Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Cameron Jones' 'Marcus Brym' _publ_contact_author_name 'Prof Cameron Jones' _publ_contact_author_address ; Department of Chemistry University of Wales PO Box 912 Park Place Cardiff CF10 3TB UNITED KINGDOM ; _publ_contact_author_email JONESCA6@CARDIFF.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthesis, Characterisation and Reactivity of the First Diphosphaalkyne ; data_compound_3 _database_code_CSD 216489 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C98 H82 O P6 Pt2' _chemical_formula_weight 1851.64 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' O O 0.0106 0.0060 '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 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 24.329(5) _cell_length_b 26.421(5) _cell_length_c 13.270(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.04(3) _cell_angle_gamma 90.00 _cell_volume 8238(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.493 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3696 _exptl_absorpt_coefficient_mu 3.558 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.543 _exptl_absorpt_correction_T_max 0.794 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24581 _diffrn_reflns_av_R_equivalents 0.1172 _diffrn_reflns_av_sigmaI/netI 0.1041 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 25.39 _reflns_number_total 7480 _reflns_number_gt 5535 _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. ; _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^)+(0.0634P)^2^+299.9397P] 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 SHELXL _refine_ls_extinction_coef 0.00016(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7480 _refine_ls_number_parameters 472 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1175 _refine_ls_R_factor_gt 0.0873 _refine_ls_wR_factor_ref 0.2057 _refine_ls_wR_factor_gt 0.1940 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.145 _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 0.30789(2) 0.125971(19) 0.68956(4) 0.0242(2) Uani 1 1 d . . . P1 P 0.32976(15) 0.17646(13) 0.5619(3) 0.0293(8) Uani 1 1 d . . . P2 P 0.21100(14) 0.12694(13) 0.6206(3) 0.0287(8) Uani 1 1 d . . . P3 P 0.32588(14) 0.08119(13) 0.8436(3) 0.0248(7) Uani 1 1 d . . . O1 O 0.0000 0.1202(12) 0.7500 0.128(10) Uiso 1 2 d S . . C1 C 0.3823(6) 0.1578(5) 0.6645(11) 0.029(3) Uani 1 1 d . . . C2 C 0.4441(6) 0.1577(5) 0.7055(9) 0.023(3) Uani 1 1 d . . . C3 C 0.4788(5) 0.1855(4) 0.6402(9) 0.020(3) Uani 1 1 d . . . C4 C 0.5390(5) 0.1846(5) 0.6889(10) 0.024(3) Uani 1 1 d . . . C5 C 0.5750(5) 0.2106(5) 0.6431(11) 0.030(3) Uani 1 1 d . . . H5 H 0.6147 0.2107 0.6758 0.036 Uiso 1 1 calc R . . C6 C 0.5548(6) 0.2367(6) 0.5498(11) 0.034(3) Uani 1 1 d . . . H6 H 0.5805 0.2540 0.5188 0.041 Uiso 1 1 calc R . . C7 C 0.4963(6) 0.2375(6) 0.5016(12) 0.036(3) Uani 1 1 d . . . H7 H 0.4819 0.2559 0.4388 0.043 Uiso 1 1 calc R . . C8 C 0.4589(6) 0.2102(6) 0.5482(11) 0.036(3) Uani 1 1 d . . . H8 H 0.4194 0.2093 0.5145 0.043 Uiso 1 1 calc R . . C9 C 0.4710(6) 0.1042(5) 0.7252(9) 0.023(3) Uani 1 1 d . . . C10 C 0.4427(6) 0.0594(4) 0.6957(10) 0.024(3) Uani 1 1 d . . . H10 H 0.4038 0.0593 0.6577 0.029 Uiso 1 1 calc R . . C11 C 0.4721(6) 0.0148(5) 0.7227(11) 0.029(3) Uani 1 1 d . . . H11 H 0.4532 -0.0165 0.7030 0.035 Uiso 1 1 calc R . . C12 C 0.1918(6) 0.1446(5) 0.4815(11) 0.031(3) Uani 1 1 d . . . C13 C 0.2157(6) 0.1156(6) 0.4147(11) 0.037(4) Uani 1 1 d . . . H13 H 0.2409 0.0884 0.4412 0.044 Uiso 1 1 calc R . . C14 C 0.2015(7) 0.1277(7) 0.3073(13) 0.049(4) Uani 1 1 d . . . H14 H 0.2174 0.1087 0.2610 0.059 Uiso 1 1 calc R . . C15 C 0.1651(8) 0.1666(7) 0.2699(13) 0.052(5) Uani 1 1 d . . . H15 H 0.1551 0.1736 0.1973 0.063 Uiso 1 1 calc R . . C16 C 0.1430(8) 0.1952(7) 0.3333(14) 0.053(5) Uani 1 1 d . . . H16 H 0.1185 0.2226 0.3054 0.064 Uiso 1 1 calc R . . C17 C 0.1560(7) 0.1846(6) 0.4412(11) 0.039(4) Uani 1 1 d . . . H17 H 0.1402 0.2048 0.4860 0.047 Uiso 1 1 calc R . . C18 C 0.1636(6) 0.0739(5) 0.6205(13) 0.034(4) Uani 1 1 d . . . C19 C 0.1164(7) 0.0649(6) 0.5325(15) 0.049(4) Uani 1 1 d . . . H19 H 0.1098 0.0867 0.4736 0.059 Uiso 1 1 calc R . . C20 C 0.0791(7) 0.0232(7) 0.5328(17) 0.062(5) Uani 1 1 d . . . H20 H 0.0470 0.0180 0.4752 0.074 Uiso 1 1 calc R . . C21 C 0.0893(7) -0.0087(6) 0.6144(15) 0.047(4) Uani 1 1 d . . . H21 H 0.0652 -0.0370 0.6136 0.057 Uiso 1 1 calc R . . C22 C 0.1354(7) -0.0002(6) 0.7000(12) 0.043(4) Uani 1 1 d . . . H22 H 0.1413 -0.0218 0.7591 0.052 Uiso 1 1 calc R . . C23 C 0.1718(7) 0.0386(5) 0.6998(12) 0.038(4) Uani 1 1 d . . . H23 H 0.2046 0.0417 0.7568 0.045 Uiso 1 1 calc R . . C24 C 0.1829(6) 0.1772(5) 0.6831(10) 0.027(3) Uani 1 1 d U . . C25 C 0.2082(6) 0.2229(5) 0.7012(12) 0.038(4) Uani 1 1 d . . . H25 H 0.2419 0.2283 0.6792 0.045 Uiso 1 1 calc R . . C26 C 0.1879(8) 0.2628(6) 0.7501(15) 0.054(5) Uani 1 1 d . . . H26 H 0.2082 0.2938 0.7644 0.064 Uiso 1 1 calc R . . C27 C 0.1374(8) 0.2558(7) 0.7771(16) 0.058(5) Uani 1 1 d . . . H27 H 0.1228 0.2826 0.8102 0.070 Uiso 1 1 calc R . . C28 C 0.1085(7) 0.2126(7) 0.7582(13) 0.047(4) Uani 1 1 d . . . H28 H 0.0745 0.2087 0.7801 0.057 Uiso 1 1 calc R . . C29 C 0.1279(7) 0.1721(6) 0.7055(13) 0.043(4) Uani 1 1 d . . . H29 H 0.1054 0.1426 0.6855 0.051 Uiso 1 1 calc R . . C30 C 0.2701(5) 0.0891(5) 0.9122(9) 0.027(3) Uani 1 1 d . . . C31 C 0.2453(7) 0.0496(7) 0.9533(12) 0.045(4) Uani 1 1 d . . . H31 H 0.2587 0.0163 0.9472 0.054 Uiso 1 1 calc R . . C32 C 0.2020(7) 0.0563(8) 1.0030(13) 0.053(5) Uani 1 1 d . . . H32 H 0.1844 0.0284 1.0274 0.063 Uiso 1 1 calc R . . C33 C 0.1860(7) 0.1052(8) 1.0148(12) 0.050(4) Uani 1 1 d . . . H33 H 0.1583 0.1108 1.0525 0.060 Uiso 1 1 calc R . . C34 C 0.2083(9) 0.1477(7) 0.9744(14) 0.057(5) Uani 1 1 d . . . H34 H 0.1943 0.1808 0.9802 0.068 Uiso 1 1 calc R . . C35 C 0.2519(7) 0.1387(7) 0.9256(12) 0.043(4) Uani 1 1 d . . . H35 H 0.2695 0.1665 0.9011 0.052 Uiso 1 1 calc R . . C36 C 0.3905(6) 0.0921(5) 0.9486(10) 0.029(3) Uani 1 1 d . . . C37 C 0.3928(6) 0.1248(6) 1.0323(11) 0.040(4) Uani 1 1 d . . . H37 H 0.3591 0.1412 1.0386 0.048 Uiso 1 1 calc R . . C38 C 0.4428(7) 0.1334(6) 1.1049(14) 0.044(4) Uani 1 1 d . . . H38 H 0.4435 0.1575 1.1585 0.053 Uiso 1 1 calc R . . C39 C 0.4923(6) 0.1086(6) 1.1034(12) 0.036(3) Uani 1 1 d . . . H39 H 0.5267 0.1145 1.1555 0.043 Uiso 1 1 calc R . . C40 C 0.4901(7) 0.0739(6) 1.0217(12) 0.044(4) Uani 1 1 d . . . H40 H 0.5230 0.0552 1.0192 0.053 Uiso 1 1 calc R . . C41 C 0.4405(6) 0.0673(6) 0.9462(11) 0.031(3) Uani 1 1 d . . . H41 H 0.4402 0.0449 0.8901 0.038 Uiso 1 1 calc R . . C42 C 0.3309(6) 0.0130(5) 0.8282(11) 0.030(3) Uani 1 1 d . . . C43 C 0.3519(6) -0.0193(5) 0.9156(11) 0.035(3) Uani 1 1 d . . . H43 H 0.3615 -0.0060 0.9845 0.042 Uiso 1 1 calc R . . C44 C 0.3580(6) -0.0709(5) 0.8983(12) 0.038(4) Uani 1 1 d . . . H44 H 0.3712 -0.0925 0.9568 0.046 Uiso 1 1 calc R . . C45 C 0.3459(6) -0.0914(6) 0.8010(11) 0.036(3) Uani 1 1 d . . . H45 H 0.3515 -0.1265 0.7915 0.043 Uiso 1 1 calc R . . C46 C 0.3252(6) -0.0600(5) 0.7160(13) 0.038(4) Uani 1 1 d . . . H46 H 0.3157 -0.0736 0.6474 0.046 Uiso 1 1 calc R . . C47 C 0.3183(6) -0.0085(6) 0.7309(12) 0.035(3) Uani 1 1 d . . . H47 H 0.3042 0.0124 0.6717 0.042 Uiso 1 1 calc R . . C48 C 0.0253(10) 0.1271(8) 0.9191(18) 0.075(6) Uiso 1 1 d . . . H48A H 0.0416 0.1093 0.9848 0.113 Uiso 1 1 calc R . . H48B H -0.0123 0.1404 0.9194 0.113 Uiso 1 1 calc R . . H48C H 0.0503 0.1551 0.9116 0.113 Uiso 1 1 calc R . . C49 C -0.0198(11) 0.0937(10) 0.6639(19) 0.089(7) Uiso 1 1 d . . . H49A H -0.0572 0.0787 0.6632 0.107 Uiso 1 1 calc R . . H49B H 0.0069 0.0660 0.6592 0.107 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 0.0255(3) 0.0247(3) 0.0201(3) 0.0003(2) 0.00188(18) 0.0031(2) P1 0.0335(19) 0.0285(18) 0.0221(18) 0.0077(15) 0.0000(15) -0.0005(15) P2 0.0266(16) 0.0258(17) 0.0319(19) 0.0014(16) 0.0043(14) 0.0012(16) P3 0.0235(17) 0.0309(18) 0.0186(17) -0.0004(14) 0.0030(14) 0.0022(14) C1 0.038(8) 0.017(6) 0.033(8) 0.021(6) 0.010(6) 0.015(6) C2 0.036(7) 0.021(6) 0.012(6) 0.005(5) 0.005(5) -0.008(6) C3 0.030(7) 0.019(6) 0.011(6) -0.002(5) 0.005(5) -0.003(5) C4 0.028(7) 0.019(6) 0.025(7) 0.003(5) 0.007(5) 0.000(5) C5 0.018(6) 0.031(7) 0.032(8) 0.000(6) -0.008(6) -0.002(6) C6 0.032(7) 0.042(8) 0.029(8) 0.008(7) 0.009(6) 0.001(7) C7 0.036(8) 0.033(7) 0.036(9) 0.013(6) 0.003(7) -0.001(6) C8 0.037(8) 0.043(8) 0.025(8) 0.003(7) 0.003(6) 0.000(7) C9 0.034(7) 0.024(6) 0.011(6) 0.001(5) 0.007(5) 0.009(6) C10 0.034(7) 0.014(6) 0.023(7) 0.000(5) 0.007(6) -0.006(5) C11 0.035(7) 0.027(7) 0.031(8) 0.001(6) 0.017(6) 0.002(6) C12 0.029(7) 0.026(7) 0.032(8) 0.004(6) -0.006(6) 0.002(6) C13 0.038(8) 0.043(9) 0.022(7) -0.014(6) -0.004(6) 0.004(7) C14 0.049(10) 0.054(10) 0.041(9) -0.010(9) 0.008(8) -0.008(9) C15 0.067(12) 0.050(10) 0.029(9) 0.001(8) -0.006(8) -0.011(9) C16 0.059(11) 0.048(10) 0.044(11) 0.003(8) -0.002(9) 0.002(9) C17 0.048(9) 0.040(8) 0.024(8) 0.011(7) -0.001(7) 0.010(7) C18 0.025(7) 0.023(7) 0.059(10) 0.013(7) 0.018(7) 0.012(6) C19 0.035(8) 0.039(9) 0.066(12) 0.010(8) -0.002(8) 0.004(7) C20 0.030(9) 0.064(12) 0.082(15) -0.015(11) -0.002(9) -0.023(9) C21 0.042(9) 0.021(7) 0.077(13) -0.003(8) 0.012(9) -0.009(7) C22 0.050(10) 0.045(9) 0.033(9) 0.010(7) 0.006(7) -0.003(8) C23 0.039(8) 0.033(8) 0.037(9) 0.009(7) 0.004(7) -0.007(7) C24 0.037(5) 0.026(5) 0.013(4) -0.002(4) 0.000(4) -0.006(4) C25 0.033(8) 0.027(7) 0.050(10) -0.010(7) 0.004(7) 0.000(6) C26 0.066(12) 0.028(8) 0.074(13) -0.011(8) 0.032(10) 0.002(8) C27 0.055(11) 0.043(10) 0.076(14) -0.001(9) 0.016(10) 0.023(9) C28 0.034(8) 0.064(11) 0.049(10) 0.008(9) 0.019(8) 0.017(8) C29 0.037(8) 0.038(9) 0.052(10) -0.013(8) 0.010(7) 0.005(7) C30 0.025(7) 0.043(8) 0.011(6) -0.008(6) 0.003(5) 0.001(6) C31 0.047(9) 0.058(10) 0.031(9) 0.001(8) 0.014(7) -0.004(8) C32 0.041(9) 0.090(14) 0.031(9) 0.000(9) 0.017(7) -0.014(10) C33 0.039(9) 0.086(14) 0.022(8) 0.002(9) 0.003(7) 0.008(9) C34 0.077(13) 0.052(10) 0.043(10) -0.019(9) 0.021(9) 0.018(10) C35 0.040(8) 0.061(11) 0.027(8) 0.004(7) 0.005(7) 0.006(8) C36 0.027(7) 0.039(8) 0.018(7) 0.006(6) 0.003(5) 0.002(6) C37 0.043(8) 0.044(9) 0.028(8) -0.003(7) 0.000(6) 0.009(8) C38 0.047(9) 0.030(8) 0.054(10) -0.009(7) 0.012(8) -0.004(7) C39 0.029(7) 0.043(8) 0.036(8) -0.010(7) 0.008(6) -0.013(6) C40 0.039(9) 0.056(10) 0.038(9) 0.009(8) 0.012(7) -0.002(8) C41 0.035(8) 0.043(8) 0.020(7) -0.010(6) 0.016(6) -0.008(7) C42 0.022(7) 0.037(8) 0.033(8) 0.000(6) 0.008(6) -0.004(6) C43 0.043(8) 0.038(8) 0.016(7) 0.012(6) -0.007(6) 0.002(7) C44 0.041(8) 0.030(8) 0.041(9) 0.012(7) 0.004(7) 0.009(7) C45 0.031(8) 0.034(8) 0.036(9) 0.001(7) -0.003(6) 0.000(6) C46 0.034(8) 0.032(8) 0.044(9) -0.008(7) 0.003(7) -0.002(6) C47 0.031(8) 0.041(8) 0.030(8) 0.007(7) 0.003(6) 0.003(6) _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 C1 2.098(14) . ? Pt1 P2 2.297(3) . ? Pt1 P3 2.304(3) . ? Pt1 P1 2.323(4) . ? P1 C1 1.681(13) . ? P2 C24 1.791(14) . ? P2 C18 1.815(14) . ? P2 C12 1.843(14) . ? P3 C42 1.822(14) . ? P3 C30 1.832(13) . ? P3 C36 1.833(13) . ? O1 C49 1.32(3) 2_556 ? O1 C49 1.32(3) . ? C1 C2 1.462(19) . ? C2 C4 1.529(17) 2_656 ? C2 C3 1.543(17) . ? C2 C9 1.550(17) . ? C3 C8 1.357(18) . ? C3 C4 1.439(18) . ? C4 C5 1.375(19) . ? C4 C2 1.529(17) 2_656 ? C5 C6 1.391(19) . ? C6 C7 1.40(2) . ? C7 C8 1.42(2) . ? C9 C10 1.374(18) . ? C9 C9 1.39(3) 2_656 ? C10 C11 1.378(18) . ? C11 C11 1.36(3) 2_656 ? C12 C17 1.387(19) . ? C12 C13 1.41(2) . ? C13 C14 1.41(2) . ? C14 C15 1.36(2) . ? C15 C16 1.34(3) . ? C16 C17 1.41(2) . ? C18 C23 1.38(2) . ? C18 C19 1.43(2) . ? C19 C20 1.43(2) . ? C20 C21 1.34(3) . ? C21 C22 1.39(2) . ? C22 C23 1.36(2) . ? C24 C25 1.349(19) . ? C24 C29 1.45(2) . ? C25 C26 1.39(2) . ? C26 C27 1.38(3) . ? C27 C28 1.33(2) . ? C28 C29 1.42(2) . ? C30 C31 1.38(2) . ? C30 C35 1.41(2) . ? C31 C32 1.39(2) . ? C32 C33 1.37(3) . ? C33 C34 1.41(3) . ? C34 C35 1.40(2) . ? C36 C41 1.389(19) . ? C36 C37 1.40(2) . ? C37 C38 1.36(2) . ? C38 C39 1.38(2) . ? C39 C40 1.41(2) . ? C40 C41 1.36(2) . ? C42 C47 1.37(2) . ? C42 C43 1.423(19) . ? C43 C44 1.40(2) . ? C44 C45 1.36(2) . ? C45 C46 1.39(2) . ? C46 C47 1.39(2) . ? C48 C49 1.39(3) 2_556 ? C49 C48 1.39(3) 2_556 ? 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 C1 Pt1 P2 140.4(3) . . ? C1 Pt1 P3 111.9(3) . . ? P2 Pt1 P3 107.36(13) . . ? C1 Pt1 P1 44.3(3) . . ? P2 Pt1 P1 96.24(13) . . ? P3 Pt1 P1 156.21(12) . . ? C1 P1 Pt1 60.7(5) . . ? C24 P2 C18 104.7(6) . . ? C24 P2 C12 104.4(6) . . ? C18 P2 C12 101.4(7) . . ? C24 P2 Pt1 107.4(4) . . ? C18 P2 Pt1 125.3(4) . . ? C12 P2 Pt1 111.6(5) . . ? C42 P3 C30 104.4(6) . . ? C42 P3 C36 99.9(6) . . ? C30 P3 C36 101.9(6) . . ? C42 P3 Pt1 114.3(5) . . ? C30 P3 Pt1 112.8(4) . . ? C36 P3 Pt1 121.4(5) . . ? C49 O1 C49 116(3) 2_556 . ? C2 C1 P1 142.6(10) . . ? C2 C1 Pt1 142.0(9) . . ? P1 C1 Pt1 75.0(5) . . ? C1 C2 C4 110.3(11) . 2_656 ? C1 C2 C3 116.8(10) . . ? C4 C2 C3 103.7(10) 2_656 . ? C1 C2 C9 114.4(10) . . ? C4 C2 C9 105.5(9) 2_656 . ? C3 C2 C9 105.1(10) . . ? C8 C3 C4 119.7(12) . . ? C8 C3 C2 128.0(12) . . ? C4 C3 C2 112.3(10) . . ? C5 C4 C3 119.0(11) . . ? C5 C4 C2 125.9(12) . 2_656 ? C3 C4 C2 114.9(11) . 2_656 ? C4 C5 C6 121.5(12) . . ? C5 C6 C7 119.8(13) . . ? C6 C7 C8 118.9(13) . . ? C3 C8 C7 121.1(13) . . ? C10 C9 C9 120.4(8) . 2_656 ? C10 C9 C2 125.3(11) . . ? C9 C9 C2 114.3(6) 2_656 . ? C9 C10 C11 118.4(12) . . ? C11 C11 C10 121.1(8) 2_656 . ? C17 C12 C13 119.6(14) . . ? C17 C12 P2 123.3(12) . . ? C13 C12 P2 117.1(10) . . ? C12 C13 C14 118.6(14) . . ? C15 C14 C13 120.2(16) . . ? C16 C15 C14 121.6(16) . . ? C15 C16 C17 120.3(16) . . ? C12 C17 C16 119.6(16) . . ? C23 C18 C19 115.9(13) . . ? C23 C18 P2 123.6(12) . . ? C19 C18 P2 120.4(12) . . ? C20 C19 C18 120.2(16) . . ? C21 C20 C19 120.0(16) . . ? C20 C21 C22 120.0(14) . . ? C23 C22 C21 120.5(15) . . ? C22 C23 C18 123.1(14) . . ? C25 C24 C29 116.6(13) . . ? C25 C24 P2 122.4(11) . . ? C29 C24 P2 120.6(10) . . ? C24 C25 C26 124.1(15) . . ? C27 C26 C25 117.9(16) . . ? C28 C27 C26 122.0(17) . . ? C27 C28 C29 120.7(16) . . ? C28 C29 C24 118.3(14) . . ? C31 C30 C35 117.9(14) . . ? C31 C30 P3 124.3(11) . . ? C35 C30 P3 117.8(11) . . ? C30 C31 C32 123.5(17) . . ? C33 C32 C31 116.4(17) . . ? C32 C33 C34 124.0(16) . . ? C35 C34 C33 117.0(16) . . ? C34 C35 C30 121.1(16) . . ? C41 C36 C37 117.1(12) . . ? C41 C36 P3 119.5(10) . . ? C37 C36 P3 123.4(11) . . ? C38 C37 C36 120.7(14) . . ? C37 C38 C39 122.3(15) . . ? C38 C39 C40 117.5(14) . . ? C41 C40 C39 119.9(15) . . ? C40 C41 C36 122.3(14) . . ? C47 C42 C43 117.7(13) . . ? C47 C42 P3 120.7(11) . . ? C43 C42 P3 121.4(11) . . ? C44 C43 C42 118.8(13) . . ? C45 C44 C43 122.6(14) . . ? C44 C45 C46 118.5(14) . . ? C45 C46 C47 120.1(14) . . ? C42 C47 C46 122.3(14) . . ? O1 C49 C48 107(2) . 2_556 ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.39 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 3.231 #(near Pt1) _refine_diff_density_min -1.907 _refine_diff_density_rms 0.227 data_cmpd2 _database_code_CSD 216490 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H12 P2' _chemical_formula_weight 338.26 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.1140(16) _cell_length_b 10.161(2) _cell_length_c 20.829(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.23(3) _cell_angle_gamma 90.00 _cell_volume 1684.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.334 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 0.257 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9505 _exptl_absorpt_correction_T_max 0.9748 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13682 _diffrn_reflns_av_R_equivalents 0.0860 _diffrn_reflns_av_sigmaI/netI 0.0657 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3732 _reflns_number_gt 2626 _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. ; _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^)+(0.0639P)^2^+0.8720P] 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 SHELXL _refine_ls_extinction_coef 0.009(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3732 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0853 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.1478 _refine_ls_wR_factor_gt 0.1294 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 P1 P 0.88711(11) 0.12758(7) 0.06549(4) 0.0423(2) Uani 1 1 d . . . P2 P 1.14272(10) -0.66392(7) 0.20129(4) 0.0410(2) Uani 1 1 d . . . C1 C 0.9335(3) -0.0106(2) 0.09246(11) 0.0293(5) Uani 1 1 d . . . C2 C 1.0980(3) -0.5231(2) 0.17777(11) 0.0283(5) Uani 1 1 d . . . C3 C 0.9773(3) -0.1456(2) 0.11536(10) 0.0237(5) Uani 1 1 d . . . C4 C 1.1658(3) -0.1788(2) 0.12112(10) 0.0243(5) Uani 1 1 d . . . C5 C 1.2060(3) -0.3076(2) 0.14230(10) 0.0238(5) Uani 1 1 d . . . C6 C 1.3695(3) -0.3518(2) 0.15071(11) 0.0287(5) Uani 1 1 d . . . H6 H 1.3970 -0.4391 0.1653 0.034 Uiso 1 1 calc R . . C7 C 1.4940(3) -0.2671(3) 0.13755(12) 0.0351(6) Uani 1 1 d . . . H7 H 1.6066 -0.2972 0.1427 0.042 Uiso 1 1 calc R . . C8 C 1.4544(3) -0.1396(3) 0.11699(12) 0.0349(6) Uani 1 1 d . . . H8 H 1.5401 -0.0824 0.1084 0.042 Uiso 1 1 calc R . . C9 C 1.2898(3) -0.0947(2) 0.10882(11) 0.0284(5) Uani 1 1 d . . . H9 H 1.2628 -0.0070 0.0949 0.034 Uiso 1 1 calc R . . C10 C 0.9402(3) -0.1751(2) 0.18393(10) 0.0224(5) Uani 1 1 d . . . C11 C 0.9805(3) -0.3042(2) 0.20494(10) 0.0226(5) Uani 1 1 d . . . C12 C 0.9538(3) -0.3457(2) 0.26535(11) 0.0281(5) Uani 1 1 d . . . H12 H 0.9813 -0.4331 0.2798 0.034 Uiso 1 1 calc R . . C13 C 0.8862(3) -0.2582(3) 0.30481(11) 0.0331(6) Uani 1 1 d . . . H13 H 0.8667 -0.2865 0.3462 0.040 Uiso 1 1 calc R . . C14 C 0.8472(3) -0.1306(3) 0.28418(12) 0.0325(6) Uani 1 1 d . . . H14 H 0.8014 -0.0716 0.3114 0.039 Uiso 1 1 calc R . . C15 C 0.8750(3) -0.0882(2) 0.22338(11) 0.0280(5) Uani 1 1 d . . . H15 H 0.8494 -0.0003 0.2093 0.034 Uiso 1 1 calc R . . C16 C 0.8816(3) -0.2522(2) 0.07033(10) 0.0237(5) Uani 1 1 d . . . C17 C 0.9227(3) -0.3806(2) 0.09176(10) 0.0226(5) Uani 1 1 d . . . C18 C 0.8459(3) -0.4869(2) 0.05720(11) 0.0290(5) Uani 1 1 d . . . H18 H 0.8741 -0.5740 0.0720 0.035 Uiso 1 1 calc R . . C19 C 0.7269(3) -0.4656(3) 0.00057(12) 0.0365(6) Uani 1 1 d . . . H19 H 0.6729 -0.5384 -0.0234 0.044 Uiso 1 1 calc R . . C20 C 0.6866(3) -0.3385(3) -0.02107(12) 0.0359(6) Uani 1 1 d . . . H20 H 0.6060 -0.3247 -0.0601 0.043 Uiso 1 1 calc R . . C21 C 0.7632(3) -0.2314(2) 0.01394(11) 0.0302(6) Uani 1 1 d . . . H21 H 0.7343 -0.1444 -0.0008 0.036 Uiso 1 1 calc R . . C22 C 1.0552(3) -0.3871(2) 0.15570(10) 0.0221(5) Uani 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 P1 0.0572(5) 0.0281(4) 0.0434(4) 0.0053(3) 0.0145(4) 0.0054(3) P2 0.0446(5) 0.0312(4) 0.0435(4) 0.0090(3) -0.0008(3) 0.0064(3) C1 0.0284(14) 0.0317(13) 0.0278(12) -0.0024(10) 0.0056(10) -0.0019(10) C2 0.0227(13) 0.0329(13) 0.0275(12) -0.0001(10) 0.0007(10) 0.0000(10) C3 0.0240(12) 0.0256(11) 0.0211(11) 0.0006(9) 0.0030(9) 0.0005(9) C4 0.0220(13) 0.0308(12) 0.0192(10) -0.0041(9) 0.0019(9) -0.0016(9) C5 0.0235(13) 0.0281(12) 0.0187(10) -0.0035(9) 0.0010(9) -0.0017(9) C6 0.0230(13) 0.0347(13) 0.0273(12) -0.0049(10) 0.0018(10) 0.0006(10) C7 0.0211(13) 0.0497(16) 0.0344(13) -0.0072(12) 0.0049(11) -0.0008(11) C8 0.0270(14) 0.0464(15) 0.0329(13) -0.0065(11) 0.0098(11) -0.0129(11) C9 0.0313(14) 0.0317(12) 0.0229(11) -0.0014(9) 0.0065(10) -0.0085(10) C10 0.0172(12) 0.0279(11) 0.0212(10) -0.0021(9) 0.0014(9) -0.0043(9) C11 0.0168(11) 0.0280(12) 0.0213(10) -0.0020(9) -0.0006(9) -0.0040(9) C12 0.0240(13) 0.0333(13) 0.0250(12) 0.0014(10) -0.0004(10) -0.0090(10) C13 0.0327(15) 0.0460(15) 0.0216(11) -0.0042(11) 0.0079(10) -0.0125(11) C14 0.0251(13) 0.0441(15) 0.0289(12) -0.0101(11) 0.0071(10) -0.0049(11) C15 0.0237(13) 0.0294(12) 0.0302(12) -0.0062(10) 0.0036(10) -0.0022(10) C16 0.0224(12) 0.0283(12) 0.0210(10) 0.0009(9) 0.0056(9) -0.0007(9) C17 0.0190(12) 0.0290(12) 0.0198(10) -0.0014(9) 0.0036(9) -0.0011(9) C18 0.0282(14) 0.0288(12) 0.0293(12) -0.0042(10) 0.0034(10) -0.0027(10) C19 0.0328(15) 0.0422(15) 0.0320(13) -0.0105(12) 0.0002(11) -0.0082(11) C20 0.0303(15) 0.0503(16) 0.0227(12) 0.0011(11) -0.0054(10) -0.0007(12) C21 0.0293(14) 0.0371(13) 0.0231(11) 0.0049(10) 0.0020(10) 0.0006(11) C22 0.0205(12) 0.0245(11) 0.0208(11) -0.0002(9) 0.0025(9) 0.0001(9) _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 P1 C1 1.531(2) . ? P2 C2 1.533(2) . ? C1 C3 1.473(3) . ? C2 C22 1.476(3) . ? C3 C16 1.541(3) . ? C3 C10 1.545(3) . ? C3 C4 1.547(3) . ? C4 C9 1.381(3) . ? C4 C5 1.400(3) . ? C5 C6 1.379(3) . ? C5 C22 1.537(3) . ? C6 C7 1.394(3) . ? C7 C8 1.383(4) . ? C8 C9 1.390(4) . ? C10 C15 1.380(3) . ? C10 C11 1.401(3) . ? C11 C12 1.384(3) . ? C11 C22 1.539(3) . ? C12 C13 1.394(3) . ? C13 C14 1.384(4) . ? C14 C15 1.397(3) . ? C16 C21 1.381(3) . ? C16 C17 1.398(3) . ? C17 C18 1.378(3) . ? C17 C22 1.541(3) . ? C18 C19 1.388(3) . ? C19 C20 1.386(4) . ? C20 C21 1.388(3) . ? 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 C3 C1 P1 177.44(19) . . ? C22 C2 P2 179.52(19) . . ? C1 C3 C16 113.36(18) . . ? C1 C3 C10 113.70(19) . . ? C16 C3 C10 105.06(17) . . ? C1 C3 C4 113.63(19) . . ? C16 C3 C4 105.49(17) . . ? C10 C3 C4 104.70(17) . . ? C9 C4 C5 120.2(2) . . ? C9 C4 C3 126.5(2) . . ? C5 C4 C3 113.25(19) . . ? C6 C5 C4 120.3(2) . . ? C6 C5 C22 125.9(2) . . ? C4 C5 C22 113.82(19) . . ? C5 C6 C7 119.4(2) . . ? C8 C7 C6 120.4(2) . . ? C7 C8 C9 120.3(2) . . ? C4 C9 C8 119.5(2) . . ? C15 C10 C11 120.4(2) . . ? C15 C10 C3 126.3(2) . . ? C11 C10 C3 113.24(19) . . ? C12 C11 C10 120.0(2) . . ? C12 C11 C22 126.2(2) . . ? C10 C11 C22 113.74(18) . . ? C11 C12 C13 119.4(2) . . ? C14 C13 C12 120.5(2) . . ? C13 C14 C15 120.2(2) . . ? C10 C15 C14 119.4(2) . . ? C21 C16 C17 119.8(2) . . ? C21 C16 C3 126.5(2) . . ? C17 C16 C3 113.66(19) . . ? C18 C17 C16 120.6(2) . . ? C18 C17 C22 125.9(2) . . ? C16 C17 C22 113.50(18) . . ? C17 C18 C19 119.4(2) . . ? C20 C19 C18 120.2(2) . . ? C19 C20 C21 120.5(2) . . ? C16 C21 C20 119.5(2) . . ? C2 C22 C5 113.65(19) . . ? C2 C22 C11 113.84(18) . . ? C5 C22 C11 105.29(17) . . ? C2 C22 C17 113.04(18) . . ? C5 C22 C17 105.45(17) . . ? C11 C22 C17 104.70(17) . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.444 _refine_diff_density_min -0.377 _refine_diff_density_rms 0.065