0556(12) Uani 1 1 d . . . H32A H 0.5202 0.6279 0.3824 0.067 Uiso 1 1 calc R B . H32B H 0.4484 0.6183 0.3243 0.067 Uiso 1 1 calc R . . C33 C 0.5110(5) 0.5111(3) 0.3743(3) 0.0640(14) Uani 1 1 d . B . H33A H 0.5861 0.5108 0.3325 0.077 Uiso 1 1 calc R . . H33B H 0.5305 0.4904 0.4224 0.077 Uiso 1 1 calc R . . C34 C 0.4199(5) 0.4586(3) 0.3647(3) 0.0670(14) Uani 1 1 d . . . H34A H 0.4530 0.4048 0.3665 0.080 Uiso 1 1 calc R B . H34B H 0.4047 0.4768 0.3149 0.080 Uiso 1 1 calc R . . C35 C 0.3004(6) 0.4601(3) 0.4286(4) 0.0756(17) Uani 1 1 d . B . H35A H 0.3150 0.4383 0.4781 0.091 Uiso 1 1 calc R . . H35B H 0.2415 0.4272 0.4212 0.091 Uiso 1 1 calc R . . C36 C 0.2476(5) 0.5445(3) 0.4289(3) 0.0642(14) Uani 1 1 d . . . H36A H 0.1736 0.5440 0.4716 0.077 Uiso 1 1 calc R B . H36B H 0.2255 0.5642 0.3815 0.077 Uiso 1 1 calc R . . C37 C 0.3945(4) 0.7573(3) 0.4521(2) 0.0429(9) Uani 1 1 d . B . H37 H 0.4660 0.7589 0.4067 0.052 Uiso 1 1 calc R . . C38 C 0.4395(5) 0.7184(3) 0.5219(3) 0.0613(13) Uani 1 1 d . . . H38A H 0.4729 0.6659 0.5154 0.074 Uiso 1 1 calc R B . H38B H 0.3708 0.7130 0.5683 0.074 Uiso 1 1 calc R . . C39 C 0.5392(6) 0.7682(3) 0.5313(4) 0.0729(16) Uani 1 1 d . B . H39A H 0.5616 0.7442 0.5778 0.088 Uiso 1 1 calc R . . H39B H 0.6118 0.7682 0.4878 0.088 Uiso 1 1 calc R . . C40 C 0.4949(6) 0.8521(3) 0.5361(3) 0.0711(15) Uani 1 1 d . . . H40A H 0.5605 0.8823 0.5394 0.085 Uiso 1 1 calc R B . H40B H 0.4271 0.8526 0.5823 0.085 Uiso 1 1 calc R . . C41 C 0.4536(5) 0.8905(3) 0.4657(3) 0.0648(14) Uani 1 1 d . B . H41A H 0.5233 0.8940 0.4200 0.078 Uiso 1 1 calc R . . H41B H 0.4229 0.9438 0.4708 0.078 Uiso 1 1 calc R . . C42 C 0.3531(5) 0.8432(3) 0.4560(3) 0.0577(12) Uani 1 1 d . . . H42A H 0.2801 0.8446 0.4990 0.069 Uiso 1 1 calc R B . H42B H 0.3323 0.8677 0.4090 0.069 Uiso 1 1 calc R . . C43 C -0.0332(4) 0.8779(3) 0.3630(3) 0.0472(10) Uani 1 1 d . B . H43 H -0.0185 0.8951 0.3072 0.057 Uiso 1 1 calc R . . C44 C 0.0475(5) 0.9288(3) 0.3870(3) 0.0607(13) Uani 1 1 d . . . H44A H 0.0385 0.9124 0.4417 0.073 Uiso 1 1 calc R B . H44B H 0.1328 0.9203 0.3595 0.073 Uiso 1 1 calc R . . C45 C 0.0139(6) 1.0171(3) 0.3699(4) 0.0747(16) Uani 1 1 d . B . H45A H 0.0626 1.0467 0.3895 0.090 Uiso 1 1 calc R . . H45B H 0.0328 1.0353 0.3146 0.090 Uiso 1 1 calc R . . C46 C -0.1215(6) 1.0325(4) 0.4070(4) 0.0826(18) Uani 1 1 d . . . H46A H -0.1384 1.0197 0.4627 0.099 Uiso 1 1 calc R B . H46B H -0.1413 1.0883 0.3929 0.099 Uiso 1 1 calc R . . C47 C -0.2009(5) 0.9842(3) 0.3823(4) 0.0744(16) Uani 1 1 d . B . H47A H -0.1905 1.0008 0.3274 0.089 Uiso 1 1 calc R . . H47B H -0.2863 0.9932 0.4091 0.089 Uiso 1 1 calc R . . C48 C -0.1685(4) 0.8964(3) 0.3996(3) 0.0621(13) Uani 1 1 d . . . H48A H -0.2184 0.8671 0.3805 0.075 Uiso 1 1 calc R B . H48B H -0.1878 0.8787 0.4550 0.075 Uiso 1 1 calc R . . C49 C -0.0956(4) 0.7207(3) 0.3514(3) 0.0487(10) Uani 1 1 d . B . H49 H -0.1767 0.7288 0.3866 0.058 Uiso 1 1 calc R . . C50 C -0.0673(5) 0.6324(3) 0.3614(3) 0.0574(12) Uani 1 1 d . . . H50A H -0.0701 0.6119 0.4149 0.069 Uiso 1 1 calc R B . H50B H 0.0152 0.6233 0.3299 0.069 Uiso 1 1 calc R . . C51 C -0.1568(6) 0.5873(4) 0.3393(4) 0.0782(17) Uani 1 1 d . B . H51A H -0.2382 0.5914 0.3744 0.094 Uiso 1 1 calc R . . H51B H -0.1321 0.5317 0.3440 0.094 Uiso 1 1 calc R . . C52 C -0.1608(6) 0.6199(4) 0.2568(3) 0.0785(17) Uani 1 1 d . . . H52A H -0.0819 0.6103 0.2211 0.094 Uiso 1 1 calc R B . H52B H -0.2223 0.5926 0.2454 0.094 Uiso 1 1 calc R . . C53 C -0.1908(5) 0.7077(4) 0.2459(3) 0.0712(15) Uani 1 1 d . B . H53A H -0.2738 0.7165 0.2769 0.085 Uiso 1 1 calc R . . H53B H -0.1872 0.7277 0.1922 0.085 Uiso 1 1 calc R . . C54 C -0.1020(4) 0.7535(3) 0.2687(3) 0.0545(12) Uani 1 1 d . . . H54A H -0.1282 0.8088 0.2647 0.065 Uiso 1 1 calc R B . H54B H -0.0207 0.7506 0.2331 0.065 Uiso 1 1 calc 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 0.03346(8) 0.03839(8) 0.02774(8) -0.00246(6) -0.00653(6) -0.00421(6) Pt2 0.03458(8) 0.04315(9) 0.02772(8) -0.00292(6) -0.00680(6) 0.00000(6) P1 0.0365(5) 0.0411(5) 0.0317(5) -0.0064(4) -0.0073(4) -0.0039(4) P2 0.0370(5) 0.0397(5) 0.0320(5) -0.0018(4) -0.0110(4) -0.0070(4) P3 0.0380(5) 0.0496(6) 0.0313(5) -0.0039(5) -0.0099(4) 0.0008(5) P4 0.0337(5) 0.0533(6) 0.0354(5) -0.0077(5) -0.0067(4) 0.0010(5) C1A 0.054(3) 0.056(3) 0.029(2) -0.0086(19) -0.0004(18) -0.009(2) C2A 0.055(4) 0.057(4) 0.031(3) -0.005(3) -0.002(3) -0.008(3) C3A 0.060(3) 0.047(2) 0.037(2) 0.0005(19) -0.011(2) -0.015(2) C1B 0.054(3) 0.056(3) 0.029(2) -0.0086(19) -0.0004(18) -0.009(2) C2B 0.055(4) 0.057(4) 0.031(3) -0.005(3) -0.002(3) -0.008(3) C3B 0.060(3) 0.047(2) 0.037(2) 0.0005(19) -0.011(2) -0.015(2) C4 0.040(2) 0.053(3) 0.044(2) -0.016(2) -0.0108(18) 0.0004(19) C5 0.044(3) 0.075(4) 0.071(3) -0.008(3) -0.017(2) -0.006(2) C6 0.041(3) 0.103(5) 0.093(5) -0.013(4) -0.019(3) 0.008(3) C7 0.061(3) 0.102(5) 0.068(4) -0.020(3) -0.023(3) 0.028(3) C8 0.068(3) 0.060(3) 0.080(4) -0.012(3) -0.026(3) 0.017(3) C9 0.047(3) 0.051(3) 0.072(3) -0.005(2) -0.015(2) 0.006(2) C10 0.042(2) 0.044(2) 0.036(2) -0.0074(18) -0.0099(17) -0.0050(18) C11 0.054(3) 0.078(4) 0.066(3) -0.035(3) -0.017(2) -0.004(3) C12 0.061(3) 0.094(4) 0.086(4) -0.049(4) -0.026(3) -0.009(3) C13 0.060(3) 0.108(5) 0.062(3) -0.023(3) -0.026(3) -0.019(3) C14 0.047(3) 0.078(4) 0.071(4) -0.014(3) -0.021(2) -0.004(2) C15 0.047(3) 0.058(3) 0.057(3) -0.012(2) -0.019(2) 0.000(2) C16 0.043(2) 0.045(2) 0.046(2) -0.0013(19) -0.0167(19) -0.0112(18) C17 0.052(3) 0.054(3) 0.046(2) -0.005(2) -0.019(2) -0.012(2) C18 0.082(4) 0.059(3) 0.065(3) -0.009(3) -0.038(3) -0.017(3) C19 0.073(4) 0.094(4) 0.077(4) 0.001(3) -0.049(3) -0.018(3) C20 0.048(3) 0.082(4) 0.072(4) 0.006(3) -0.028(3) -0.010(3) C21 0.042(2) 0.065(3) 0.060(3) -0.003(2) -0.019(2) -0.008(2) C22 0.043(2) 0.042(2) 0.046(2) -0.0065(19) -0.0190(18) -0.0049(18) C23 0.065(3) 0.044(3) 0.077(4) 0.000(2) -0.028(3) -0.006(2) C24 0.086(4) 0.050(3) 0.100(5) -0.007(3) -0.045(4) 0.013(3) C25 0.081(4) 0.079(4) 0.080(4) -0.012(3) -0.042(3) 0.026(3) C26 0.053(3) 0.082(4) 0.085(4) -0.013(3) -0.028(3) 0.012(3) C27 0.048(3) 0.060(3) 0.067(3) -0.011(2) -0.025(2) 0.000(2) C28A 0.047(2) 0.073(3) 0.029(2) 0.004(2) -0.0060(18) 0.002(2) C29A 0.053(4) 0.079(5) 0.035(3) -0.008(3) -0.006(3) -0.003(4) C30A 0.041(2) 0.081(3) 0.034(2) -0.010(2) -0.0023(18) 0.004(2) C28B 0.047(2) 0.073(3) 0.029(2) 0.004(2) -0.0060(18) 0.002(2) C29B 0.053(4) 0.079(5) 0.035(3) -0.008(3) -0.006(3) -0.003(4) C30B 0.041(2) 0.081(3) 0.034(2) -0.010(2) -0.0023(18) 0.004(2) C31 0.050(3) 0.049(2) 0.041(2) -0.0005(19) -0.0189(19) -0.002(2) C32 0.046(3) 0.047(3) 0.073(3) -0.011(2) -0.017(2) 0.005(2) C33 0.068(3) 0.059(3) 0.070(4) -0.015(3) -0.029(3) 0.014(3) C34 0.090(4) 0.049(3) 0.064(3) -0.012(3) -0.026(3) 0.002(3) C35 0.100(5) 0.051(3) 0.074(4) -0.013(3) -0.017(3) -0.019(3) C36 0.059(3) 0.065(3) 0.066(3) -0.014(3) -0.010(3) -0.013(3) C37 0.045(2) 0.048(2) 0.038(2) -0.0106(19) -0.0134(18) -0.0005(19) C38 0.075(3) 0.059(3) 0.062(3) -0.005(2) -0.041(3) -0.002(3) C39 0.092(4) 0.074(4) 0.071(4) -0.007(3) -0.052(3) -0.012(3) C40 0.094(4) 0.068(3) 0.062(3) -0.015(3) -0.032(3) -0.016(3) C41 0.081(4) 0.054(3) 0.066(3) -0.017(3) -0.025(3) -0.005(3) C42 0.066(3) 0.051(3) 0.057(3) -0.013(2) -0.020(2) 0.007(2) C43 0.042(2) 0.057(3) 0.042(2) -0.013(2) -0.0097(18) 0.003(2) C44 0.060(3) 0.062(3) 0.066(3) -0.018(3) -0.025(3) 0.004(2) C45 0.087(4) 0.061(3) 0.085(4) -0.026(3) -0.030(3) 0.001(3) C46 0.093(5) 0.076(4) 0.085(4) -0.041(4) -0.025(4) 0.022(3) C47 0.065(3) 0.075(4) 0.087(4) -0.032(3) -0.022(3) 0.022(3) C48 0.044(3) 0.069(3) 0.071(3) -0.021(3) -0.011(2) 0.010(2) C49 0.038(2) 0.063(3) 0.044(2) -0.012(2) -0.0076(18) -0.002(2) C50 0.062(3) 0.060(3) 0.048(3) -0.004(2) -0.012(2) -0.013(2) C51 0.093(4) 0.071(4) 0.074(4) -0.008(3) -0.024(3) -0.036(3) C52 0.091(4) 0.089(4) 0.063(4) -0.014(3) -0.024(3) -0.033(4) C53 0.062(3) 0.095(4) 0.065(3) -0.014(3) -0.028(3) -0.015(3) C54 0.052(3) 0.066(3) 0.049(3) -0.010(2) -0.019(2) 0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P1 2.2487(11) . ? Pt1 P2 2.2602(10) . ? Pt1 Pt2 2.6069(2) . ? Pt1 H1PT 1.48(4) . ? Pt2 P3 2.2488(10) . ? Pt2 P4 2.2634(11) . ? Pt2 H2PT 1.59(4) . ? P1 C1A 1.851(4) . ? P1 C4 1.856(4) . ? P1 C10 1.857(4) . ? P2 C16 1.851(4) . ? P2 C22 1.852(4) . ? P2 C3A 1.854(4) . ? P3 C28A 1.844(4) . ? P3 C31 1.854(5) . ? P3 C37 1.860(4) . ? P4 C30A 1.848(4) . ? P4 C43 1.853(5) . ? P4 C49 1.859(5) . ? C1A C2A 1.537(9) . ? C1A H1A1 0.9700 . ? C1A H1A2 0.9700 . ? C2A C3A 1.495(9) . ? C2A H2A1 0.9700 . ? C2A H2A2 0.9700 . ? C3A H3A1 0.9700 . ? C3A H3A2 0.9700 . ? C2B H2B1 0.9700 . ? C2B H2B2 0.9700 . ? C4 C9 1.522(6) . ? C4 C5 1.539(6) . ? C4 H4 0.9800 . ? C5 C6 1.544(7) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.515(9) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.501(8) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.540(6) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.520(6) . ? C10 C15 1.534(6) . ? C10 H10 0.9800 . ? C11 C12 1.532(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.505(8) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.522(8) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.523(7) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.525(6) . ? C16 C21 1.546(6) . ? C16 H16 0.9800 . ? C17 C18 1.529(6) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.516(8) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.521(8) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.527(7) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.522(6) . ? C22 C27 1.532(6) . ? C22 H22 0.9800 . ? C23 C24 1.516(7) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.510(8) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.525(8) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.532(7) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28A C29A 1.564(11) . ? C28A H28A 0.9700 . ? C28A H28B 0.9700 . ? C29A C30A 1.540(11) . ? C29A H29A 0.9700 . ? C29A H29B 0.9700 . ? C30A H30A 0.9700 . ? C30A H30B 0.9700 . ? C29B H29C 0.9700 . ? C29B H29D 0.9700 . ? C31 C32 1.519(6) . ? C31 C36 1.542(7) . ? C31 H31 0.9800 . ? C32 C33 1.530(6) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.504(8) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.521(8) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.529(8) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C42 1.526(6) . ? C37 C38 1.534(6) . ? C37 H37 0.9800 . ? C38 C39 1.549(7) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.504(8) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 C41 1.518(7) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C42 1.532(7) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C48 1.528(6) . ? C43 C44 1.532(7) . ? C43 H43 0.9800 . ? C44 C45 1.530(7) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 C46 1.520(8) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 C47 1.499(8) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 C48 1.520(7) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 C50 1.515(7) . ? C49 C54 1.536(6) . ? C49 H49 0.9800 . ? C50 C51 1.524(7) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 C52 1.525(8) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 C53 1.510(9) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 C54 1.534(7) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pt1 P2 98.74(4) . . ? P1 Pt1 Pt2 152.18(3) . . ? P2 Pt1 Pt2 106.33(3) . . ? P1 Pt1 H1PT 91.0(17) . . ? P2 Pt1 H1PT 170.1(17) . . ? Pt2 Pt1 H1PT 64.6(17) . . ? P3 Pt2 P4 99.17(4) . . ? P3 Pt2 Pt1 151.26(3) . . ? P4 Pt2 Pt1 107.10(3) . . ? P3 Pt2 H2PT 90.4(16) . . ? P4 Pt2 H2PT 169.3(16) . . ? Pt1 Pt2 H2PT 64.7(16) . . ? C1A P1 C4 100.8(2) . . ? C1A P1 C10 102.1(2) . . ? C4 P1 C10 103.71(19) . . ? C1A P1 Pt1 118.97(15) . . ? C4 P1 Pt1 112.33(14) . . ? C10 P1 Pt1 116.66(14) . . ? C16 P2 C22 103.36(19) . . ? C16 P2 C3A 100.3(2) . . ? C22 P2 C3A 100.9(2) . . ? C16 P2 Pt1 118.23(14) . . ? C22 P2 Pt1 116.22(14) . . ? C3A P2 Pt1 115.22(15) . . ? C28A P3 C31 101.2(2) . . ? C28A P3 C37 102.6(2) . . ? C31 P3 C37 103.2(2) . . ? C28A P3 Pt2 118.14(15) . . ? C31 P3 Pt2 112.23(15) . . ? C37 P3 Pt2 117.19(14) . . ? C30A P4 C43 102.0(2) . . ? C30A P4 C49 99.4(2) . . ? C43 P4 C49 104.0(2) . . ? C30A P4 Pt2 115.37(15) . . ? C43 P4 Pt2 114.57(15) . . ? C49 P4 Pt2 119.02(15) . . ? C2A C1A P1 115.4(4) . . ? C2A C1A H1A1 108.4 . . ? P1 C1A H1A1 108.4 . . ? C2A C1A H1A2 108.4 . . ? P1 C1A H1A2 108.4 . . ? H1A1 C1A H1A2 107.5 . . ? C3A C2A C1A 114.9(6) . . ? C3A C2A H2A1 108.5 . . ? C1A C2A H2A1 108.5 . . ? C3A C2A H2A2 108.5 . . ? C1A C2A H2A2 108.5 . . ? H2A1 C2A H2A2 107.5 . . ? C2A C3A P2 120.0(4) . . ? C2A C3A H3A1 107.3 . . ? P2 C3A H3A1 107.3 . . ? C2A C3A H3A2 107.3 . . ? P2 C3A H3A2 107.3 . . ? H3A1 C3A H3A2 106.9 . . ? H2B1 C2B H2B2 107.4 . . ? C9 C4 C5 109.8(4) . . ? C9 C4 P1 112.4(3) . . ? C5 C4 P1 110.0(3) . . ? C9 C4 H4 108.1 . . ? C5 C4 H4 108.1 . . ? P1 C4 H4 108.1 . . ? C4 C5 C6 111.9(5) . . ? C4 C5 H5A 109.2 . . ? C6 C5 H5A 109.2 . . ? C4 C5 H5B 109.2 . . ? C6 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? C7 C6 C5 110.7(5) . . ? C7 C6 H6A 109.5 . . ? C5 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? C8 C7 C6 112.2(5) . . ? C8 C7 H7A 109.2 . . ? C6 C7 H7A 109.2 . . ? C8 C7 H7B 109.2 . . ? C6 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C7 C8 C9 111.5(5) . . ? C7 C8 H8A 109.3 . . ? C9 C8 H8A 109.3 . . ? C7 C8 H8B 109.3 . . ? C9 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? C4 C9 C8 112.0(4) . . ? C4 C9 H9A 109.2 . . ? C8 C9 H9A 109.2 . . ? C4 C9 H9B 109.2 . . ? C8 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C11 C10 C15 111.0(4) . . ? C11 C10 P1 116.0(3) . . ? C15 C10 P1 109.6(3) . . ? C11 C10 H10 106.5 . . ? C15 C10 H10 106.5 . . ? P1 C10 H10 106.5 . . ? C10 C11 C12 111.1(4) . . ? C10 C11 H11A 109.4 . . ? C12 C11 H11A 109.4 . . ? C10 C11 H11B 109.4 . . ? C12 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? C13 C12 C11 111.2(5) . . ? C13 C12 H12A 109.4 . . ? C11 C12 H12A 109.4 . . ? C13 C12 H12B 109.4 . . ? C11 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? C12 C13 C14 111.2(5) . . ? C12 C13 H13A 109.4 . . ? C14 C13 H13A 109.4 . . ? C12 C13 H13B 109.4 . . ? C14 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? C13 C14 C15 111.6(4) . . ? C13 C14 H14A 109.3 . . ? C15 C14 H14A 109.3 . . ? C13 C14 H14B 109.3 . . ? C15 C14 H14B 109.3 . . ? H14A C14 H14B 108.0 . . ? C14 C15 C10 111.5(4) . . ? C14 C15 H15A 109.3 . . ? C10 C15 H15A 109.3 . . ? C14 C15 H15B 109.3 . . ? C10 C15 H15B 109.3 . . ? H15A C15 H15B 108.0 . . ? C17 C16 C21 110.4(4) . . ? C17 C16 P2 113.3(3) . . ? C21 C16 P2 110.0(3) . . ? C17 C16 H16 107.7 . . ? C21 C16 H16 107.7 . . ? P2 C16 H16 107.7 . . ? C16 C17 C18 111.9(4) . . ? C16 C17 H17A 109.2 . . ? C18 C17 H17A 109.2 . . ? C16 C17 H17B 109.2 . . ? C18 C17 H17B 109.2 . . ? H17A C17 H17B 107.9 . . ? C19 C18 C17 111.1(4) . . ? C19 C18 H18A 109.4 . . ? C17 C18 H18A 109.4 . . ? C19 C18 H18B 109.4 . . ? C17 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? C18 C19 C20 112.0(4) . . ? C18 C19 H19A 109.2 . . ? C20 C19 H19A 109.2 . . ? C18 C19 H19B 109.2 . . ? C20 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? C19 C20 C21 110.7(4) . . ? C19 C20 H20A 109.5 . . ? C21 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? C21 C20 H20B 109.5 . . ? H20A C20 H20B 108.1 . . ? C20 C21 C16 111.6(4) . . ? C20 C21 H21A 109.3 . . ? C16 C21 H21A 109.3 . . ? C20 C21 H21B 109.3 . . ? C16 C21 H21B 109.3 . . ? H21A C21 H21B 108.0 . . ? C23 C22 C27 110.4(4) . . ? C23 C22 P2 116.8(3) . . ? C27 C22 P2 110.8(3) . . ? C23 C22 H22 106.0 . . ? C27 C22 H22 106.0 . . ? P2 C22 H22 106.0 . . ? C24 C23 C22 113.0(4) . . ? C24 C23 H23A 109.0 . . ? C22 C23 H23A 109.0 . . ? C24 C23 H23B 109.0 . . ? C22 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? C25 C24 C23 110.6(5) . . ? C25 C24 H24A 109.5 . . ? C23 C24 H24A 109.5 . . ? C25 C24 H24B 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 108.1 . . ? C24 C25 C26 111.2(4) . . ? C24 C25 H25A 109.4 . . ? C26 C25 H25A 109.4 . . ? C24 C25 H25B 109.4 . . ? C26 C25 H25B 109.4 . . ? H25A C25 H25B 108.0 . . ? C25 C26 C27 111.2(5) . . ? C25 C26 H26A 109.4 . . ? C27 C26 H26A 109.4 . . ? C25 C26 H26B 109.4 . . ? C27 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C26 C27 C22 111.7(4) . . ? C26 C27 H27A 109.3 . . ? C22 C27 H27A 109.3 . . ? C26 C27 H27B 109.3 . . ? C22 C27 H27B 109.3 . . ? H27A C27 H27B 107.9 . . ? C29A C28A P3 114.5(4) . . ? C29A C28A H28A 108.6 . . ? P3 C28A H28A 108.6 . . ? C29A C28A H28B 108.6 . . ? P3 C28A H28B 108.6 . . ? H28A C28A H28B 107.6 . . ? C30A C29A C28A 111.5(7) . . ? C30A C29A H29A 109.3 . . ? C28A C29A H29A 109.3 . . ? C30A C29A H29B 109.3 . . ? C28A C29A H29B 109.3 . . ? H29A C29A H29B 108.0 . . ? C29A C30A P4 116.9(5) . . ? C29A C30A H30A 108.1 . . ? P4 C30A H30A 108.1 . . ? C29A C30A H30B 108.1 . . ? P4 C30A H30B 108.1 . . ? H30A C30A H30B 107.3 . . ? H29C C29B H29D 107.9 . . ? C32 C31 C36 109.8(4) . . ? C32 C31 P3 112.3(3) . . ? C36 C31 P3 110.8(3) . . ? C32 C31 H31 107.9 . . ? C36 C31 H31 107.9 . . ? P3 C31 H31 107.9 . . ? C31 C32 C33 112.3(4) . . ? C31 C32 H32A 109.2 . . ? C33 C32 H32A 109.2 . . ? C31 C32 H32B 109.2 . . ? C33 C32 H32B 109.2 . . ? H32A C32 H32B 107.9 . . ? C34 C33 C32 111.3(4) . . ? C34 C33 H33A 109.4 . . ? C32 C33 H33A 109.4 . . ? C34 C33 H33B 109.4 . . ? C32 C33 H33B 109.4 . . ? H33A C33 H33B 108.0 . . ? C33 C34 C35 110.0(5) . . ? C33 C34 H34A 109.7 . . ? C35 C34 H34A 109.7 . . ? C33 C34 H34B 109.7 . . ? C35 C34 H34B 109.7 . . ? H34A C34 H34B 108.2 . . ? C34 C35 C36 111.0(5) . . ? C34 C35 H35A 109.4 . . ? C36 C35 H35A 109.4 . . ? C34 C35 H35B 109.4 . . ? C36 C35 H35B 109.4 . . ? H35A C35 H35B 108.0 . . ? C35 C36 C31 111.8(5) . . ? C35 C36 H36A 109.3 . . ? C31 C36 H36A 109.3 . . ? C35 C36 H36B 109.3 . . ? C31 C36 H36B 109.3 . . ? H36A C36 H36B 107.9 . . ? C42 C37 C38 111.2(4) . . ? C42 C37 P3 110.5(3) . . ? C38 C37 P3 115.7(3) . . ? C42 C37 H37 106.3 . . ? C38 C37 H37 106.3 . . ? P3 C37 H37 106.3 . . ? C37 C38 C39 111.2(4) . . ? C37 C38 H38A 109.4 . . ? C39 C38 H38A 109.4 . . ? C37 C38 H38B 109.4 . . ? C39 C38 H38B 109.4 . . ? H38A C38 H38B 108.0 . . ? C40 C39 C38 111.5(5) . . ? C40 C39 H39A 109.3 . . ? C38 C39 H39A 109.3 . . ? C40 C39 H39B 109.3 . . ? C38 C39 H39B 109.3 . . ? H39A C39 H39B 108.0 . . ? C39 C40 C41 110.7(5) . . ? C39 C40 H40A 109.5 . . ? C41 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? C41 C40 H40B 109.5 . . ? H40A C40 H40B 108.1 . . ? C40 C41 C42 111.6(5) . . ? C40 C41 H41A 109.3 . . ? C42 C41 H41A 109.3 . . ? C40 C41 H41B 109.3 . . ? C42 C41 H41B 109.3 . . ? H41A C41 H41B 108.0 . . ? C37 C42 C41 111.4(4) . . ? C37 C42 H42A 109.3 . . ? C41 C42 H42A 109.3 . . ? C37 C42 H42B 109.3 . . ? C41 C42 H42B 109.3 . . ? H42A C42 H42B 108.0 . . ? C48 C43 C44 110.0(4) . . ? C48 C43 P4 116.7(3) . . ? C44 C43 P4 110.6(3) . . ? C48 C43 H43 106.3 . . ? C44 C43 H43 106.3 . . ? P4 C43 H43 106.3 . . ? C45 C44 C43 112.0(4) . . ? C45 C44 H44A 109.2 . . ? C43 C44 H44A 109.2 . . ? C45 C44 H44B 109.2 . . ? C43 C44 H44B 109.2 . . ? H44A C44 H44B 107.9 . . ? C46 C45 C44 111.1(5) . . ? C46 C45 H45A 109.4 . . ? C44 C45 H45A 109.4 . . ? C46 C45 H45B 109.4 . . ? C44 C45 H45B 109.4 . . ? H45A C45 H45B 108.0 . . ? C47 C46 C45 111.6(5) . . ? C47 C46 H46A 109.3 . . ? C45 C46 H46A 109.3 . . ? C47 C46 H46B 109.3 . . ? C45 C46 H46B 109.3 . . ? H46A C46 H46B 108.0 . . ? C46 C47 C48 111.2(5) . . ? C46 C47 H47A 109.4 . . ? C48 C47 H47A 109.4 . . ? C46 C47 H47B 109.4 . . ? C48 C47 H47B 109.4 . . ? H47A C47 H47B 108.0 . . ? C47 C48 C43 112.5(5) . . ? C47 C48 H48A 109.1 . . ? C43 C48 H48A 109.1 . . ? C47 C48 H48B 109.1 . . ? C43 C48 H48B 109.1 . . ? H48A C48 H48B 107.8 . . ? C50 C49 C54 110.2(4) . . ? C50 C49 P4 110.6(3) . . ? C54 C49 P4 112.5(3) . . ? C50 C49 H49 107.8 . . ? C54 C49 H49 107.8 . . ? P4 C49 H49 107.8 . . ? C49 C50 C51 112.7(5) . . ? C49 C50 H50A 109.1 . . ? C51 C50 H50A 109.1 . . ? C49 C50 H50B 109.1 . . ? C51 C50 H50B 109.1 . . ? H50A C50 H50B 107.8 . . ? C50 C51 C52 111.2(5) . . ? C50 C51 H51A 109.4 . . ? C52 C51 H51A 109.4 . . ? C50 C51 H51B 109.4 . . ? C52 C51 H51B 109.4 . . ? H51A C51 H51B 108.0 . . ? C53 C52 C51 110.8(5) . . ? C53 C52 H52A 109.5 . . ? C51 C52 H52A 109.5 . . ? C53 C52 H52B 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 108.1 . . ? C52 C53 C54 112.0(5) . . ? C52 C53 H53A 109.2 . . ? C54 C53 H53A 109.2 . . ? C52 C53 H53B 109.2 . . ? C54 C53 H53B 109.2 . . ? H53A C53 H53B 107.9 . . ? C53 C54 C49 112.0(4) . . ? C53 C54 H54A 109.2 . . ? C49 C54 H54A 109.2 . . ? C53 C54 H54B 109.2 . . ? C49 C54 H54B 109.2 . . ? H54A C54 H54B 107.9 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.337 _refine_diff_density_min -1.124 _refine_diff_density_rms 0.099