data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Cameron Jones' _publ_contact_author_address ; Chemistry Department Cardiff University Ctre Fund & App Main Grp Chemistry Main Building Cardiff CF10 3AT UNITED KINGDOM ; _publ_contact_author_email JONESCA6@CARDIFF.AC.UK _publ_section_title ; The First Complexes and Cyclooligomerisations of Methylphosphaalkyne (P CMe) ; loop_ _publ_author_name 'Cameron Jones' 'Christian Schulten' 'Andreas Stasch' # Attachment 'compound3.CIF' data_compound3 _database_code_depnum_ccdc_archive 'CCDC 609152' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H61 O P5 Pt2' _chemical_formula_weight 1319.10 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 P2(1)/c 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 13.450(3) _cell_length_b 17.802(4) _cell_length_c 22.023(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.08(3) _cell_angle_gamma 90.00 _cell_volume 5252.7(18) _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 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.668 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2592 _exptl_absorpt_coefficient_mu 5.512 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.603 _exptl_absorpt_correction_T_max 0.952 _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 20104 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0436 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10300 _reflns_number_gt 8883 _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. During the course of refinement, the PCMe ligand was found to be disordered over two sites. This disorder was successfuly modelled. ; _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^)+(0.0082P)^2^+8.1388P] 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 10300 _refine_ls_number_parameters 627 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.0375 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0526 _refine_ls_wR_factor_gt 0.0504 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.037 _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 0.726148(11) 0.854327(8) 0.821860(6) 0.01761(4) Uani 1 1 d . . . P1 P 0.57651(16) 0.85784(11) 0.75660(8) 0.0185(5) Uani 0.738(5) 1 d PDU A 1 O1 O 0.2462(3) 0.6336(2) 1.10544(16) 0.0520(9) Uani 1 1 d . . . C1 C 0.5754(10) 0.8511(6) 0.8351(5) 0.018(3) Uani 0.738(5) 1 d PDU A 1 Pt2 Pt 0.555283(11) 0.742228(8) 0.805025(6) 0.01610(4) Uani 1 1 d . . . P2 P 0.83486(8) 0.87725(6) 0.90379(4) 0.0204(2) Uani 1 1 d . A . C2 C 0.5167(4) 0.8848(3) 0.8854(2) 0.0262(14) Uani 0.738(5) 1 d PD A 1 H2A H 0.5335 0.9382 0.8905 0.039 Uiso 0.738(5) 1 calc PR A 1 H2B H 0.5344 0.8583 0.9238 0.039 Uiso 0.738(5) 1 calc PR A 1 H2C H 0.4450 0.8795 0.8740 0.039 Uiso 0.738(5) 1 calc PR A 1 P3 P 0.86000(8) 0.85237(6) 0.76652(4) 0.0211(2) Uani 1 1 d . A . C3 C 0.9446(3) 0.9191(2) 0.87130(17) 0.0263(9) Uani 1 1 d . . . H3A H 0.9283 0.9703 0.8559 0.032 Uiso 1 1 calc R A . H3B H 1.0013 0.9226 0.9030 0.032 Uiso 1 1 calc R . . P4 P 0.49597(7) 0.67418(5) 0.87998(4) 0.0181(2) Uani 1 1 d . A . C4 C 0.9725(3) 0.8687(2) 0.81907(17) 0.0259(9) Uani 1 1 d . A . H4A H 0.9991 0.8202 0.8355 0.031 Uiso 1 1 calc R . . H4B H 1.0247 0.8933 0.7971 0.031 Uiso 1 1 calc R . . P5 P 0.54196(8) 0.63607(5) 0.74852(4) 0.0189(2) Uani 1 1 d . A . C5 C 0.8060(3) 0.9414(2) 0.96412(17) 0.0242(9) Uani 1 1 d . . . C6 C 0.8518(3) 1.0108(2) 0.9742(2) 0.0332(10) Uani 1 1 d . A . H6 H 0.9034 1.0257 0.9500 0.040 Uiso 1 1 calc R . . C7 C 0.8229(3) 1.0586(3) 1.0194(2) 0.0398(12) Uani 1 1 d . . . H7 H 0.8539 1.1063 1.0253 0.048 Uiso 1 1 calc R A . C8 C 0.7495(4) 1.0370(3) 1.05561(19) 0.0384(12) Uani 1 1 d . A . H8 H 0.7305 1.0697 1.0867 0.046 Uiso 1 1 calc R . . C9 C 0.7036(4) 0.9685(3) 1.04697(18) 0.0364(11) Uani 1 1 d . . . H9 H 0.6537 0.9533 1.0723 0.044 Uiso 1 1 calc R A . C10 C 0.7308(3) 0.9213(2) 1.00072(18) 0.0293(10) Uani 1 1 d . A . H10 H 0.6974 0.8747 0.9940 0.035 Uiso 1 1 calc R . . C11 C 0.8947(3) 0.7986(2) 0.94695(17) 0.0224(9) Uani 1 1 d . . . C12 C 0.9472(3) 0.8078(2) 1.00369(18) 0.0268(9) Uani 1 1 d . A . H12 H 0.9504 0.8560 1.0222 0.032 Uiso 1 1 calc R . . C13 C 0.9949(3) 0.7477(3) 1.03362(19) 0.0342(11) Uani 1 1 d . . . H13 H 1.0303 0.7548 1.0725 0.041 Uiso 1 1 calc R A . C14 C 0.9911(3) 0.6776(3) 1.0071(2) 0.0355(11) Uani 1 1 d . A . H14 H 1.0250 0.6365 1.0272 0.043 Uiso 1 1 calc R . . C15 C 0.9376(3) 0.6670(2) 0.9510(2) 0.0331(11) Uani 1 1 d . . . H15 H 0.9339 0.6185 0.9330 0.040 Uiso 1 1 calc R A . C16 C 0.8894(3) 0.7276(2) 0.92081(18) 0.0257(9) Uani 1 1 d . A . H16 H 0.8529 0.7202 0.8823 0.031 Uiso 1 1 calc R . . C17 C 0.8668(3) 0.9271(2) 0.71002(18) 0.0241(9) Uani 1 1 d . . . C18 C 0.8152(3) 0.9929(2) 0.7179(2) 0.0390(12) Uani 1 1 d . A . H18 H 0.7747 0.9972 0.7509 0.047 Uiso 1 1 calc R . . C19 C 0.8215(4) 1.0527(3) 0.6783(2) 0.0456(13) Uani 1 1 d . . . H19 H 0.7869 1.0980 0.6850 0.055 Uiso 1 1 calc R A . C20 C 0.8775(3) 1.0468(3) 0.6296(2) 0.0410(12) Uani 1 1 d . A . H20 H 0.8809 1.0876 0.6020 0.049 Uiso 1 1 calc R . . C21 C 0.9288(4) 0.9815(3) 0.6209(2) 0.0401(12) Uani 1 1 d . . . H21 H 0.9677 0.9773 0.5870 0.048 Uiso 1 1 calc R A . C22 C 0.9246(3) 0.9219(2) 0.66069(19) 0.0329(10) Uani 1 1 d . A . H22 H 0.9611 0.8773 0.6545 0.039 Uiso 1 1 calc R . . C23 C 0.8857(3) 0.7675(2) 0.72441(18) 0.0248(9) Uani 1 1 d . . . C24 C 0.9763(4) 0.7297(3) 0.7284(2) 0.0445(13) Uani 1 1 d . A . H24 H 1.0314 0.7493 0.7534 0.053 Uiso 1 1 calc R . . C25 C 0.9873(4) 0.6631(3) 0.6959(2) 0.0499(14) Uani 1 1 d . . . H25 H 1.0495 0.6375 0.6992 0.060 Uiso 1 1 calc R A . C26 C 0.9082(4) 0.6347(3) 0.6592(2) 0.0438(13) Uani 1 1 d . A . H26 H 0.9156 0.5894 0.6373 0.053 Uiso 1 1 calc R . . C27 C 0.8183(4) 0.6721(3) 0.6544(2) 0.0391(12) Uani 1 1 d . . . H27 H 0.7641 0.6533 0.6282 0.047 Uiso 1 1 calc R A . C28 C 0.8068(3) 0.7369(2) 0.68742(19) 0.0311(10) Uani 1 1 d . A . H28 H 0.7436 0.7611 0.6848 0.037 Uiso 1 1 calc R . . C29 C 0.4700(3) 0.5774(2) 0.85222(17) 0.0229(9) Uani 1 1 d . . . H29A H 0.5282 0.5449 0.8643 0.027 Uiso 1 1 calc R A . H29B H 0.4117 0.5571 0.8713 0.027 Uiso 1 1 calc R . . C30 C 0.4487(3) 0.5763(2) 0.78265(16) 0.0214(9) Uani 1 1 d . A . H30A H 0.3806 0.5956 0.7711 0.026 Uiso 1 1 calc R . . H30B H 0.4527 0.5242 0.7674 0.026 Uiso 1 1 calc R . . C31 C 0.3722(3) 0.7067(2) 0.89768(17) 0.0197(8) Uani 1 1 d . . . C32 C 0.3148(3) 0.7433(2) 0.85126(19) 0.0256(9) Uani 1 1 d . A . H32 H 0.3417 0.7528 0.8136 0.031 Uiso 1 1 calc R . . C33 C 0.2182(3) 0.7661(2) 0.85967(19) 0.0282(10) Uani 1 1 d . . . H33 H 0.1793 0.7906 0.8274 0.034 Uiso 1 1 calc R A . C34 C 0.1782(3) 0.7536(2) 0.91456(19) 0.0274(10) Uani 1 1 d . A . H34 H 0.1117 0.7684 0.9199 0.033 Uiso 1 1 calc R . . C35 C 0.2358(3) 0.7193(2) 0.96139(19) 0.0286(10) Uani 1 1 d . . . H35 H 0.2094 0.7115 0.9995 0.034 Uiso 1 1 calc R A . C36 C 0.3323(3) 0.6959(2) 0.95343(18) 0.0279(10) Uani 1 1 d . A . H36 H 0.3714 0.6725 0.9861 0.033 Uiso 1 1 calc R . . C37 C 0.5672(3) 0.6590(2) 0.95331(17) 0.0203(8) Uani 1 1 d . . . C38 C 0.6515(3) 0.7027(2) 0.96736(17) 0.0224(9) Uani 1 1 d . A . H38 H 0.6699 0.7396 0.9393 0.027 Uiso 1 1 calc R . . C39 C 0.7091(3) 0.6928(2) 1.02242(19) 0.0306(10) Uani 1 1 d . . . H39 H 0.7665 0.7231 1.0318 0.037 Uiso 1 1 calc R A . C40 C 0.6835(3) 0.6394(2) 1.06340(19) 0.0343(11) Uani 1 1 d . A . H40 H 0.7228 0.6330 1.1011 0.041 Uiso 1 1 calc R . . C41 C 0.6000(3) 0.5952(2) 1.04925(19) 0.0344(11) Uani 1 1 d . . . H41 H 0.5819 0.5585 1.0776 0.041 Uiso 1 1 calc R A . C42 C 0.5430(3) 0.6039(2) 0.99454(18) 0.0282(10) Uani 1 1 d . A . H42 H 0.4869 0.5722 0.9849 0.034 Uiso 1 1 calc R . . C43 C 0.6534(3) 0.5762(2) 0.75368(16) 0.0219(9) Uani 1 1 d . . . C44 C 0.7378(3) 0.6018(2) 0.78823(17) 0.0264(9) Uani 1 1 d . A . H44 H 0.7373 0.6495 0.8075 0.032 Uiso 1 1 calc R . . C45 C 0.8230(3) 0.5575(3) 0.7946(2) 0.0382(11) Uani 1 1 d . . . H45 H 0.8807 0.5753 0.8182 0.046 Uiso 1 1 calc R A . C46 C 0.8248(4) 0.4881(3) 0.7672(2) 0.0474(14) Uani 1 1 d . A . H46 H 0.8833 0.4581 0.7719 0.057 Uiso 1 1 calc R . . C47 C 0.7404(4) 0.4625(3) 0.7326(2) 0.0447(13) Uani 1 1 d . . . H47 H 0.7414 0.4148 0.7133 0.054 Uiso 1 1 calc R A . C48 C 0.6545(3) 0.5061(2) 0.72598(18) 0.0324(10) Uani 1 1 d . A . H48 H 0.5967 0.4881 0.7026 0.039 Uiso 1 1 calc R . . C49 C 0.4981(3) 0.6346(2) 0.66759(17) 0.0210(9) Uani 1 1 d . . . C50 C 0.5299(3) 0.6918(2) 0.63094(18) 0.0286(10) Uani 1 1 d . A . H50 H 0.5740 0.7292 0.6484 0.034 Uiso 1 1 calc R . . C51 C 0.4984(3) 0.6950(2) 0.56945(19) 0.0340(11) Uani 1 1 d . . . H51 H 0.5213 0.7340 0.5447 0.041 Uiso 1 1 calc R A . C52 C 0.4336(3) 0.6413(2) 0.5444(2) 0.0366(11) Uani 1 1 d . A . H52 H 0.4115 0.6432 0.5023 0.044 Uiso 1 1 calc R . . C53 C 0.4009(4) 0.5850(3) 0.5804(2) 0.0420(12) Uani 1 1 d . . . H53 H 0.3561 0.5481 0.5629 0.050 Uiso 1 1 calc R A . C54 C 0.4327(3) 0.5816(2) 0.64159(19) 0.0338(11) Uani 1 1 d . A . H54 H 0.4094 0.5425 0.6660 0.041 Uiso 1 1 calc R . . C55 C 0.3072(5) 0.6810(4) 1.1457(3) 0.0734(19) Uani 1 1 d . . . H55A H 0.3683 0.6952 1.1264 0.088 Uiso 1 1 calc R . . H55B H 0.3277 0.6535 1.1839 0.088 Uiso 1 1 calc R . . C56 C 0.2520(6) 0.7491(4) 1.1599(3) 0.097(3) Uani 1 1 d . . . H56A H 0.2331 0.7768 1.1222 0.145 Uiso 1 1 calc R . . H56B H 0.2944 0.7809 1.1878 0.145 Uiso 1 1 calc R . . H56C H 0.1918 0.7350 1.1792 0.145 Uiso 1 1 calc R . . C57 C 0.2921(4) 0.5648(3) 1.0924(3) 0.0601(17) Uani 1 1 d . . . H57A H 0.3089 0.5367 1.1307 0.072 Uiso 1 1 calc R . . H57B H 0.3547 0.5746 1.0733 0.072 Uiso 1 1 calc R . . C58 C 0.2233(5) 0.5199(3) 1.0507(3) 0.0729(19) Uani 1 1 d . . . H58A H 0.1621 0.5095 1.0702 0.109 Uiso 1 1 calc R . . H58B H 0.2556 0.4724 1.0414 0.109 Uiso 1 1 calc R . . H58C H 0.2069 0.5480 1.0129 0.109 Uiso 1 1 calc R . . C2A C 0.5768(11) 0.8726(8) 0.7027(6) 0.022(4) Uani 0.262(5) 1 d PD A 2 H2A1 H 0.5046 0.8687 0.6928 0.033 Uiso 0.262(5) 1 calc PR A 2 H2A2 H 0.6113 0.8411 0.6747 0.033 Uiso 0.262(5) 1 calc PR A 2 H2A3 H 0.5976 0.9250 0.6986 0.033 Uiso 0.262(5) 1 calc PR A 2 C1A C 0.604(2) 0.8461(18) 0.7686(8) 0.072(15) Uani 0.262(5) 1 d PDU A 2 P1A P 0.5603(8) 0.8696(5) 0.8391(4) 0.0127(17) Uani 0.262(5) 1 d PDU A 2 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 0.01703(9) 0.01844(8) 0.01716(8) -0.00011(6) 0.00048(6) -0.00303(6) P1 0.0184(9) 0.0186(8) 0.0183(9) 0.0015(6) 0.0007(7) -0.0041(7) O1 0.044(2) 0.056(2) 0.055(2) 0.0157(18) -0.0018(18) -0.0011(18) C1 0.013(5) 0.017(5) 0.026(4) -0.007(3) 0.009(3) 0.006(4) Pt2 0.01592(8) 0.01469(7) 0.01751(8) 0.00034(6) 0.00049(6) -0.00126(6) P2 0.0210(6) 0.0206(5) 0.0188(5) -0.0009(4) -0.0023(4) -0.0025(4) C2 0.028(3) 0.022(3) 0.030(3) -0.005(2) 0.010(3) 0.003(2) P3 0.0171(6) 0.0270(6) 0.0192(5) 0.0022(4) 0.0005(4) -0.0024(4) C3 0.022(2) 0.029(2) 0.026(2) 0.0032(18) -0.0049(18) -0.0089(18) P4 0.0181(5) 0.0175(5) 0.0185(5) 0.0025(4) 0.0007(4) -0.0008(4) C4 0.018(2) 0.033(2) 0.026(2) 0.0064(18) -0.0002(18) -0.0038(18) P5 0.0203(6) 0.0170(5) 0.0190(5) -0.0017(4) -0.0002(4) -0.0017(4) C5 0.025(2) 0.022(2) 0.024(2) -0.0021(17) -0.0045(18) 0.0039(17) C6 0.029(3) 0.033(2) 0.036(3) -0.007(2) -0.006(2) 0.000(2) C7 0.034(3) 0.032(3) 0.049(3) -0.020(2) -0.018(2) 0.005(2) C8 0.044(3) 0.042(3) 0.026(2) -0.015(2) -0.012(2) 0.019(2) C9 0.047(3) 0.041(3) 0.021(2) 0.001(2) 0.004(2) 0.016(2) C10 0.035(3) 0.028(2) 0.024(2) 0.0000(18) -0.001(2) 0.0039(19) C11 0.019(2) 0.027(2) 0.023(2) 0.0007(17) 0.0059(17) -0.0006(17) C12 0.026(2) 0.032(2) 0.023(2) 0.0016(18) 0.0029(18) 0.0018(19) C13 0.034(3) 0.046(3) 0.022(2) 0.007(2) 0.004(2) 0.006(2) C14 0.029(3) 0.037(3) 0.042(3) 0.016(2) 0.012(2) 0.011(2) C15 0.031(3) 0.027(2) 0.043(3) 0.004(2) 0.013(2) 0.004(2) C16 0.025(2) 0.027(2) 0.026(2) -0.0009(18) 0.0048(18) -0.0006(18) C17 0.014(2) 0.031(2) 0.027(2) 0.0020(18) -0.0019(18) -0.0044(17) C18 0.035(3) 0.036(3) 0.048(3) 0.011(2) 0.017(2) 0.011(2) C19 0.035(3) 0.037(3) 0.068(4) 0.019(3) 0.018(3) 0.010(2) C20 0.034(3) 0.041(3) 0.047(3) 0.023(2) 0.001(2) -0.002(2) C21 0.046(3) 0.044(3) 0.033(3) 0.006(2) 0.017(2) -0.008(2) C22 0.038(3) 0.030(2) 0.032(2) 0.0017(19) 0.008(2) -0.004(2) C23 0.027(2) 0.026(2) 0.022(2) 0.0048(17) 0.0080(18) -0.0027(18) C24 0.033(3) 0.049(3) 0.050(3) -0.009(2) -0.004(2) 0.006(2) C25 0.046(3) 0.052(3) 0.052(3) -0.008(3) 0.006(3) 0.022(3) C26 0.063(4) 0.033(3) 0.037(3) 0.001(2) 0.012(3) 0.002(3) C27 0.044(3) 0.040(3) 0.033(3) -0.007(2) 0.004(2) -0.007(2) C28 0.031(3) 0.033(2) 0.029(2) 0.0013(19) 0.000(2) -0.003(2) C29 0.024(2) 0.017(2) 0.028(2) 0.0031(16) 0.0050(18) -0.0024(17) C30 0.021(2) 0.018(2) 0.024(2) -0.0032(16) -0.0006(17) -0.0074(16) C31 0.020(2) 0.0149(19) 0.024(2) -0.0002(16) 0.0017(17) -0.0013(16) C32 0.022(2) 0.027(2) 0.028(2) 0.0049(18) 0.0047(18) -0.0004(18) C33 0.022(2) 0.027(2) 0.034(2) 0.0075(19) -0.0023(19) 0.0035(18) C34 0.017(2) 0.024(2) 0.042(3) -0.0034(19) 0.0059(19) 0.0025(17) C35 0.024(2) 0.039(3) 0.024(2) -0.0006(19) 0.0078(19) 0.004(2) C36 0.026(2) 0.033(2) 0.024(2) 0.0054(18) 0.0010(19) 0.0024(19) C37 0.016(2) 0.020(2) 0.025(2) -0.0002(16) 0.0000(17) 0.0041(16) C38 0.022(2) 0.026(2) 0.019(2) 0.0033(17) 0.0020(17) 0.0011(17) C39 0.021(2) 0.038(3) 0.031(2) 0.001(2) -0.0044(19) -0.0044(19) C40 0.036(3) 0.039(3) 0.026(2) 0.005(2) -0.008(2) 0.003(2) C41 0.042(3) 0.030(2) 0.031(2) 0.0091(19) 0.000(2) -0.005(2) C42 0.034(3) 0.019(2) 0.031(2) 0.0030(18) -0.004(2) -0.0037(18) C43 0.026(2) 0.026(2) 0.0140(19) 0.0028(16) 0.0026(17) 0.0019(17) C44 0.023(2) 0.035(2) 0.022(2) -0.0026(18) 0.0023(18) 0.0006(19) C45 0.029(3) 0.056(3) 0.029(2) 0.003(2) -0.001(2) 0.011(2) C46 0.043(3) 0.070(4) 0.031(3) 0.002(2) 0.008(2) 0.034(3) C47 0.058(3) 0.042(3) 0.034(3) -0.011(2) 0.001(2) 0.023(3) C48 0.038(3) 0.035(3) 0.023(2) -0.0060(19) -0.004(2) 0.006(2) C49 0.019(2) 0.021(2) 0.023(2) -0.0020(16) -0.0024(17) 0.0029(16) C50 0.030(3) 0.027(2) 0.028(2) 0.0007(18) -0.0012(19) -0.0065(19) C51 0.043(3) 0.032(2) 0.026(2) 0.0080(19) -0.001(2) -0.010(2) C52 0.043(3) 0.040(3) 0.024(2) -0.001(2) -0.011(2) -0.002(2) C53 0.050(3) 0.036(3) 0.036(3) 0.001(2) -0.019(2) -0.012(2) C54 0.049(3) 0.023(2) 0.027(2) 0.0049(18) -0.010(2) -0.015(2) C55 0.061(4) 0.091(5) 0.065(4) 0.022(4) -0.011(3) -0.031(4) C56 0.111(7) 0.089(6) 0.088(5) -0.016(4) 0.004(5) -0.043(5) C57 0.044(3) 0.073(4) 0.066(4) 0.035(3) 0.023(3) 0.012(3) C58 0.089(5) 0.053(4) 0.079(4) 0.002(3) 0.021(4) 0.014(4) C2A 0.027(9) 0.013(7) 0.025(9) 0.008(6) 0.004(7) -0.010(6) C1A 0.077(16) 0.069(16) 0.069(16) 0.001(7) 0.007(7) -0.003(7) P1A 0.009(3) 0.011(3) 0.019(3) -0.006(2) 0.005(2) 0.005(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 C1A 1.94(3) . ? Pt1 C1 2.075(13) . ? Pt1 P2 2.2568(12) . ? Pt1 P3 2.2618(12) . ? Pt1 P1A 2.312(10) . ? Pt1 P1 2.368(2) . ? P1 C1 1.734(12) . ? P1 Pt2 2.347(2) . ? O1 C57 1.412(6) . ? O1 C55 1.430(7) . ? C1 C2 1.537(10) . ? C1 Pt2 2.059(11) . ? Pt2 C1A 2.14(3) . ? Pt2 P4 2.2498(10) . ? Pt2 P5 2.2611(10) . ? Pt2 P1A 2.387(9) . ? P2 C5 1.819(4) . ? P2 C11 1.838(4) . ? P2 C3 1.852(4) . ? P3 C23 1.822(4) . ? P3 C17 1.830(4) . ? P3 C4 1.845(4) . ? C3 C4 1.531(5) . ? P4 C37 1.824(4) . ? P4 C31 1.837(4) . ? P4 C29 1.851(4) . ? P5 C49 1.828(4) . ? P5 C43 1.834(4) . ? P5 C30 1.854(4) . ? C5 C6 1.390(5) . ? C5 C10 1.394(6) . ? C6 C7 1.391(6) . ? C7 C8 1.378(7) . ? C8 C9 1.373(6) . ? C9 C10 1.393(6) . ? C11 C16 1.388(5) . ? C11 C12 1.389(5) . ? C12 C13 1.385(6) . ? C13 C14 1.376(6) . ? C14 C15 1.387(6) . ? C15 C16 1.396(6) . ? C17 C18 1.381(6) . ? C17 C22 1.393(6) . ? C18 C19 1.382(6) . ? C19 C20 1.370(6) . ? C20 C21 1.374(6) . ? C21 C22 1.381(6) . ? C23 C24 1.388(6) . ? C23 C28 1.391(6) . ? C24 C25 1.399(6) . ? C25 C26 1.374(7) . ? C26 C27 1.376(7) . ? C27 C28 1.379(6) . ? C29 C30 1.534(5) . ? C31 C32 1.388(5) . ? C31 C36 1.396(5) . ? C32 C33 1.388(6) . ? C33 C34 1.384(6) . ? C34 C35 1.377(6) . ? C35 C36 1.388(6) . ? C37 C38 1.388(5) . ? C37 C42 1.395(5) . ? C38 C39 1.391(5) . ? C39 C40 1.375(6) . ? C40 C41 1.384(6) . ? C41 C42 1.379(5) . ? C43 C44 1.387(5) . ? C43 C48 1.389(5) . ? C44 C45 1.387(6) . ? C45 C46 1.376(7) . ? C46 C47 1.387(7) . ? C47 C48 1.389(6) . ? C49 C54 1.378(5) . ? C49 C50 1.391(5) . ? C50 C51 1.384(5) . ? C51 C52 1.375(6) . ? C52 C53 1.374(6) . ? C53 C54 1.380(6) . ? C55 C56 1.469(9) . ? C57 C58 1.480(8) . ? C2A C1A 1.539(17) . ? C1A P1A 1.755(17) . ? 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 C1A Pt1 C1 45.2(7) . . ? C1A Pt1 P2 162.1(6) . . ? C1 Pt1 P2 117.7(3) . . ? C1A Pt1 P3 110.3(6) . . ? C1 Pt1 P3 155.5(3) . . ? P2 Pt1 P3 86.75(4) . . ? C1A Pt1 P1A 47.8(6) . . ? C1 Pt1 P1A 8.4(5) . . ? P2 Pt1 P1A 114.5(2) . . ? P3 Pt1 P1A 156.3(2) . . ? C1A Pt1 P1 5.8(10) . . ? C1 Pt1 P1 45.4(3) . . ? P2 Pt1 P1 159.41(5) . . ? P3 Pt1 P1 110.35(5) . . ? P1A Pt1 P1 46.8(2) . . ? C1 P1 Pt2 58.3(4) . . ? C1 P1 Pt1 58.4(5) . . ? Pt2 P1 Pt1 80.34(7) . . ? C57 O1 C55 113.6(5) . . ? C2 C1 P1 137.9(8) . . ? C2 C1 Pt2 122.6(8) . . ? P1 C1 Pt2 75.9(4) . . ? C2 C1 Pt1 131.3(9) . . ? P1 C1 Pt1 76.3(5) . . ? Pt2 C1 Pt1 94.7(4) . . ? C1 Pt2 C1A 43.2(7) . . ? C1 Pt2 P4 108.4(3) . . ? C1A Pt2 P4 151.6(5) . . ? C1 Pt2 P5 165.0(3) . . ? C1A Pt2 P5 121.9(5) . . ? P4 Pt2 P5 86.43(4) . . ? C1 Pt2 P1 45.8(3) . . ? C1A Pt2 P1 11.1(8) . . ? P4 Pt2 P1 150.55(5) . . ? P5 Pt2 P1 119.33(5) . . ? C1 Pt2 P1A 5.9(6) . . ? C1A Pt2 P1A 45.2(5) . . ? P4 Pt2 P1A 106.4(2) . . ? P5 Pt2 P1A 164.9(2) . . ? P1 Pt2 P1A 46.3(2) . . ? C5 P2 C11 102.26(18) . . ? C5 P2 C3 104.99(19) . . ? C11 P2 C3 100.29(18) . . ? C5 P2 Pt1 122.16(13) . . ? C11 P2 Pt1 119.93(13) . . ? C3 P2 Pt1 104.23(13) . . ? C23 P3 C17 103.50(18) . . ? C23 P3 C4 105.55(19) . . ? C17 P3 C4 102.95(18) . . ? C23 P3 Pt1 118.89(13) . . ? C17 P3 Pt1 116.46(13) . . ? C4 P3 Pt1 107.90(13) . . ? C4 C3 P2 108.2(3) . . ? C37 P4 C31 105.90(17) . . ? C37 P4 C29 102.89(17) . . ? C31 P4 C29 102.44(18) . . ? C37 P4 Pt2 122.49(13) . . ? C31 P4 Pt2 111.89(12) . . ? C29 P4 Pt2 109.13(13) . . ? C3 C4 P3 108.8(3) . . ? C49 P5 C43 104.09(17) . . ? C49 P5 C30 102.43(18) . . ? C43 P5 C30 102.71(18) . . ? C49 P5 Pt2 123.51(13) . . ? C43 P5 Pt2 115.27(13) . . ? C30 P5 Pt2 106.26(12) . . ? C6 C5 C10 118.0(4) . . ? C6 C5 P2 123.7(3) . . ? C10 C5 P2 118.3(3) . . ? C5 C6 C7 120.7(4) . . ? C8 C7 C6 120.2(4) . . ? C9 C8 C7 120.3(4) . . ? C8 C9 C10 119.5(4) . . ? C9 C10 C5 121.3(4) . . ? C16 C11 C12 118.9(4) . . ? C16 C11 P2 118.4(3) . . ? C12 C11 P2 122.6(3) . . ? C13 C12 C11 120.9(4) . . ? C14 C13 C12 120.1(4) . . ? C13 C14 C15 119.8(4) . . ? C14 C15 C16 120.2(4) . . ? C11 C16 C15 120.1(4) . . ? C18 C17 C22 118.4(4) . . ? C18 C17 P3 118.4(3) . . ? C22 C17 P3 123.2(3) . . ? C17 C18 C19 121.0(4) . . ? C20 C19 C18 120.3(4) . . ? C19 C20 C21 119.4(4) . . ? C20 C21 C22 120.8(4) . . ? C21 C22 C17 120.1(4) . . ? C24 C23 C28 117.9(4) . . ? C24 C23 P3 125.1(3) . . ? C28 C23 P3 117.0(3) . . ? C23 C24 C25 120.7(5) . . ? C26 C25 C24 120.1(5) . . ? C25 C26 C27 119.8(5) . . ? C26 C27 C28 120.2(5) . . ? C27 C28 C23 121.4(4) . . ? C30 C29 P4 110.8(2) . . ? C29 C30 P5 108.9(2) . . ? C32 C31 C36 118.7(4) . . ? C32 C31 P4 116.6(3) . . ? C36 C31 P4 124.7(3) . . ? C31 C32 C33 120.3(4) . . ? C34 C33 C32 120.7(4) . . ? C35 C34 C33 119.3(4) . . ? C34 C35 C36 120.6(4) . . ? C35 C36 C31 120.4(4) . . ? C38 C37 C42 118.9(4) . . ? C38 C37 P4 117.9(3) . . ? C42 C37 P4 123.1(3) . . ? C37 C38 C39 120.2(4) . . ? C40 C39 C38 120.5(4) . . ? C39 C40 C41 119.3(4) . . ? C42 C41 C40 120.7(4) . . ? C41 C42 C37 120.2(4) . . ? C44 C43 C48 119.7(4) . . ? C44 C43 P5 117.9(3) . . ? C48 C43 P5 122.3(3) . . ? C43 C44 C45 119.9(4) . . ? C46 C45 C44 120.8(4) . . ? C45 C46 C47 119.4(4) . . ? C46 C47 C48 120.4(4) . . ? C43 C48 C47 119.8(4) . . ? C54 C49 C50 118.5(4) . . ? C54 C49 P5 123.7(3) . . ? C50 C49 P5 117.8(3) . . ? C51 C50 C49 121.0(4) . . ? C52 C51 C50 119.5(4) . . ? C53 C52 C51 120.0(4) . . ? C52 C53 C54 120.5(4) . . ? C49 C54 C53 120.5(4) . . ? O1 C55 C56 110.2(5) . . ? O1 C57 C58 109.6(5) . . ? C2A C1A P1A 133.9(19) . . ? C2A C1A Pt1 131(2) . . ? P1A C1A Pt1 77.2(10) . . ? C2A C1A Pt2 124(2) . . ? P1A C1A Pt2 74.9(10) . . ? Pt1 C1A Pt2 96.2(10) . . ? C1A P1A Pt1 55.0(11) . . ? C1A P1A Pt2 59.9(11) . . ? Pt1 P1A Pt2 80.7(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.689 _refine_diff_density_min -0.802 _refine_diff_density_rms 0.111 # Attachment 'compound4.CIF' data_compound4 _database_code_depnum_ccdc_archive 'CCDC 609153' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H63 P5 Pt2' _chemical_formula_weight 920.79 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 orthorhombic _symmetry_space_group_name_H-M Pcab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' 'x+1/2, -y, -z+1/2' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' '-x-1/2, y, z-1/2' 'x-1/2, -y-1/2, z' _cell_length_a 14.460(3) _cell_length_b 20.302(4) _cell_length_c 24.218(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7110(2) _cell_formula_units_Z 8 _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 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.720 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3600 _exptl_absorpt_coefficient_mu 8.100 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.140 _exptl_absorpt_correction_T_max 0.376 _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 13229 _diffrn_reflns_av_R_equivalents 0.0268 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6945 _reflns_number_gt 6011 _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. During the course of refinement, the PCMe ligand was found to be disordered over two sites. This disorder was successfuly modelled. The largest electron density peak and hole in the final difference map were located near to Pt1 and Pt2 respectively. ; _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^)+(0.0283P)^2^+72.8915P] 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 6945 _refine_ls_number_parameters 340 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.0575 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.1147 _refine_ls_wR_factor_gt 0.1112 _refine_ls_goodness_of_fit_ref 1.245 _refine_ls_restrained_S_all 1.245 _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 0.22710(2) 0.133966(16) 0.252207(12) 0.02965(11) Uani 1 1 d . . . Pt2 Pt 0.23531(2) 0.133926(16) 0.382503(12) 0.02710(10) Uani 1 1 d . . . P1 P 0.2888(4) 0.2119(3) 0.3166(2) 0.0312(17) Uani 0.555(12) 1 d PD A 1 P2 P 0.23789(18) 0.03415(12) 0.21053(10) 0.0375(5) Uani 1 1 d . A . P3 P 0.12559(16) 0.19328(12) 0.20084(9) 0.0342(5) Uani 1 1 d . A . P4 P 0.26865(17) 0.04718(12) 0.43783(9) 0.0351(5) Uani 1 1 d . A . P5 P 0.12681(15) 0.19424(11) 0.42801(9) 0.0303(5) Uani 1 1 d . A . C1 C 0.334(2) 0.1338(12) 0.3172(18) 0.019(7) Uani 0.555(12) 1 d PDU A 1 C2 C 0.4264(12) 0.0983(10) 0.3155(7) 0.045(5) Uani 0.555(12) 1 d PD A 1 H2A H 0.4669 0.1197 0.2885 0.068 Uiso 0.555(12) 1 calc PR A 1 H2B H 0.4167 0.0522 0.3048 0.068 Uiso 0.555(12) 1 calc PR A 1 H2C H 0.4553 0.1000 0.3521 0.068 Uiso 0.555(12) 1 calc PR A 1 C3 C 0.2244(9) -0.0338(5) 0.2599(5) 0.061(3) Uani 1 1 d . . . H3A H 0.2296 -0.0761 0.2399 0.073 Uiso 1 1 calc R A . H3B H 0.2753 -0.0318 0.2872 0.073 Uiso 1 1 calc R . . C4 C 0.1339(11) -0.0320(7) 0.2898(5) 0.078(4) Uani 1 1 d . A . H4A H 0.1316 0.0071 0.3136 0.117 Uiso 1 1 calc R . . H4B H 0.1276 -0.0717 0.3125 0.117 Uiso 1 1 calc R . . H4C H 0.0832 -0.0302 0.2630 0.117 Uiso 1 1 calc R . . C5 C 0.1594(7) 0.0098(5) 0.1548(4) 0.043(2) Uani 1 1 d . . . H5A H 0.0955 0.0120 0.1693 0.052 Uiso 1 1 calc R A . H5B H 0.1644 0.0431 0.1251 0.052 Uiso 1 1 calc R . . C6 C 0.1729(10) -0.0583(6) 0.1286(5) 0.069(4) Uani 1 1 d . A . H6A H 0.2324 -0.0596 0.1092 0.103 Uiso 1 1 calc R . . H6B H 0.1228 -0.0668 0.1023 0.103 Uiso 1 1 calc R . . H6C H 0.1721 -0.0921 0.1575 0.103 Uiso 1 1 calc R . . C7 C 0.3493(7) 0.0181(6) 0.1809(4) 0.057(3) Uani 1 1 d . . . H7A H 0.3971 0.0225 0.2099 0.069 Uiso 1 1 calc R A . H7B H 0.3510 -0.0279 0.1673 0.069 Uiso 1 1 calc R . . C8 C 0.3725(9) 0.0645(7) 0.1333(5) 0.073(4) Uani 1 1 d . A . H8A H 0.3199 0.0668 0.1079 0.110 Uiso 1 1 calc R . . H8B H 0.4269 0.0480 0.1136 0.110 Uiso 1 1 calc R . . H8C H 0.3857 0.1085 0.1479 0.110 Uiso 1 1 calc R . . C9 C 0.1785(8) 0.2227(6) 0.1357(4) 0.057(3) Uani 1 1 d . . . H9A H 0.2010 0.1845 0.1142 0.069 Uiso 1 1 calc R A . H9B H 0.1311 0.2458 0.1134 0.069 Uiso 1 1 calc R . . C10 C 0.2602(9) 0.2702(8) 0.1473(6) 0.085(5) Uani 1 1 d . A . H10A H 0.2366 0.3110 0.1636 0.127 Uiso 1 1 calc R . . H10B H 0.2920 0.2803 0.1125 0.127 Uiso 1 1 calc R . . H10C H 0.3037 0.2493 0.1729 0.127 Uiso 1 1 calc R . . C11 C 0.0227(7) 0.1533(6) 0.1726(5) 0.058(3) Uani 1 1 d . . . H11A H -0.0133 0.1857 0.1510 0.069 Uiso 1 1 calc R A . H11B H 0.0419 0.1175 0.1473 0.069 Uiso 1 1 calc R . . C12 C -0.0389(9) 0.1244(8) 0.2183(7) 0.097(5) Uani 1 1 d . A . H12A H -0.0024 0.0944 0.2412 0.146 Uiso 1 1 calc R . . H12B H -0.0904 0.1003 0.2015 0.146 Uiso 1 1 calc R . . H12C H -0.0632 0.1602 0.2412 0.146 Uiso 1 1 calc R . . C13 C 0.0800(9) 0.2675(5) 0.2313(5) 0.061(3) Uani 1 1 d . . . H13A H 0.0470 0.2552 0.2656 0.073 Uiso 1 1 calc R A . H13B H 0.1328 0.2957 0.2421 0.073 Uiso 1 1 calc R . . C14 C 0.0146(9) 0.3087(6) 0.1960(6) 0.074(4) Uani 1 1 d . A . H14A H 0.0471 0.3238 0.1629 0.111 Uiso 1 1 calc R . . H14B H -0.0066 0.3469 0.2173 0.111 Uiso 1 1 calc R . . H14C H -0.0388 0.2818 0.1852 0.111 Uiso 1 1 calc R . . C15 C 0.3331(7) -0.0204(5) 0.4071(4) 0.048(3) Uani 1 1 d . . . H15A H 0.2944 -0.0394 0.3774 0.058 Uiso 1 1 calc R A . H15B H 0.3887 -0.0015 0.3893 0.058 Uiso 1 1 calc R . . C16 C 0.3651(11) -0.0769(6) 0.4436(5) 0.079(4) Uani 1 1 d . A . H16A H 0.4116 -0.0609 0.4697 0.118 Uiso 1 1 calc R . . H16B H 0.3921 -0.1117 0.4206 0.118 Uiso 1 1 calc R . . H16C H 0.3121 -0.0947 0.4640 0.118 Uiso 1 1 calc R . . C17 C 0.3428(9) 0.0756(6) 0.4955(5) 0.066(3) Uani 1 1 d . . . H17A H 0.3043 0.1017 0.5212 0.079 Uiso 1 1 calc R A . H17B H 0.3652 0.0365 0.5159 0.079 Uiso 1 1 calc R . . C18 C 0.4215(11) 0.1147(8) 0.4800(7) 0.105(6) Uani 1 1 d . A . H18A H 0.4645 0.0877 0.4584 0.157 Uiso 1 1 calc R . . H18B H 0.4527 0.1308 0.5133 0.157 Uiso 1 1 calc R . . H18C H 0.4010 0.1522 0.4577 0.157 Uiso 1 1 calc R . . C19 C 0.1806(8) 0.0023(5) 0.4784(4) 0.055(3) Uani 1 1 d . . . H19A H 0.2122 -0.0320 0.5006 0.066 Uiso 1 1 calc R A . H19B H 0.1513 0.0335 0.5044 0.066 Uiso 1 1 calc R . . C20 C 0.1059(10) -0.0301(7) 0.4447(6) 0.084(4) Uani 1 1 d . A . H20A H 0.0740 0.0032 0.4225 0.126 Uiso 1 1 calc R . . H20B H 0.0614 -0.0515 0.4695 0.126 Uiso 1 1 calc R . . H20C H 0.1336 -0.0632 0.4203 0.126 Uiso 1 1 calc R . . C21 C 0.1595(8) 0.2800(5) 0.4370(5) 0.053(3) Uani 1 1 d . . . H21A H 0.1642 0.3012 0.4003 0.064 Uiso 1 1 calc R A . H21B H 0.1105 0.3030 0.4580 0.064 Uiso 1 1 calc R . . C22 C 0.2526(8) 0.2879(6) 0.4677(6) 0.065(3) Uani 1 1 d . A . H22A H 0.2466 0.2707 0.5053 0.097 Uiso 1 1 calc R . . H22B H 0.2693 0.3346 0.4691 0.097 Uiso 1 1 calc R . . H22C H 0.3008 0.2634 0.4480 0.097 Uiso 1 1 calc R . . C23 C 0.0927(8) 0.1689(6) 0.4971(4) 0.052(3) Uani 1 1 d . . . H23A H 0.0663 0.1240 0.4944 0.062 Uiso 1 1 calc R A . H23B H 0.1494 0.1656 0.5198 0.062 Uiso 1 1 calc R . . C24 C 0.0220(9) 0.2128(7) 0.5289(5) 0.072(4) Uani 1 1 d . A . H24A H 0.0479 0.2570 0.5338 0.109 Uiso 1 1 calc R . . H24B H 0.0093 0.1933 0.5651 0.109 Uiso 1 1 calc R . . H24C H -0.0356 0.2158 0.5077 0.109 Uiso 1 1 calc R . . C25 C 0.0163(7) 0.2036(7) 0.3925(5) 0.062(3) Uani 1 1 d . . . H25A H -0.0245 0.2323 0.4148 0.074 Uiso 1 1 calc R A . H25B H 0.0269 0.2257 0.3566 0.074 Uiso 1 1 calc R . . C26 C -0.0333(10) 0.1373(7) 0.3821(6) 0.087(4) Uani 1 1 d U A . H26A H 0.0065 0.1087 0.3598 0.130 Uiso 1 1 calc R . . H26B H -0.0914 0.1453 0.3625 0.130 Uiso 1 1 calc R . . H26C H -0.0463 0.1160 0.4176 0.130 Uiso 1 1 calc R . . P1A P 0.3475(9) 0.1227(7) 0.3133(6) 0.040(3) Uani 0.445(12) 1 d PD A 2 C1A C 0.2748(18) 0.1909(10) 0.3142(14) 0.032(8) Uani 0.445(12) 1 d PDU A 2 C2A C 0.2843(17) 0.2654(10) 0.3145(8) 0.043(6) Uani 0.445(12) 1 d PD A 2 H2A1 H 0.3251 0.2788 0.3448 0.065 Uiso 0.445(12) 1 calc PR A 2 H2A2 H 0.2232 0.2855 0.3195 0.065 Uiso 0.445(12) 1 calc PR A 2 H2A3 H 0.3106 0.2800 0.2793 0.065 Uiso 0.445(12) 1 calc PR A 2 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 0.0371(2) 0.03131(19) 0.02049(17) 0.00030(13) 0.00013(12) 0.00295(14) Pt2 0.03158(18) 0.02883(18) 0.02089(17) 0.00094(12) 0.00078(12) -0.00212(14) P1 0.038(3) 0.031(4) 0.024(2) 0.002(2) 0.0012(18) -0.008(2) P2 0.0492(14) 0.0349(12) 0.0284(12) -0.0027(10) -0.0039(10) 0.0101(11) P3 0.0373(12) 0.0367(13) 0.0288(11) 0.0013(10) -0.0044(9) 0.0046(10) P4 0.0443(13) 0.0364(12) 0.0246(11) 0.0042(9) -0.0017(10) -0.0023(10) P5 0.0317(11) 0.0303(12) 0.0288(11) -0.0008(9) 0.0035(9) -0.0010(9) C1 0.019(8) 0.022(7) 0.015(8) 0.000(4) -0.006(5) -0.001(4) C2 0.034(10) 0.072(13) 0.030(9) -0.002(9) 0.007(7) 0.002(9) C3 0.097(10) 0.030(5) 0.056(7) 0.001(5) -0.018(7) 0.012(6) C4 0.112(12) 0.064(8) 0.058(8) 0.022(7) 0.010(8) -0.020(8) C5 0.054(6) 0.037(5) 0.039(5) -0.004(4) -0.005(5) 0.002(5) C6 0.112(11) 0.043(7) 0.052(7) -0.013(5) -0.023(7) 0.006(7) C7 0.046(6) 0.076(8) 0.050(6) -0.023(6) 0.000(5) 0.010(6) C8 0.064(8) 0.110(11) 0.045(7) -0.019(7) 0.010(6) -0.003(8) C9 0.063(7) 0.071(8) 0.038(6) 0.010(5) -0.002(5) 0.028(6) C10 0.062(8) 0.110(12) 0.082(10) 0.048(9) 0.007(7) -0.008(8) C11 0.041(6) 0.053(7) 0.079(8) -0.005(6) -0.016(5) 0.007(5) C12 0.044(7) 0.103(12) 0.145(15) 0.022(11) -0.006(8) -0.039(8) C13 0.086(9) 0.046(7) 0.051(7) -0.003(5) 0.005(6) 0.014(6) C14 0.082(9) 0.044(7) 0.097(10) -0.013(7) -0.009(8) 0.030(6) C15 0.051(6) 0.055(6) 0.039(6) 0.011(5) 0.010(5) 0.015(5) C16 0.109(11) 0.061(8) 0.066(8) 0.012(7) -0.002(8) 0.043(8) C17 0.076(8) 0.068(8) 0.054(7) 0.013(6) -0.027(6) 0.005(7) C18 0.083(10) 0.111(13) 0.120(13) 0.036(10) -0.055(10) -0.042(9) C19 0.075(8) 0.052(6) 0.037(6) 0.015(5) 0.009(5) 0.011(6) C20 0.085(10) 0.078(10) 0.089(10) 0.023(8) 0.010(8) -0.033(8) C21 0.059(7) 0.037(6) 0.064(7) -0.005(5) 0.015(6) -0.001(5) C22 0.057(7) 0.054(7) 0.083(9) -0.029(6) 0.005(6) -0.009(6) C23 0.061(7) 0.050(6) 0.044(6) 0.003(5) 0.015(5) 0.014(5) C24 0.089(9) 0.079(9) 0.049(7) 0.003(6) 0.030(6) 0.025(7) C25 0.040(6) 0.095(10) 0.050(7) -0.014(6) -0.009(5) 0.006(6) C26 0.077(6) 0.088(7) 0.095(7) -0.024(6) -0.005(5) -0.009(5) P1A 0.041(6) 0.057(6) 0.022(4) 0.000(4) 0.004(4) 0.001(4) C1A 0.034(9) 0.030(10) 0.031(9) 0.004(5) -0.005(5) 0.001(5) C2A 0.060(15) 0.036(15) 0.032(11) -0.001(9) -0.019(10) -0.021(11) _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 C1A 2.02(3) . ? Pt1 C1 2.21(4) . ? Pt1 P2 2.269(2) . ? Pt1 P3 2.270(2) . ? Pt1 P1A 2.296(15) . ? Pt1 P1 2.394(7) . ? Pt2 C1A 2.10(3) . ? Pt2 C1 2.13(4) . ? Pt2 P4 2.265(2) . ? Pt2 P5 2.275(2) . ? Pt2 P1A 2.345(14) . ? Pt2 P1 2.376(6) . ? P1 C1 1.715(17) . ? P2 C7 1.794(11) . ? P2 C5 1.831(10) . ? P2 C3 1.835(11) . ? P3 C13 1.803(11) . ? P3 C11 1.828(11) . ? P3 C9 1.852(11) . ? P4 C15 1.819(10) . ? P4 C19 1.848(11) . ? P4 C17 1.854(11) . ? P5 C21 1.817(10) . ? P5 C23 1.819(10) . ? P5 C25 1.825(10) . ? C1 C2 1.518(17) . ? C3 C4 1.496(18) . ? C5 C6 1.534(14) . ? C7 C8 1.526(17) . ? C9 C10 1.550(18) . ? C11 C12 1.536(18) . ? C13 C14 1.524(16) . ? C15 C16 1.519(14) . ? C17 C18 1.437(18) . ? C19 C20 1.505(17) . ? C21 C22 1.545(16) . ? C23 C24 1.560(14) . ? C25 C26 1.544(18) . ? P1A C1A 1.740(17) . ? C1A C2A 1.519(17) . ? 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 C1A Pt1 C1 39.7(9) . . ? C1A Pt1 P2 145.0(6) . . ? C1 Pt1 P2 105.5(6) . . ? C1A Pt1 P3 109.0(6) . . ? C1 Pt1 P3 147.7(6) . . ? P2 Pt1 P3 105.93(9) . . ? C1A Pt1 P1A 47.0(6) . . ? C1 Pt1 P1A 7.6(9) . . ? P2 Pt1 P1A 98.3(3) . . ? P3 Pt1 P1A 153.7(3) . . ? C1A Pt1 P1 7.5(9) . . ? C1 Pt1 P1 43.5(5) . . ? P2 Pt1 P1 148.66(15) . . ? P3 Pt1 P1 104.34(15) . . ? P1A Pt1 P1 50.5(4) . . ? C1A Pt2 C1 39.9(9) . . ? C1A Pt2 P4 146.9(6) . . ? C1 Pt2 P4 107.2(6) . . ? C1A Pt2 P5 105.8(6) . . ? C1 Pt2 P5 145.3(6) . . ? P4 Pt2 P5 106.19(8) . . ? C1A Pt2 P1A 45.7(6) . . ? C1 Pt2 P1A 5.9(8) . . ? P4 Pt2 P1A 101.5(3) . . ? P5 Pt2 P1A 151.2(3) . . ? C1A Pt2 P1 9.9(8) . . ? C1 Pt2 P1 44.3(6) . . ? P4 Pt2 P1 147.74(15) . . ? P5 Pt2 P1 101.03(15) . . ? P1A Pt2 P1 50.2(4) . . ? C1 P1 Pt2 60.2(13) . . ? C1 P1 Pt1 62.4(13) . . ? Pt2 P1 Pt1 82.9(2) . . ? C7 P2 C5 102.3(5) . . ? C7 P2 C3 102.7(6) . . ? C5 P2 C3 102.2(5) . . ? C7 P2 Pt1 113.7(4) . . ? C5 P2 Pt1 121.8(3) . . ? C3 P2 Pt1 112.0(4) . . ? C13 P3 C11 103.1(6) . . ? C13 P3 C9 103.3(5) . . ? C11 P3 C9 99.3(6) . . ? C13 P3 Pt1 117.1(4) . . ? C11 P3 Pt1 119.7(4) . . ? C9 P3 Pt1 111.8(3) . . ? C15 P4 C19 101.4(5) . . ? C15 P4 C17 104.3(6) . . ? C19 P4 C17 98.7(5) . . ? C15 P4 Pt2 117.0(3) . . ? C19 P4 Pt2 123.5(4) . . ? C17 P4 Pt2 109.1(4) . . ? C21 P5 C23 103.4(5) . . ? C21 P5 C25 100.6(6) . . ? C23 P5 C25 103.0(5) . . ? C21 P5 Pt2 113.2(4) . . ? C23 P5 Pt2 118.7(3) . . ? C25 P5 Pt2 115.5(4) . . ? C2 C1 P1 141(2) . . ? C2 C1 Pt2 128(2) . . ? P1 C1 Pt2 75.5(11) . . ? C2 C1 Pt1 127(2) . . ? P1 C1 Pt1 74.1(11) . . ? Pt2 C1 Pt1 93.5(12) . . ? C4 C3 P2 113.0(8) . . ? C6 C5 P2 118.0(8) . . ? C8 C7 P2 112.8(9) . . ? C10 C9 P3 111.3(8) . . ? C12 C11 P3 111.8(9) . . ? C14 C13 P3 117.1(8) . . ? C16 C15 P4 119.2(8) . . ? C18 C17 P4 115.6(10) . . ? C20 C19 P4 115.0(8) . . ? C22 C21 P5 112.6(8) . . ? C24 C23 P5 118.0(8) . . ? C26 C25 P5 113.1(10) . . ? C1A P1A Pt1 58.0(11) . . ? C1A P1A Pt2 59.6(11) . . ? Pt1 P1A Pt2 85.7(4) . . ? C2A C1A P1A 138(2) . . ? C2A C1A Pt1 127(2) . . ? P1A C1A Pt1 74.9(10) . . ? C2A C1A Pt2 125(2) . . ? P1A C1A Pt2 74.7(10) . . ? Pt1 C1A Pt2 100.2(11) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.533 _refine_diff_density_min -2.424 _refine_diff_density_rms 0.198 # Attachment 'compound5.CIF' data_compound5 _database_code_depnum_ccdc_archive 'CCDC 609154' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H77 P3 Pt' _chemical_formula_weight 906.07 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 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 11.466(2) _cell_length_b 9.938(2) _cell_length_c 41.029(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.56(3) _cell_angle_gamma 90.00 _cell_volume 4675.0(16) _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 red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.287 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1880 _exptl_absorpt_coefficient_mu 3.131 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.508 _exptl_absorpt_correction_T_max 0.650 _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 15312 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_sigmaI/netI 0.0397 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8153 _reflns_number_gt 7085 _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. During the course of refinement, the PCMe ligand was found to be disordered over two sites. This disorder was successfuly modelled. ; _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^)+(0.0251P)^2^+4.1827P] 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 8153 _refine_ls_number_parameters 458 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0331 _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0665 _refine_ls_wR_factor_gt 0.0641 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 0.790239(10) -0.032018(14) 0.120626(3) 0.02710(6) Uani 1 1 d . . . P1 P 0.6401(3) -0.1715(2) 0.10044(6) 0.0391(7) Uani 0.550(5) 1 d PD A 1 P1A P 0.7455(3) -0.2589(4) 0.13607(9) 0.0406(10) Uiso 0.450(5) 1 d PD A 2 P2 P 0.76130(7) 0.14531(9) 0.08516(2) 0.0289(2) Uani 1 1 d . A . P3 P 0.94146(7) 0.00306(9) 0.15701(2) 0.02666(19) Uani 1 1 d . A . C1 C 0.7228(7) -0.2164(9) 0.1309(2) 0.037(2) Uani 0.550(5) 1 d PDU A 1 C1A C 0.6737(12) -0.1809(15) 0.1079(4) 0.052(5) Uiso 0.450(5) 1 d PD A 2 C2 C 0.7432(6) -0.3328(7) 0.15368(19) 0.0429(19) Uani 0.550(5) 1 d PD A 1 H2A H 0.6860 -0.4038 0.1490 0.064 Uiso 0.550(5) 1 calc PR A 1 H2B H 0.7347 -0.3024 0.1762 0.064 Uiso 0.550(5) 1 calc PR A 1 H2C H 0.8221 -0.3682 0.1506 0.064 Uiso 0.550(5) 1 calc PR A 1 C2A C 0.5762(9) -0.2032(11) 0.0839(3) 0.059(3) Uiso 0.450(5) 1 d PD A 2 H2A1 H 0.5458 -0.2948 0.0864 0.088 Uiso 0.450(5) 1 calc PR A 2 H2A2 H 0.6054 -0.1913 0.0617 0.088 Uiso 0.450(5) 1 calc PR A 2 H2A3 H 0.5138 -0.1382 0.0879 0.088 Uiso 0.450(5) 1 calc PR A 2 C3 C 0.8670(3) 0.2887(3) 0.08301(8) 0.0315(8) Uani 1 1 d . . . H3 H 0.8845 0.3132 0.1062 0.038 Uiso 1 1 calc R A . C4 C 0.9835(3) 0.2440(4) 0.06880(8) 0.0338(8) Uani 1 1 d . A . H4A H 1.0108 0.1623 0.0804 0.041 Uiso 1 1 calc R . . H4B H 0.9721 0.2205 0.0455 0.041 Uiso 1 1 calc R . . C5 C 1.0767(3) 0.3529(4) 0.07167(9) 0.0412(9) Uani 1 1 d . . . H5A H 1.0942 0.3702 0.0950 0.049 Uiso 1 1 calc R A . H5B H 1.1493 0.3215 0.0612 0.049 Uiso 1 1 calc R . . C6 C 1.0361(4) 0.4822(4) 0.05549(11) 0.0476(10) Uani 1 1 d . A . H6A H 1.0274 0.4674 0.0317 0.057 Uiso 1 1 calc R . . H6B H 1.0957 0.5531 0.0589 0.057 Uiso 1 1 calc R . . C7 C 0.9200(4) 0.5296(4) 0.06929(11) 0.0474(10) Uani 1 1 d . . . H7A H 0.9309 0.5545 0.0925 0.057 Uiso 1 1 calc R A . H7B H 0.8935 0.6106 0.0573 0.057 Uiso 1 1 calc R . . C8 C 0.8269(3) 0.4206(4) 0.06657(10) 0.0397(9) Uani 1 1 d . A . H8A H 0.8092 0.4032 0.0433 0.048 Uiso 1 1 calc R . . H8B H 0.7544 0.4525 0.0770 0.048 Uiso 1 1 calc R . . C9 C 0.6219(3) 0.2369(4) 0.09073(8) 0.0329(8) Uani 1 1 d . . . H9 H 0.6178 0.3077 0.0734 0.039 Uiso 1 1 calc R A . C10 C 0.6212(3) 0.3100(4) 0.12368(10) 0.0465(10) Uani 1 1 d . A . H10A H 0.6927 0.3652 0.1260 0.056 Uiso 1 1 calc R . . H10B H 0.6205 0.2432 0.1416 0.056 Uiso 1 1 calc R . . C11 C 0.5124(4) 0.4015(5) 0.12604(13) 0.0670(14) Uani 1 1 d . . . H11A H 0.5115 0.4456 0.1477 0.080 Uiso 1 1 calc R A . H11B H 0.5167 0.4728 0.1092 0.080 Uiso 1 1 calc R . . C12 C 0.4004(4) 0.3215(5) 0.12122(12) 0.0650(13) Uani 1 1 d . A . H12A H 0.3900 0.2599 0.1399 0.078 Uiso 1 1 calc R . . H12B H 0.3332 0.3840 0.1206 0.078 Uiso 1 1 calc R . . C13 C 0.4023(3) 0.2404(4) 0.08999(11) 0.0544(12) Uani 1 1 d . . . H13A H 0.3992 0.3026 0.0712 0.065 Uiso 1 1 calc R A . H13B H 0.3321 0.1825 0.0889 0.065 Uiso 1 1 calc R . . C14 C 0.5113(3) 0.1518(4) 0.08740(10) 0.0424(9) Uani 1 1 d . A . H14A H 0.5105 0.0827 0.1048 0.051 Uiso 1 1 calc R . . H14B H 0.5110 0.1051 0.0661 0.051 Uiso 1 1 calc R . . C15 C 0.7453(3) 0.0725(4) 0.04343(8) 0.0338(8) Uani 1 1 d . . . H15 H 0.6727 0.0170 0.0446 0.041 Uiso 1 1 calc R A . C16 C 0.7223(3) 0.1680(4) 0.01474(8) 0.0417(9) Uani 1 1 d . A . H16A H 0.7929 0.2226 0.0106 0.050 Uiso 1 1 calc R . . H16B H 0.6578 0.2300 0.0202 0.050 Uiso 1 1 calc R . . C17 C 0.6900(4) 0.0866(5) -0.01616(9) 0.0539(11) Uani 1 1 d . . . H17A H 0.6160 0.0378 -0.0125 0.065 Uiso 1 1 calc R A . H17B H 0.6779 0.1491 -0.0347 0.065 Uiso 1 1 calc R . . C18 C 0.7858(5) -0.0140(5) -0.02455(10) 0.0596(13) Uani 1 1 d . A . H18A H 0.7616 -0.0671 -0.0439 0.071 Uiso 1 1 calc R . . H18B H 0.8581 0.0352 -0.0300 0.071 Uiso 1 1 calc R . . C19 C 0.8097(4) -0.1082(4) 0.00385(9) 0.0546(11) Uani 1 1 d . . . H19A H 0.8749 -0.1691 -0.0017 0.065 Uiso 1 1 calc R A . H19B H 0.7398 -0.1642 0.0078 0.065 Uiso 1 1 calc R . . C20 C 0.8413(4) -0.0299(4) 0.03526(9) 0.0412(9) Uani 1 1 d . A . H20A H 0.8509 -0.0938 0.0536 0.049 Uiso 1 1 calc R . . H20B H 0.9162 0.0178 0.0323 0.049 Uiso 1 1 calc R . . C21 C 0.9979(3) 0.1759(3) 0.16416(8) 0.0281(7) Uani 1 1 d . . . H21 H 1.0118 0.2134 0.1419 0.034 Uiso 1 1 calc R A . C22 C 1.1148(3) 0.1942(3) 0.18267(8) 0.0300(8) Uani 1 1 d . A . H22A H 1.1066 0.1613 0.2053 0.036 Uiso 1 1 calc R . . H22B H 1.1759 0.1400 0.1720 0.036 Uiso 1 1 calc R . . C23 C 1.1518(3) 0.3421(4) 0.18324(9) 0.0364(8) Uani 1 1 d . . . H23A H 1.2243 0.3512 0.1963 0.044 Uiso 1 1 calc R A . H23B H 1.1688 0.3716 0.1607 0.044 Uiso 1 1 calc R . . C24 C 1.0583(3) 0.4328(4) 0.19749(10) 0.0399(9) Uani 1 1 d . A . H24A H 1.0481 0.4111 0.2208 0.048 Uiso 1 1 calc R . . H24B H 1.0835 0.5278 0.1959 0.048 Uiso 1 1 calc R . . C25 C 0.9427(3) 0.4148(4) 0.17953(9) 0.0376(8) Uani 1 1 d . . . H25A H 0.9504 0.4475 0.1569 0.045 Uiso 1 1 calc R A . H25B H 0.8822 0.4697 0.1903 0.045 Uiso 1 1 calc R . . C26 C 0.9041(3) 0.2675(3) 0.17900(8) 0.0323(8) Uani 1 1 d . A . H26A H 0.8310 0.2592 0.1661 0.039 Uiso 1 1 calc R . . H26B H 0.8879 0.2376 0.2015 0.039 Uiso 1 1 calc R . . C27 C 0.9024(3) -0.0689(4) 0.19758(8) 0.0348(8) Uani 1 1 d . . . H27 H 0.8970 -0.1679 0.1934 0.042 Uiso 1 1 calc R A . C28 C 0.9879(3) -0.0581(5) 0.22575(10) 0.0480(10) Uani 1 1 d . A . H28A H 0.9909 0.0362 0.2335 0.058 Uiso 1 1 calc R . . H28B H 1.0668 -0.0832 0.2183 0.058 Uiso 1 1 calc R . . C29 C 0.9524(4) -0.1504(5) 0.25391(10) 0.0555(12) Uani 1 1 d . . . H29A H 1.0091 -0.1415 0.2721 0.067 Uiso 1 1 calc R A . H29B H 0.9525 -0.2453 0.2465 0.067 Uiso 1 1 calc R . . C30 C 0.8300(4) -0.1118(6) 0.26559(10) 0.0610(13) Uani 1 1 d . A . H30A H 0.8058 -0.1747 0.2830 0.073 Uiso 1 1 calc R . . H30B H 0.8323 -0.0201 0.2750 0.073 Uiso 1 1 calc R . . C31 C 0.7434(4) -0.1160(6) 0.23858(10) 0.0615(13) Uani 1 1 d . . . H31A H 0.6675 -0.0830 0.2467 0.074 Uiso 1 1 calc R A . H31B H 0.7327 -0.2105 0.2315 0.074 Uiso 1 1 calc R . . C32 C 0.7793(3) -0.0306(4) 0.20894(9) 0.0395(9) Uani 1 1 d . A . H32A H 0.7228 -0.0450 0.1909 0.047 Uiso 1 1 calc R . . H32B H 0.7777 0.0659 0.2149 0.047 Uiso 1 1 calc R . . C33 C 1.0774(3) -0.0903(3) 0.14711(8) 0.0275(7) Uani 1 1 d . . . H33 H 1.1309 -0.0831 0.1664 0.033 Uiso 1 1 calc R A . C34 C 1.0555(3) -0.2413(4) 0.14079(9) 0.0371(9) Uani 1 1 d . A . H34A H 1.0170 -0.2814 0.1600 0.045 Uiso 1 1 calc R . . H34B H 1.0024 -0.2516 0.1218 0.045 Uiso 1 1 calc R . . C35 C 1.1693(3) -0.3163(4) 0.13425(10) 0.0412(9) Uani 1 1 d . . . H35A H 1.2181 -0.3159 0.1543 0.049 Uiso 1 1 calc R A . H35B H 1.1513 -0.4111 0.1287 0.049 Uiso 1 1 calc R . . C36 C 1.2375(3) -0.2533(4) 0.10653(9) 0.0404(9) Uani 1 1 d . A . H36A H 1.3139 -0.2990 0.1046 0.048 Uiso 1 1 calc R . . H36B H 1.1942 -0.2663 0.0858 0.048 Uiso 1 1 calc R . . C37 C 1.2569(3) -0.1042(4) 0.11224(8) 0.0342(8) Uani 1 1 d . . . H37A H 1.2962 -0.0647 0.0931 0.041 Uiso 1 1 calc R A . H37B H 1.3084 -0.0916 0.1315 0.041 Uiso 1 1 calc R . . C38 C 1.1412(3) -0.0313(4) 0.11780(8) 0.0320(8) Uani 1 1 d . A . H38A H 1.1563 0.0656 0.1216 0.038 Uiso 1 1 calc R . . H38B H 1.0913 -0.0397 0.0981 0.038 Uiso 1 1 calc R . . C39 C 1.0296(4) 0.2935(5) 0.31026(11) 0.0590(12) Uani 1 1 d . . . H39 H 0.9636 0.3045 0.3239 0.071 Uiso 1 1 calc R . . C40 C 1.0654(5) 0.1648(5) 0.30161(12) 0.0687(14) Uani 1 1 d . . . H40 H 1.0239 0.0884 0.3091 0.082 Uiso 1 1 calc R . . C41 C 1.1602(4) 0.1488(6) 0.28231(12) 0.0647(13) Uani 1 1 d . . . H41 H 1.1843 0.0609 0.2763 0.078 Uiso 1 1 calc R . . C42 C 1.2197(4) 0.2560(6) 0.27177(11) 0.0621(13) Uani 1 1 d . . . H42 H 1.2869 0.2439 0.2587 0.075 Uiso 1 1 calc R . . C43 C 1.1836(3) 0.3833(5) 0.27986(10) 0.0541(12) Uani 1 1 d . . . H43 H 1.2255 0.4584 0.2717 0.065 Uiso 1 1 calc R . . C44 C 1.0887(4) 0.4055(5) 0.29931(10) 0.0511(11) Uani 1 1 d . . . C45 C 1.0488(5) 0.5434(5) 0.30774(16) 0.0876(19) Uani 1 1 d . . . H45A H 0.9934 0.5751 0.2911 0.131 Uiso 1 1 calc R . . H45B H 1.1160 0.6042 0.3087 0.131 Uiso 1 1 calc R . . H45C H 1.0105 0.5418 0.3290 0.131 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 0.02457(8) 0.03084(9) 0.02588(8) -0.00176(6) -0.00056(5) -0.00257(6) P1 0.0400(15) 0.0383(13) 0.0387(14) -0.0019(9) -0.0100(12) -0.0101(10) P2 0.0269(4) 0.0339(5) 0.0258(5) -0.0032(4) -0.0022(4) 0.0009(4) P3 0.0254(4) 0.0301(5) 0.0244(5) -0.0002(4) -0.0006(3) 0.0002(4) C1 0.030(3) 0.034(4) 0.047(4) 0.001(3) 0.000(3) -0.005(3) C2 0.045(4) 0.029(4) 0.055(5) 0.008(4) -0.008(3) -0.001(3) C3 0.0324(18) 0.035(2) 0.0273(18) -0.0025(15) -0.0044(14) 0.0006(15) C4 0.0339(19) 0.039(2) 0.0285(19) 0.0014(16) -0.0014(15) 0.0032(16) C5 0.031(2) 0.052(2) 0.041(2) 0.0021(19) -0.0030(16) -0.0001(18) C6 0.045(2) 0.045(2) 0.053(3) 0.001(2) 0.000(2) -0.0150(19) C7 0.049(2) 0.031(2) 0.062(3) -0.002(2) -0.005(2) -0.0042(19) C8 0.037(2) 0.031(2) 0.051(2) -0.0003(18) -0.0049(17) 0.0030(16) C9 0.0262(18) 0.039(2) 0.033(2) -0.0028(16) -0.0008(15) 0.0044(15) C10 0.037(2) 0.058(3) 0.044(2) -0.015(2) 0.0013(18) 0.0077(19) C11 0.046(3) 0.077(3) 0.078(3) -0.029(3) 0.002(2) 0.016(2) C12 0.040(2) 0.082(4) 0.073(3) 0.002(3) 0.013(2) 0.014(2) C13 0.030(2) 0.053(3) 0.081(3) 0.012(2) -0.002(2) 0.0026(19) C14 0.031(2) 0.042(2) 0.054(2) 0.0023(19) -0.0045(17) 0.0009(17) C15 0.037(2) 0.040(2) 0.0252(18) -0.0035(15) -0.0036(15) -0.0006(16) C16 0.046(2) 0.048(2) 0.032(2) -0.0017(18) -0.0048(17) 0.0037(19) C17 0.068(3) 0.062(3) 0.032(2) -0.002(2) -0.009(2) 0.005(2) C18 0.090(4) 0.059(3) 0.030(2) -0.011(2) -0.002(2) 0.004(3) C19 0.083(3) 0.044(3) 0.038(2) -0.012(2) 0.008(2) 0.007(2) C20 0.051(2) 0.041(2) 0.031(2) -0.0049(17) 0.0005(17) 0.0040(18) C21 0.0292(18) 0.0307(19) 0.0245(17) -0.0023(14) 0.0007(14) 0.0021(15) C22 0.0285(18) 0.034(2) 0.0277(18) -0.0042(15) -0.0021(14) -0.0008(15) C23 0.036(2) 0.037(2) 0.036(2) 0.0011(17) -0.0013(16) -0.0076(16) C24 0.046(2) 0.033(2) 0.041(2) -0.0076(17) 0.0032(18) -0.0056(17) C25 0.045(2) 0.036(2) 0.033(2) -0.0047(17) 0.0037(16) 0.0059(18) C26 0.0319(19) 0.036(2) 0.0290(19) -0.0035(16) -0.0011(15) 0.0041(16) C27 0.0334(19) 0.044(2) 0.0270(19) 0.0048(16) 0.0039(15) 0.0041(16) C28 0.038(2) 0.066(3) 0.040(2) 0.010(2) 0.0019(18) -0.007(2) C29 0.048(2) 0.082(3) 0.037(2) 0.024(2) -0.0017(19) 0.000(2) C30 0.049(3) 0.091(4) 0.044(3) 0.020(2) 0.009(2) -0.011(3) C31 0.045(2) 0.096(4) 0.044(3) 0.006(2) 0.012(2) -0.011(3) C32 0.033(2) 0.052(2) 0.033(2) 0.0040(18) 0.0030(16) -0.0002(18) C33 0.0249(16) 0.0293(18) 0.0283(18) -0.0012(15) -0.0013(14) -0.0010(14) C34 0.0315(19) 0.032(2) 0.048(2) -0.0004(17) -0.0003(17) -0.0001(16) C35 0.043(2) 0.029(2) 0.052(2) -0.0008(18) 0.0043(18) 0.0054(17) C36 0.041(2) 0.036(2) 0.044(2) -0.0034(18) 0.0077(18) 0.0084(17) C37 0.0348(19) 0.041(2) 0.0272(18) -0.0005(16) 0.0081(15) 0.0031(17) C38 0.0344(19) 0.034(2) 0.0279(19) 0.0022(15) 0.0055(15) 0.0032(16) C39 0.041(2) 0.083(4) 0.053(3) 0.006(3) 0.005(2) 0.000(2) C40 0.073(3) 0.066(3) 0.066(3) 0.018(3) -0.004(3) -0.017(3) C41 0.065(3) 0.068(3) 0.061(3) -0.007(3) -0.013(3) 0.012(3) C42 0.047(3) 0.097(4) 0.043(3) -0.015(3) -0.001(2) 0.001(3) C43 0.038(2) 0.084(4) 0.040(2) 0.009(2) -0.0012(18) -0.014(2) C44 0.043(2) 0.063(3) 0.047(3) 0.005(2) -0.0160(19) 0.002(2) C45 0.068(4) 0.073(4) 0.121(5) -0.011(3) -0.032(3) 0.012(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 C1 2.034(8) . ? Pt1 C1A 2.057(15) . ? Pt1 P3 2.3035(11) . ? Pt1 P2 2.3072(10) . ? Pt1 P1 2.354(3) . ? Pt1 P1A 2.399(4) . ? P1 C1 1.623(9) . ? P1A C1A 1.611(12) . ? P2 C9 1.855(3) . ? P2 C15 1.866(3) . ? P2 C3 1.873(4) . ? P3 C21 1.858(3) . ? P3 C33 1.862(3) . ? P3 C27 1.870(3) . ? C1 C2 1.505(11) . ? C1A C2A 1.499(13) . ? C3 C4 1.529(5) . ? C3 C8 1.543(5) . ? C4 C5 1.525(5) . ? C5 C6 1.518(6) . ? C6 C7 1.527(6) . ? C7 C8 1.524(5) . ? C9 C14 1.529(5) . ? C9 C10 1.535(5) . ? C10 C11 1.547(6) . ? C11 C12 1.522(6) . ? C12 C13 1.514(6) . ? C13 C14 1.534(5) . ? C15 C16 1.533(5) . ? C15 C20 1.539(5) . ? C16 C17 1.546(5) . ? C17 C18 1.527(6) . ? C18 C19 1.518(6) . ? C19 C20 1.546(5) . ? C21 C26 1.539(4) . ? C21 C22 1.545(5) . ? C22 C23 1.529(5) . ? C23 C24 1.522(5) . ? C24 C25 1.521(5) . ? C25 C26 1.529(5) . ? C27 C28 1.512(5) . ? C27 C32 1.538(5) . ? C28 C29 1.534(5) . ? C29 C30 1.535(6) . ? C30 C31 1.482(6) . ? C31 C32 1.542(5) . ? C33 C38 1.531(4) . ? C33 C34 1.543(5) . ? C34 C35 1.528(5) . ? C35 C36 1.522(5) . ? C36 C37 1.516(5) . ? C37 C38 1.531(5) . ? C39 C44 1.381(6) . ? C39 C40 1.390(7) . ? C40 C41 1.360(7) . ? C41 C42 1.339(7) . ? C42 C43 1.373(7) . ? C43 C44 1.373(6) . ? C44 C45 1.487(7) . ? 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 C1A 32.6(4) . . ? C1 Pt1 P3 106.7(3) . . ? C1A Pt1 P3 139.1(4) . . ? C1 Pt1 P2 140.0(3) . . ? C1A Pt1 P2 107.5(4) . . ? P3 Pt1 P2 113.32(3) . . ? C1 Pt1 P1 42.6(3) . . ? C1A Pt1 P1 10.5(4) . . ? P3 Pt1 P1 149.35(8) . . ? P2 Pt1 P1 97.33(8) . . ? C1 Pt1 P1A 10.3(3) . . ? C1A Pt1 P1A 41.5(3) . . ? P3 Pt1 P1A 97.61(9) . . ? P2 Pt1 P1A 148.73(9) . . ? P1 Pt1 P1A 51.84(11) . . ? C1 P1 Pt1 58.1(3) . . ? C1A P1A Pt1 57.8(6) . . ? C9 P2 C15 103.06(16) . . ? C9 P2 C3 101.01(16) . . ? C15 P2 C3 108.02(16) . . ? C9 P2 Pt1 114.57(12) . . ? C15 P2 Pt1 107.15(12) . . ? C3 P2 Pt1 121.45(11) . . ? C21 P3 C33 101.80(15) . . ? C21 P3 C27 107.41(16) . . ? C33 P3 C27 102.24(16) . . ? C21 P3 Pt1 120.07(11) . . ? C33 P3 Pt1 114.16(11) . . ? C27 P3 Pt1 109.49(12) . . ? C2 C1 P1 140.9(6) . . ? C2 C1 Pt1 139.8(6) . . ? P1 C1 Pt1 79.2(4) . . ? C2A C1A P1A 140.6(11) . . ? C2A C1A Pt1 138.7(10) . . ? P1A C1A Pt1 80.7(6) . . ? C4 C3 C8 109.8(3) . . ? C4 C3 P2 111.4(2) . . ? C8 C3 P2 118.5(2) . . ? C5 C4 C3 112.3(3) . . ? C6 C5 C4 110.8(3) . . ? C5 C6 C7 111.3(3) . . ? C8 C7 C6 111.5(3) . . ? C7 C8 C3 111.5(3) . . ? C14 C9 C10 109.2(3) . . ? C14 C9 P2 115.6(3) . . ? C10 C9 P2 110.7(2) . . ? C9 C10 C11 110.2(3) . . ? C12 C11 C10 111.4(4) . . ? C13 C12 C11 111.7(4) . . ? C12 C13 C14 112.5(4) . . ? C9 C14 C13 110.6(3) . . ? C16 C15 C20 111.1(3) . . ? C16 C15 P2 118.6(3) . . ? C20 C15 P2 113.1(2) . . ? C15 C16 C17 110.1(3) . . ? C18 C17 C16 111.1(4) . . ? C19 C18 C17 110.9(4) . . ? C18 C19 C20 111.6(3) . . ? C15 C20 C19 110.7(3) . . ? C26 C21 C22 110.0(3) . . ? C26 C21 P3 111.4(2) . . ? C22 C21 P3 119.1(2) . . ? C23 C22 C21 111.1(3) . . ? C24 C23 C22 112.3(3) . . ? C25 C24 C23 111.0(3) . . ? C24 C25 C26 111.7(3) . . ? C25 C26 C21 111.6(3) . . ? C28 C27 C32 109.9(3) . . ? C28 C27 P3 119.6(3) . . ? C32 C27 P3 113.8(2) . . ? C27 C28 C29 111.0(3) . . ? C28 C29 C30 109.6(4) . . ? C31 C30 C29 111.6(4) . . ? C30 C31 C32 113.1(4) . . ? C27 C32 C31 110.9(3) . . ? C38 C33 C34 108.6(3) . . ? C38 C33 P3 112.8(2) . . ? C34 C33 P3 112.7(2) . . ? C35 C34 C33 111.5(3) . . ? C36 C35 C34 112.1(3) . . ? C37 C36 C35 111.3(3) . . ? C36 C37 C38 111.1(3) . . ? C33 C38 C37 110.9(3) . . ? C44 C39 C40 120.7(4) . . ? C41 C40 C39 119.8(5) . . ? C42 C41 C40 120.5(5) . . ? C41 C42 C43 119.9(4) . . ? C44 C43 C42 122.1(5) . . ? C43 C44 C39 117.0(5) . . ? C43 C44 C45 122.1(5) . . ? C39 C44 C45 120.9(4) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.740 _refine_diff_density_min -0.556 _refine_diff_density_rms 0.076 # Attachment 'compound6.CIF' data_compound6 _database_code_depnum_ccdc_archive 'CCDC 609155' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H6 O14 P2 W3' _chemical_formula_weight 1059.72 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' O O 0.0106 0.0060 '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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x-1/2, y, z-1/2' 'x, -y-1/2, z-1/2' _cell_length_a 14.323(3) _cell_length_b 30.107(6) _cell_length_c 12.311(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5308.7(19) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.652 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3824 _exptl_absorpt_coefficient_mu 13.154 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.311 _exptl_absorpt_correction_T_max 0.505 _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 9836 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5201 _reflns_number_gt 4534 _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^)+(0.0000P)^2^+19.6088P] 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 5201 _refine_ls_number_parameters 336 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0343 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_ref 0.0518 _refine_ls_wR_factor_gt 0.0500 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _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 W1 W 0.047412(16) 0.287301(8) 0.564249(18) 0.02489(7) Uani 1 1 d . . . P1 P 0.04242(10) 0.35278(5) 0.68595(11) 0.0222(3) Uani 1 1 d . . . O1 O 0.1492(4) 0.22857(17) 0.7429(4) 0.0546(13) Uani 1 1 d . . . C1 C 0.1370(4) 0.38039(18) 0.7543(4) 0.0230(12) Uani 1 1 d . . . W2 W -0.158371(15) 0.374069(8) 0.948943(18) 0.02370(6) Uani 1 1 d . . . P2 P -0.02875(10) 0.38507(5) 0.81911(11) 0.0220(3) Uani 1 1 d . . . O2 O 0.0673(3) 0.20516(14) 0.4090(4) 0.0408(11) Uani 1 1 d . . . C2 C 0.0920(4) 0.40092(19) 0.8427(4) 0.0235(12) Uani 1 1 d . . . W3 W 0.041892(15) 0.436846(7) 0.682065(18) 0.02237(6) Uani 1 1 d . . . O3 O 0.2430(3) 0.32053(17) 0.4750(4) 0.0511(13) Uani 1 1 d . . . C3 C 0.2421(4) 0.3761(2) 0.7357(5) 0.0315(14) Uani 1 1 d . . . H3A H 0.2741 0.4014 0.7692 0.047 Uiso 1 1 calc R . . H3B H 0.2549 0.3758 0.6575 0.047 Uiso 1 1 calc R . . H3C H 0.2646 0.3485 0.7684 0.047 Uiso 1 1 calc R . . O4 O -0.0582(4) 0.3389(2) 0.3762(4) 0.0780(19) Uani 1 1 d . . . C4 C 0.1328(4) 0.4223(2) 0.9421(4) 0.0312(14) Uani 1 1 d . . . H4A H 0.1886 0.4393 0.9219 0.047 Uiso 1 1 calc R . . H4B H 0.1499 0.3993 0.9948 0.047 Uiso 1 1 calc R . . H4C H 0.0867 0.4423 0.9746 0.047 Uiso 1 1 calc R . . O5 O -0.1457(3) 0.24522(18) 0.6430(4) 0.0609(15) Uani 1 1 d . . . C5 C 0.1138(4) 0.2508(2) 0.6809(5) 0.0331(14) Uani 1 1 d . . . O6 O -0.1613(3) 0.27250(16) 0.8751(4) 0.0511(13) Uani 1 1 d . . . C6 C 0.0603(4) 0.2350(2) 0.4656(5) 0.0319(14) Uani 1 1 d . . . O7 O -0.0053(4) 0.34914(18) 1.1276(4) 0.0525(13) Uani 1 1 d . . . C7 C 0.1728(4) 0.3093(2) 0.5079(5) 0.0332(14) Uani 1 1 d . . . O8 O -0.3184(3) 0.35408(16) 1.1178(3) 0.0436(12) Uani 1 1 d . . . C8 C -0.0203(5) 0.3213(2) 0.4442(5) 0.0418(16) Uani 1 1 d . . . O9 O -0.1443(4) 0.47195(15) 1.0437(4) 0.0555(13) Uani 1 1 d . . . C9 C -0.0780(5) 0.2616(2) 0.6180(5) 0.0403(16) Uani 1 1 d . . . O10 O -0.3111(3) 0.40640(16) 0.7766(4) 0.0460(12) Uani 1 1 d . . . C10 C -0.1630(4) 0.3090(2) 0.8988(5) 0.0346(14) Uani 1 1 d . . . O11 O -0.0457(4) 0.51591(17) 0.8210(4) 0.0587(14) Uani 1 1 d . . . C11 C -0.0593(4) 0.3577(2) 1.0630(5) 0.0328(14) Uani 1 1 d . . . O12 O -0.1357(3) 0.46317(18) 0.5432(4) 0.0580(14) Uani 1 1 d . . . C12 C -0.2605(4) 0.3615(2) 1.0560(4) 0.0307(14) Uani 1 1 d . . . O13 O 0.2217(3) 0.49749(17) 0.6886(4) 0.0595(15) Uani 1 1 d . . . C13 C -0.1493(4) 0.4371(2) 1.0070(5) 0.0349(14) Uani 1 1 d . . . O14 O 0.1148(4) 0.42151(19) 0.4419(4) 0.0621(15) Uani 1 1 d . . . C14 C -0.2563(4) 0.3941(2) 0.8376(5) 0.0323(14) Uani 1 1 d . . . C15 C -0.0125(5) 0.4872(2) 0.7742(5) 0.0376(15) Uani 1 1 d . . . C16 C -0.0712(5) 0.4539(2) 0.5913(5) 0.0354(15) Uani 1 1 d . . . C17 C 0.1550(5) 0.4770(2) 0.6842(5) 0.0414(16) Uani 1 1 d . . . C18 C 0.0901(4) 0.4270(2) 0.5291(5) 0.0406(16) 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 W1 0.02942(12) 0.02253(13) 0.02271(12) -0.00500(9) 0.00109(10) 0.00115(10) P1 0.0270(7) 0.0194(8) 0.0203(7) -0.0005(6) 0.0015(6) 0.0002(6) O1 0.067(3) 0.048(3) 0.049(3) 0.009(3) -0.006(3) 0.024(3) C1 0.029(3) 0.021(3) 0.019(3) 0.003(2) -0.002(2) 0.001(2) W2 0.02702(12) 0.02252(13) 0.02157(12) -0.00033(9) 0.00450(10) -0.00110(10) P2 0.0281(7) 0.0174(7) 0.0204(7) -0.0001(6) 0.0035(6) -0.0011(6) O2 0.045(3) 0.031(3) 0.046(3) -0.022(2) 0.010(2) -0.006(2) C2 0.029(3) 0.022(3) 0.019(3) -0.001(2) 0.000(2) 0.000(2) W3 0.02564(12) 0.01823(12) 0.02322(12) 0.00360(9) 0.00167(10) 0.00004(9) O3 0.043(3) 0.063(4) 0.047(3) -0.006(3) 0.018(2) -0.012(3) C3 0.032(3) 0.036(4) 0.027(3) -0.002(3) 0.002(3) 0.005(3) O4 0.082(4) 0.111(5) 0.040(3) 0.017(3) -0.006(3) 0.045(4) C4 0.037(3) 0.027(3) 0.029(3) -0.005(3) -0.003(3) 0.000(3) O5 0.037(3) 0.067(4) 0.079(4) -0.024(3) 0.022(3) -0.014(3) C5 0.034(3) 0.028(3) 0.037(4) -0.005(3) 0.007(3) 0.004(3) O6 0.058(3) 0.029(3) 0.066(3) -0.006(2) -0.001(3) -0.003(2) C6 0.032(3) 0.031(4) 0.033(3) -0.002(3) 0.003(3) -0.004(3) O7 0.055(3) 0.067(4) 0.035(3) 0.008(3) -0.009(2) 0.007(3) C7 0.045(4) 0.026(3) 0.029(3) -0.005(3) 0.005(3) 0.002(3) O8 0.034(2) 0.060(3) 0.036(3) -0.006(2) 0.017(2) -0.007(2) C8 0.042(4) 0.046(4) 0.038(4) -0.002(3) -0.001(3) 0.014(3) O9 0.072(3) 0.026(3) 0.068(3) -0.015(2) 0.002(3) -0.003(2) C9 0.037(4) 0.045(4) 0.039(4) -0.018(3) 0.008(3) -0.003(3) O10 0.047(3) 0.049(3) 0.041(3) 0.009(2) -0.011(2) 0.002(2) C10 0.032(3) 0.036(4) 0.036(3) 0.003(3) -0.002(3) -0.004(3) O11 0.063(3) 0.043(3) 0.070(4) -0.020(3) 0.004(3) 0.013(3) C11 0.044(4) 0.030(4) 0.024(3) 0.002(3) 0.010(3) 0.000(3) O12 0.043(3) 0.069(4) 0.062(3) 0.020(3) -0.022(3) 0.001(3) C12 0.035(3) 0.034(4) 0.024(3) -0.001(3) -0.003(3) 0.003(3) O13 0.042(3) 0.044(3) 0.092(4) 0.007(3) -0.001(3) -0.021(2) C13 0.033(3) 0.036(4) 0.036(3) 0.002(3) 0.002(3) -0.005(3) O14 0.072(4) 0.081(4) 0.034(3) 0.008(3) 0.021(3) 0.006(3) C14 0.036(3) 0.030(4) 0.031(3) -0.002(3) 0.009(3) -0.005(3) C15 0.042(4) 0.031(4) 0.040(4) 0.000(3) -0.006(3) 0.001(3) C16 0.040(4) 0.029(4) 0.037(4) 0.008(3) -0.005(3) -0.004(3) C17 0.045(4) 0.029(4) 0.050(4) 0.005(3) -0.001(3) 0.000(3) C18 0.039(4) 0.047(4) 0.036(4) 0.012(3) 0.010(3) 0.001(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 W1 C6 1.996(6) . ? W1 C7 2.035(7) . ? W1 C5 2.043(7) . ? W1 C8 2.043(7) . ? W1 C9 2.065(7) . ? W1 P1 2.4772(15) . ? P1 C1 1.799(6) . ? P1 P2 2.161(2) . ? P1 W3 2.5314(15) . ? O1 C5 1.134(7) . ? C1 C2 1.408(7) . ? C1 C3 1.527(8) . ? C1 W3 2.353(5) . ? W2 C12 2.005(6) . ? W2 C13 2.033(7) . ? W2 C14 2.053(7) . ? W2 C10 2.054(7) . ? W2 C11 2.056(7) . ? W2 P2 2.4721(14) . ? P2 C2 1.818(6) . ? P2 W3 2.5099(14) . ? O2 C6 1.142(7) . ? C2 C4 1.501(7) . ? C2 W3 2.366(5) . ? W3 C17 2.023(7) . ? W3 C18 2.028(7) . ? W3 C16 2.033(6) . ? W3 C15 2.047(7) . ? O3 C7 1.136(7) . ? O4 C8 1.129(7) . ? O5 C9 1.130(7) . ? O6 C10 1.138(7) . ? O7 C11 1.138(7) . ? O8 C12 1.147(7) . ? O9 C13 1.144(7) . ? O10 C14 1.147(7) . ? O11 C15 1.143(7) . ? O12 C16 1.132(7) . ? O13 C17 1.137(7) . ? O14 C18 1.142(7) . ? 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 C6 W1 C7 88.1(2) . . ? C6 W1 C5 87.7(2) . . ? C7 W1 C5 90.2(2) . . ? C6 W1 C8 89.9(3) . . ? C7 W1 C8 90.6(3) . . ? C5 W1 C8 177.5(3) . . ? C6 W1 C9 88.8(2) . . ? C7 W1 C9 176.8(2) . . ? C5 W1 C9 88.8(3) . . ? C8 W1 C9 90.4(3) . . ? C6 W1 P1 176.34(17) . . ? C7 W1 P1 88.46(17) . . ? C5 W1 P1 90.97(17) . . ? C8 W1 P1 91.44(19) . . ? C9 W1 P1 94.55(17) . . ? C1 P1 P2 78.04(18) . . ? C1 P1 W1 128.97(19) . . ? P2 P1 W1 146.13(8) . . ? C1 P1 W3 63.20(18) . . ? P2 P1 W3 64.10(5) . . ? W1 P1 W3 141.66(6) . . ? C2 C1 C3 127.2(5) . . ? C2 C1 P1 102.7(4) . . ? C3 C1 P1 129.3(4) . . ? C2 C1 W3 73.1(3) . . ? C3 C1 W3 125.0(4) . . ? P1 C1 W3 73.77(19) . . ? C12 W2 C13 89.5(2) . . ? C12 W2 C14 89.8(2) . . ? C13 W2 C14 90.2(2) . . ? C12 W2 C10 89.7(2) . . ? C13 W2 C10 176.4(2) . . ? C14 W2 C10 93.3(2) . . ? C12 W2 C11 90.5(2) . . ? C13 W2 C11 86.6(2) . . ? C14 W2 C11 176.7(2) . . ? C10 W2 C11 89.9(2) . . ? C12 W2 P2 176.57(17) . . ? C13 W2 P2 93.11(17) . . ? C14 W2 P2 92.41(16) . . ? C10 W2 P2 87.58(17) . . ? C11 W2 P2 87.44(16) . . ? C2 P2 P1 77.91(18) . . ? C2 P2 W2 130.27(18) . . ? P1 P2 W2 141.66(8) . . ? C2 P2 W3 63.95(17) . . ? P1 P2 W3 65.13(5) . . ? W2 P2 W3 145.14(6) . . ? C1 C2 C4 129.8(5) . . ? C1 C2 P2 101.4(4) . . ? C4 C2 P2 127.8(4) . . ? C1 C2 W3 72.2(3) . . ? C4 C2 W3 127.1(4) . . ? P2 C2 W3 72.39(18) . . ? C17 W3 C18 80.0(3) . . ? C17 W3 C16 119.6(3) . . ? C18 W3 C16 78.3(3) . . ? C17 W3 C15 81.6(3) . . ? C18 W3 C15 138.8(3) . . ? C16 W3 C15 79.3(3) . . ? C17 W3 C1 87.9(2) . . ? C18 W3 C1 92.8(2) . . ? C16 W3 C1 148.3(2) . . ? C15 W3 C1 123.1(2) . . ? C17 W3 C2 91.1(2) . . ? C18 W3 C2 127.3(2) . . ? C16 W3 C2 144.7(2) . . ? C15 W3 C2 89.5(2) . . ? C1 W3 C2 34.72(18) . . ? C17 W3 P2 133.31(19) . . ? C18 W3 P2 132.1(2) . . ? C16 W3 P2 101.81(18) . . ? C15 W3 P2 86.22(19) . . ? C1 W3 P2 62.02(13) . . ? C2 W3 P2 43.66(14) . . ? C17 W3 P1 126.55(19) . . ? C18 W3 P1 82.5(2) . . ? C16 W3 P1 105.36(18) . . ? C15 W3 P1 136.97(19) . . ? C1 W3 P1 43.03(14) . . ? C2 W3 P1 61.72(14) . . ? P2 W3 P1 50.77(5) . . ? O1 C5 W1 176.5(6) . . ? O2 C6 W1 179.8(6) . . ? O3 C7 W1 178.2(6) . . ? O4 C8 W1 177.9(7) . . ? O5 C9 W1 175.5(6) . . ? O6 C10 W2 175.9(6) . . ? O7 C11 W2 178.6(6) . . ? O8 C12 W2 179.4(6) . . ? O9 C13 W2 177.3(6) . . ? O10 C14 W2 178.3(5) . . ? O11 C15 W3 176.3(6) . . ? O12 C16 W3 178.2(6) . . ? O13 C17 W3 175.6(6) . . ? O14 C18 W3 178.2(6) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.285 _refine_diff_density_min -0.728 _refine_diff_density_rms 0.143 # Attachment 'compound7.CIF' data_compound7 _database_code_depnum_ccdc_archive 'CCDC 609156' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H6 O14 P2 W3' _chemical_formula_weight 1059.72 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' O O 0.0106 0.0060 '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' W W -0.8490 6.8722 '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 16.082(3) _cell_length_b 12.237(2) _cell_length_c 28.575(6) _cell_angle_alpha 90.00 _cell_angle_beta 106.02(3) _cell_angle_gamma 90.00 _cell_volume 5405.1(19) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow-orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.605 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3824 _exptl_absorpt_coefficient_mu 12.919 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.158 _exptl_absorpt_correction_T_max 0.564 _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 19315 _diffrn_reflns_av_R_equivalents 0.0523 _diffrn_reflns_av_sigmaI/netI 0.0752 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10511 _reflns_number_gt 8093 _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. Two crystallographically independent molecules were located and refined in the asymmetric unit. No significant geometric differences were found between them. The largest electron density peak and hole in the final difference map were located near W1 and W2 respectively. ; _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^)+(0.0124P)^2^+279.4335P] 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 10511 _refine_ls_number_parameters 671 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0859 _refine_ls_R_factor_gt 0.0630 _refine_ls_wR_factor_ref 0.1469 _refine_ls_wR_factor_gt 0.1385 _refine_ls_goodness_of_fit_ref 1.133 _refine_ls_restrained_S_all 1.133 _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 W1 W -0.30746(5) 1.19575(6) 0.12719(2) 0.02226(17) Uani 1 1 d . . . P1 P -0.2831(3) 1.3927(4) 0.13054(16) 0.0211(9) Uani 1 1 d . . . O1 O -0.2153(11) 1.2005(14) 0.0417(5) 0.055(4) Uani 1 1 d . . . C1 C -0.2342(10) 1.4906(14) 0.1769(6) 0.019(4) Uani 1 1 d . . . W2 W -0.08397(5) 1.70920(6) 0.13987(3) 0.02635(18) Uani 1 1 d . . . P2 P -0.2023(3) 1.5811(4) 0.13496(15) 0.0198(9) Uani 1 1 d . . . O2 O -0.1287(9) 1.1575(12) 0.2083(5) 0.045(4) Uani 1 1 d . . . C2 C -0.2080(12) 1.4834(15) 0.2300(6) 0.029(4) Uani 1 1 d . . . H2A H -0.2465 1.4329 0.2406 0.043 Uiso 1 1 calc R . . H2B H -0.2117 1.5560 0.2439 0.043 Uiso 1 1 calc R . . H2C H -0.1484 1.4566 0.2412 0.043 Uiso 1 1 calc R . . W3 W -0.36062(4) 1.57050(6) 0.12640(2) 0.02066(16) Uani 1 1 d . . . P3 P 0.1778(3) 1.0734(4) 0.12449(16) 0.0221(9) Uani 1 1 d . . . O3 O -0.3217(14) 0.9406(14) 0.1207(8) 0.081(7) Uani 1 1 d . . . C3 C -0.2626(11) 1.4919(13) 0.0902(6) 0.020(4) Uani 1 1 d . . . W4 W 0.07197(5) 1.20644(6) 0.13655(3) 0.03094(19) Uani 1 1 d . . . P4 P 0.2565(3) 0.8930(4) 0.11258(16) 0.0191(9) Uani 1 1 d . . . O4 O -0.4086(10) 1.2173(13) 0.2083(5) 0.048(4) Uani 1 1 d . . . C4 C -0.2703(13) 1.4856(16) 0.0353(6) 0.033(4) Uani 1 1 d . . . H4A H -0.2813 1.5588 0.0210 0.049 Uiso 1 1 calc R . . H4B H -0.3181 1.4369 0.0195 0.049 Uiso 1 1 calc R . . H4C H -0.2162 1.4571 0.0306 0.049 Uiso 1 1 calc R . . W5 W 0.29872(4) 0.70031(6) 0.11260(3) 0.02316(17) Uani 1 1 d . . . O5 O -0.4914(10) 1.2138(16) 0.0494(5) 0.061(5) Uani 1 1 d . . . C5 C -0.2481(12) 1.1958(16) 0.0724(6) 0.030(4) Uani 1 1 d . . . W6 W 0.32107(5) 1.07475(6) 0.10649(3) 0.02481(17) Uani 1 1 d . . . O6 O 0.0182(10) 1.5783(13) 0.2344(6) 0.056(4) Uani 1 1 d . . . C6 C -0.1917(13) 1.1763(16) 0.1799(6) 0.031(4) Uani 1 1 d . . . O7 O -0.0125(13) 1.5425(18) 0.0733(7) 0.080(6) Uani 1 1 d U . . C7 C -0.3146(14) 1.028(2) 0.1237(8) 0.050(6) Uani 1 1 d . . . O8 O 0.0760(13) 1.8584(18) 0.1479(8) 0.083(6) Uani 1 1 d U . . C8 C -0.3708(12) 1.2090(15) 0.1797(6) 0.028(4) Uani 1 1 d . . . O9 O -0.1962(12) 1.8404(15) 0.0471(6) 0.064(5) Uani 1 1 d . . . C9 C -0.4252(14) 1.2107(17) 0.0767(7) 0.036(5) Uani 1 1 d . . . O10 O -0.1482(10) 1.8863(12) 0.2040(5) 0.046(4) Uani 1 1 d . . . C10 C -0.0170(11) 1.6271(15) 0.2000(8) 0.032(4) Uani 1 1 d . . . O11 O -0.3880(12) 1.7633(13) 0.0480(6) 0.069(6) Uani 1 1 d . . . C11 C -0.0376(17) 1.6062(19) 0.1006(11) 0.059(7) Uani 1 1 d . . . O12 O -0.3421(11) 1.7727(13) 0.1973(6) 0.057(5) Uani 1 1 d . . . C12 C 0.0176(13) 1.8043(18) 0.1441(9) 0.043(5) Uani 1 1 d . . . O13 O -0.5249(10) 1.4781(15) 0.0480(6) 0.057(5) Uani 1 1 d . . . C13 C -0.1565(14) 1.7906(17) 0.0795(8) 0.039(5) Uani 1 1 d . . . O14 O -0.4677(9) 1.4829(12) 0.1972(5) 0.038(3) Uani 1 1 d . . . C14 C -0.1255(11) 1.8196(16) 0.1808(7) 0.031(4) Uani 1 1 d . . . O15 O 0.1051(11) 1.1007(16) 0.2426(6) 0.063(5) Uani 1 1 d . . . C15 C -0.3820(14) 1.6930(16) 0.0759(7) 0.043(5) Uani 1 1 d . . . O16 O -0.0797(9) 1.0337(12) 0.1024(6) 0.050(4) Uani 1 1 d . . . C16 C -0.3493(14) 1.6980(17) 0.1727(7) 0.036(5) Uani 1 1 d . . . O17 O -0.0661(11) 1.3702(12) 0.1546(8) 0.071(6) Uani 1 1 d . . . C17 C -0.4687(12) 1.5126(18) 0.0763(7) 0.035(5) Uani 1 1 d . . . O18 O 0.0504(14) 1.2858(19) 0.0273(8) 0.092(7) Uani 1 1 d . . . C18 C -0.4290(13) 1.5106(17) 0.1722(7) 0.037(5) Uani 1 1 d . . . O19 O 0.2120(12) 1.3959(16) 0.1707(8) 0.076(6) Uani 1 1 d . . . C19 C 0.2594(11) 0.9834(13) 0.1599(6) 0.023(4) Uani 1 1 d . . . O20 O 0.1290(10) 0.6464(18) 0.0279(6) 0.068(5) Uani 1 1 d . . . C20 C 0.2908(12) 0.9700(17) 0.2145(6) 0.032(4) Uani 1 1 d . . . H20A H 0.2458 0.9341 0.2262 0.049 Uiso 1 1 calc R . . H20B H 0.3035 1.0420 0.2298 0.049 Uiso 1 1 calc R . . H20C H 0.3433 0.9253 0.2229 0.049 Uiso 1 1 calc R . . O21 O 0.1946(11) 0.6567(15) 0.1909(6) 0.061(5) Uani 1 1 d . . . C21 C 0.1875(11) 0.9883(14) 0.0756(5) 0.021(4) Uani 1 1 d . . . O22 O 0.3530(10) 0.4528(13) 0.1179(7) 0.060(5) Uani 1 1 d . . . C22 C 0.1312(12) 0.9841(16) 0.0229(6) 0.032(4) Uani 1 1 d . . . H22A H 0.1677 0.9691 0.0013 0.048 Uiso 1 1 calc R . . H22B H 0.1020 1.0546 0.0142 0.048 Uiso 1 1 calc R . . H22C H 0.0879 0.9262 0.0195 0.048 Uiso 1 1 calc R . . O23 O 0.4679(9) 0.7572(13) 0.1966(5) 0.048(4) Uani 1 1 d . . . C23 C 0.0920(14) 1.140(2) 0.2061(8) 0.046(6) Uani 1 1 d . . . O24 O 0.4031(10) 0.7448(13) 0.0351(5) 0.049(4) Uani 1 1 d . . . C24 C -0.0241(12) 1.0938(14) 0.1135(6) 0.026(4) Uani 1 1 d U . . O25 O 0.3900(12) 1.2536(12) 0.1878(6) 0.068(6) Uani 1 1 d . . . C25 C -0.0164(13) 1.314(2) 0.1471(9) 0.051(6) Uani 1 1 d . . . O26 O 0.2749(15) 1.2903(13) 0.0420(6) 0.083(7) Uani 1 1 d . . . C26 C 0.0591(17) 1.263(2) 0.0673(10) 0.064(8) Uani 1 1 d . . . O27 O 0.3746(12) 1.0007(15) 0.0123(6) 0.068(5) Uani 1 1 d . . . C27 C 0.1657(13) 1.3275(19) 0.1618(8) 0.041(5) Uani 1 1 d . . . O28 O 0.5092(10) 0.9820(16) 0.1551(7) 0.070(6) Uani 1 1 d . . . C28 C 0.1882(13) 0.6679(19) 0.0597(8) 0.040(5) Uani 1 1 d . . . C29 C 0.2328(14) 0.6752(15) 0.1630(8) 0.038(5) Uani 1 1 d . . . C30 C 0.3329(13) 0.5406(16) 0.1156(9) 0.047(6) Uani 1 1 d . . . C31 C 0.4066(12) 0.7419(18) 0.1665(7) 0.038(5) Uani 1 1 d . . . C32 C 0.3645(12) 0.7301(15) 0.0616(7) 0.031(4) Uani 1 1 d . . . C33 C 0.3672(12) 1.1902(16) 0.1588(7) 0.032(4) Uani 1 1 d . . . C34 C 0.2892(18) 1.210(2) 0.0652(8) 0.056(7) Uani 1 1 d . . . C35 C 0.3563(14) 1.0284(17) 0.0448(8) 0.041(5) Uani 1 1 d . . . C36 C 0.4451(14) 1.0202(16) 0.1376(8) 0.038(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 W1 0.0281(4) 0.0142(4) 0.0245(3) -0.0006(3) 0.0072(3) -0.0033(3) P1 0.022(2) 0.016(2) 0.025(2) 0.0012(18) 0.0055(18) -0.0016(18) O1 0.077(12) 0.055(11) 0.043(9) 0.009(8) 0.033(9) 0.019(9) C1 0.014(8) 0.026(10) 0.019(8) -0.001(7) 0.007(6) -0.009(7) W2 0.0251(4) 0.0175(4) 0.0401(4) 0.0011(3) 0.0151(3) -0.0035(3) P2 0.024(2) 0.013(2) 0.023(2) -0.0004(17) 0.0082(17) -0.0024(18) O2 0.042(9) 0.045(9) 0.037(8) 0.013(7) -0.007(7) 0.013(7) C2 0.037(11) 0.023(10) 0.028(9) 0.001(8) 0.011(8) 0.000(8) W3 0.0201(3) 0.0156(4) 0.0253(3) 0.0001(3) 0.0048(3) 0.0006(3) P3 0.026(2) 0.016(2) 0.025(2) -0.0033(18) 0.0088(18) 0.0006(19) O3 0.118(17) 0.018(9) 0.131(18) -0.022(10) 0.074(15) -0.032(10) C3 0.028(9) 0.011(8) 0.023(8) 0.005(7) 0.011(7) 0.005(7) W4 0.0282(4) 0.0199(4) 0.0465(5) -0.0060(3) 0.0133(3) 0.0034(3) P4 0.021(2) 0.013(2) 0.024(2) -0.0027(17) 0.0067(17) -0.0006(18) O4 0.068(10) 0.052(10) 0.037(8) 0.008(7) 0.036(8) 0.002(8) C4 0.044(12) 0.029(11) 0.024(9) 0.002(8) 0.008(8) 0.001(9) W5 0.0241(4) 0.0166(4) 0.0305(4) 0.0024(3) 0.0104(3) 0.0024(3) O5 0.032(9) 0.099(15) 0.042(9) 0.019(9) -0.007(7) -0.016(9) C5 0.040(11) 0.030(11) 0.019(9) -0.006(8) 0.007(8) 0.000(9) W6 0.0256(4) 0.0179(4) 0.0331(4) 0.0021(3) 0.0118(3) -0.0021(3) O6 0.050(10) 0.043(10) 0.064(10) 0.019(8) -0.002(8) 0.009(8) C6 0.037(11) 0.029(11) 0.024(9) 0.008(8) 0.006(8) -0.006(9) O7 0.085(8) 0.084(8) 0.084(8) -0.011(6) 0.044(6) 0.002(6) C7 0.037(12) 0.070(19) 0.033(12) 0.012(11) -0.007(9) -0.017(12) O8 0.073(8) 0.081(8) 0.097(8) 0.009(6) 0.029(6) -0.003(6) C8 0.031(10) 0.017(9) 0.031(10) -0.005(8) -0.001(8) 0.005(8) O9 0.084(13) 0.056(11) 0.041(9) 0.020(9) 0.000(9) -0.016(10) C9 0.043(12) 0.028(11) 0.042(11) 0.012(9) 0.019(10) -0.007(9) O10 0.063(10) 0.033(9) 0.045(9) -0.016(7) 0.020(8) 0.007(8) C10 0.019(9) 0.019(10) 0.059(13) -0.003(9) 0.013(9) 0.000(8) O11 0.090(14) 0.028(9) 0.063(11) 0.026(8) -0.022(10) -0.011(9) C11 0.068(17) 0.031(13) 0.10(2) 0.006(13) 0.064(16) -0.007(12) O12 0.073(12) 0.035(9) 0.077(11) -0.027(9) 0.044(10) -0.020(8) C12 0.027(11) 0.034(12) 0.074(15) 0.002(11) 0.023(10) -0.004(10) O13 0.037(9) 0.067(12) 0.059(10) -0.006(9) -0.004(8) -0.008(8) C13 0.051(13) 0.030(12) 0.046(12) -0.012(10) 0.029(11) -0.020(10) O14 0.044(8) 0.041(9) 0.037(8) 0.008(6) 0.023(7) -0.009(7) C14 0.023(9) 0.023(11) 0.043(11) 0.002(9) 0.000(8) -0.015(8) O15 0.058(11) 0.094(15) 0.033(9) -0.001(9) 0.005(8) 0.013(10) C15 0.054(14) 0.017(11) 0.040(11) -0.004(9) -0.018(10) -0.010(10) O16 0.037(8) 0.024(8) 0.071(11) -0.006(7) -0.016(7) -0.008(7) C16 0.056(13) 0.023(11) 0.035(11) -0.002(9) 0.022(10) -0.015(10) O17 0.053(11) 0.016(8) 0.155(19) 0.001(10) 0.046(12) 0.007(8) C17 0.025(10) 0.054(14) 0.033(11) 0.015(10) 0.016(9) 0.007(10) O18 0.096(16) 0.097(17) 0.088(15) 0.044(13) 0.033(13) 0.048(14) C18 0.032(11) 0.035(12) 0.036(11) 0.007(9) -0.005(9) -0.011(9) O19 0.064(12) 0.058(12) 0.117(17) -0.031(11) 0.041(12) -0.035(11) C19 0.032(10) 0.004(8) 0.035(10) 0.006(7) 0.012(8) -0.001(7) O20 0.040(10) 0.114(17) 0.050(10) -0.013(10) 0.009(8) -0.009(10) C20 0.026(10) 0.039(12) 0.027(10) -0.011(9) -0.001(8) 0.005(9) O21 0.060(11) 0.066(12) 0.072(11) 0.028(9) 0.043(10) 0.019(9) C21 0.034(10) 0.020(9) 0.011(8) 0.001(6) 0.009(7) -0.006(7) O22 0.054(10) 0.026(9) 0.106(14) 0.020(9) 0.031(10) 0.018(8) C22 0.035(11) 0.028(11) 0.023(9) 0.000(8) -0.009(8) 0.005(9) O23 0.036(8) 0.049(10) 0.050(9) 0.010(7) -0.004(7) -0.004(7) C23 0.042(12) 0.069(17) 0.030(11) -0.022(11) 0.012(10) 0.001(12) O24 0.048(9) 0.060(11) 0.052(9) 0.008(8) 0.036(8) 0.001(8) C24 0.033(6) 0.015(6) 0.029(6) 0.005(5) 0.005(5) 0.005(5) O25 0.084(13) 0.018(8) 0.075(12) -0.009(8) -0.025(10) 0.009(8) C25 0.026(11) 0.041(14) 0.089(18) -0.016(12) 0.022(11) -0.004(11) O26 0.17(2) 0.019(9) 0.042(9) 0.007(8) 0.001(11) -0.009(11) C26 0.065(17) 0.068(19) 0.061(16) 0.031(14) 0.017(13) 0.048(15) O27 0.091(14) 0.077(14) 0.055(11) -0.011(9) 0.054(11) 0.002(11) C27 0.033(11) 0.038(13) 0.061(14) -0.003(11) 0.029(10) 0.002(10) O28 0.022(8) 0.069(13) 0.115(16) -0.002(11) 0.009(9) 0.014(9) C28 0.030(11) 0.047(14) 0.048(13) 0.014(11) 0.017(10) -0.002(10) C29 0.044(12) 0.013(10) 0.057(13) 0.008(9) 0.015(10) 0.015(9) C30 0.037(12) 0.008(10) 0.101(19) -0.007(11) 0.031(12) 0.007(9) C31 0.023(10) 0.047(13) 0.039(11) -0.005(10) -0.003(9) 0.013(9) C32 0.032(10) 0.021(10) 0.040(11) 0.006(8) 0.009(9) 0.005(8) C33 0.026(10) 0.024(11) 0.043(11) 0.011(9) 0.004(8) 0.004(8) C34 0.090(19) 0.040(14) 0.031(11) -0.019(11) 0.009(12) -0.014(13) C35 0.042(12) 0.031(12) 0.055(14) 0.001(10) 0.022(11) -0.004(10) C36 0.045(13) 0.019(10) 0.058(13) -0.019(9) 0.027(11) -0.012(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 W1 C8 2.040(19) . ? W1 C9 2.05(2) . ? W1 C5 2.048(18) . ? W1 C6 2.059(19) . ? W1 C7 2.06(3) . ? W1 P1 2.440(5) . ? P1 C3 1.765(16) . ? P1 C1 1.797(17) . ? P1 W3 2.494(5) . ? O1 C5 1.14(2) . ? C1 C2 1.46(2) . ? C1 P2 1.806(16) . ? C1 W3 2.356(17) . ? W2 C11 1.97(2) . ? W2 C12 1.98(2) . ? W2 C14 2.02(2) . ? W2 C10 2.03(2) . ? W2 C13 2.05(2) . ? W2 P2 2.440(4) . ? P2 C3 1.755(17) . ? P2 W3 2.492(4) . ? O2 C6 1.13(2) . ? W3 C16 2.02(2) . ? W3 C15 2.04(2) . ? W3 C17 2.05(2) . ? W3 C18 2.06(2) . ? W3 C3 2.318(16) . ? P3 C21 1.784(16) . ? P3 C19 1.795(18) . ? P3 W4 2.448(4) . ? P3 W6 2.495(4) . ? O3 C7 1.07(3) . ? C3 C4 1.54(2) . ? W4 C25 2.02(2) . ? W4 C24 2.040(19) . ? W4 C26 2.05(3) . ? W4 C23 2.09(2) . ? W4 C27 2.09(2) . ? P4 C19 1.737(18) . ? P4 C21 1.750(18) . ? P4 W5 2.454(4) . ? P4 W6 2.480(4) . ? O4 C8 1.15(2) . ? W5 C30 2.026(19) . ? W5 C28 2.03(2) . ? W5 C29 2.03(2) . ? W5 C31 2.04(2) . ? W5 C32 2.055(19) . ? O5 C9 1.13(2) . ? W6 C34 2.02(3) . ? W6 C33 2.04(2) . ? W6 C36 2.06(2) . ? W6 C35 2.07(2) . ? W6 C19 2.323(16) . ? W6 C21 2.339(17) . ? O6 C10 1.16(2) . ? O7 C11 1.25(3) . ? O8 C12 1.13(3) . ? O9 C13 1.14(3) . ? O10 C14 1.17(2) . ? O11 C15 1.16(2) . ? O12 C16 1.14(2) . ? O13 C17 1.12(2) . ? O14 C18 1.12(2) . ? O15 C23 1.11(3) . ? O16 C24 1.13(2) . ? O17 C25 1.12(2) . ? O18 C26 1.15(3) . ? O19 C27 1.10(3) . ? C19 C20 1.51(2) . ? O20 C28 1.15(2) . ? O21 C29 1.16(2) . ? C21 C22 1.53(2) . ? O22 C30 1.12(2) . ? O23 C31 1.13(2) . ? O24 C32 1.12(2) . ? O25 C33 1.12(2) . ? O26 C34 1.17(3) . ? O27 C35 1.10(2) . ? O28 C36 1.12(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 C8 W1 C9 87.7(7) . . ? C8 W1 C5 174.9(7) . . ? C9 W1 C5 89.8(7) . . ? C8 W1 C6 90.3(7) . . ? C9 W1 C6 177.4(7) . . ? C5 W1 C6 92.3(7) . . ? C8 W1 C7 94.7(8) . . ? C9 W1 C7 91.5(8) . . ? C5 W1 C7 89.7(8) . . ? C6 W1 C7 87.0(8) . . ? C8 W1 P1 90.0(5) . . ? C9 W1 P1 92.7(6) . . ? C5 W1 P1 85.7(6) . . ? C6 W1 P1 89.0(5) . . ? C7 W1 P1 173.8(7) . . ? C3 P1 C1 84.2(8) . . ? C3 P1 W1 135.3(6) . . ? C1 P1 W1 136.1(6) . . ? C3 P1 W3 63.2(5) . . ? C1 P1 W3 64.2(6) . . ? W1 P1 W3 141.90(19) . . ? C2 C1 P1 131.8(13) . . ? C2 C1 P2 132.2(13) . . ? P1 C1 P2 93.8(7) . . ? C2 C1 W3 127.8(12) . . ? P1 C1 W3 72.4(6) . . ? P2 C1 W3 72.2(6) . . ? C11 W2 C12 88.6(9) . . ? C11 W2 C14 176.9(9) . . ? C12 W2 C14 88.3(8) . . ? C11 W2 C10 88.2(10) . . ? C12 W2 C10 90.2(8) . . ? C14 W2 C10 91.3(8) . . ? C11 W2 C13 92.8(10) . . ? C12 W2 C13 91.9(9) . . ? C14 W2 C13 87.7(8) . . ? C10 W2 C13 177.7(7) . . ? C11 W2 P2 88.2(7) . . ? C12 W2 P2 176.0(6) . . ? C14 W2 P2 94.9(5) . . ? C10 W2 P2 87.4(5) . . ? C13 W2 P2 90.6(5) . . ? C3 P2 C1 84.3(7) . . ? C3 P2 W2 135.0(6) . . ? C1 P2 W2 135.7(5) . . ? C3 P2 W3 63.4(5) . . ? C1 P2 W3 64.2(5) . . ? W2 P2 W3 143.0(2) . . ? C16 W3 C15 82.2(8) . . ? C16 W3 C17 129.1(9) . . ? C15 W3 C17 79.4(8) . . ? C16 W3 C18 80.0(8) . . ? C15 W3 C18 133.9(9) . . ? C17 W3 C18 79.7(7) . . ? C16 W3 C3 131.5(7) . . ? C15 W3 C3 89.5(8) . . ? C17 W3 C3 95.5(7) . . ? C18 W3 C3 133.1(7) . . ? C16 W3 C1 90.7(7) . . ? C15 W3 C1 133.3(7) . . ? C17 W3 C1 134.9(7) . . ? C18 W3 C1 89.2(7) . . ? C3 W3 C1 61.5(5) . . ? C16 W3 P2 89.4(6) . . ? C15 W3 P2 89.9(7) . . ? C17 W3 P2 137.2(5) . . ? C18 W3 P2 131.7(5) . . ? C3 W3 P2 42.6(4) . . ? C1 W3 P2 43.6(4) . . ? C16 W3 P1 133.5(6) . . ? C15 W3 P1 131.1(7) . . ? C17 W3 P1 92.8(6) . . ? C18 W3 P1 90.4(6) . . ? C3 W3 P1 42.8(4) . . ? C1 W3 P1 43.4(4) . . ? P2 W3 P1 63.70(14) . . ? C21 P3 C19 82.9(8) . . ? C21 P3 W4 135.5(6) . . ? C19 P3 W4 139.2(6) . . ? C21 P3 W6 63.8(6) . . ? C19 P3 W6 63.1(5) . . ? W4 P3 W6 137.9(2) . . ? C4 C3 P2 130.2(13) . . ? C4 C3 P1 130.7(13) . . ? P2 C3 P1 96.8(8) . . ? C4 C3 W3 127.0(12) . . ? P2 C3 W3 74.0(6) . . ? P1 C3 W3 73.9(6) . . ? C25 W4 C24 89.2(8) . . ? C25 W4 C26 92.0(10) . . ? C24 W4 C26 93.0(10) . . ? C25 W4 C23 92.5(10) . . ? C24 W4 C23 87.0(8) . . ? C26 W4 C23 175.6(9) . . ? C25 W4 C27 87.6(8) . . ? C24 W4 C27 176.7(7) . . ? C26 W4 C27 87.9(11) . . ? C23 W4 C27 92.4(9) . . ? C25 W4 P3 178.9(7) . . ? C24 W4 P3 90.0(5) . . ? C26 W4 P3 88.8(7) . . ? C23 W4 P3 86.7(6) . . ? C27 W4 P3 93.2(6) . . ? C19 P4 C21 85.5(8) . . ? C19 P4 W5 131.6(6) . . ? C21 P4 W5 140.3(6) . . ? C19 P4 W6 64.0(5) . . ? C21 P4 W6 64.4(6) . . ? W5 P4 W6 137.79(18) . . ? C30 W5 C28 90.8(9) . . ? C30 W5 C29 90.7(8) . . ? C28 W5 C29 88.7(8) . . ? C30 W5 C31 92.5(9) . . ? C28 W5 C31 176.5(9) . . ? C29 W5 C31 90.2(9) . . ? C30 W5 C32 90.8(8) . . ? C28 W5 C32 91.3(8) . . ? C29 W5 C32 178.4(7) . . ? C31 W5 C32 89.7(8) . . ? C30 W5 P4 177.5(7) . . ? C28 W5 P4 90.2(7) . . ? C29 W5 P4 87.0(5) . . ? C31 W5 P4 86.4(6) . . ? C32 W5 P4 91.5(5) . . ? O1 C5 W1 177.1(18) . . ? C34 W6 C33 80.8(8) . . ? C34 W6 C36 125.4(10) . . ? C33 W6 C36 78.2(7) . . ? C34 W6 C35 79.2(9) . . ? C33 W6 C35 133.0(8) . . ? C36 W6 C35 79.6(8) . . ? C34 W6 C19 133.9(9) . . ? C33 W6 C19 89.3(7) . . ? C36 W6 C19 95.7(7) . . ? C35 W6 C19 133.9(7) . . ? C34 W6 C21 95.3(8) . . ? C33 W6 C21 134.4(7) . . ? C36 W6 C21 134.1(7) . . ? C35 W6 C21 89.6(7) . . ? C19 W6 C21 61.0(6) . . ? C34 W6 P4 137.3(7) . . ? C33 W6 P4 130.1(5) . . ? C36 W6 P4 93.0(5) . . ? C35 W6 P4 91.9(6) . . ? C19 W6 P4 42.2(4) . . ? C21 W6 P4 42.5(4) . . ? C34 W6 P3 91.5(8) . . ? C33 W6 P3 91.3(5) . . ? C36 W6 P3 138.5(6) . . ? C35 W6 P3 131.1(6) . . ? C19 W6 P3 43.6(4) . . ? C21 W6 P3 43.2(4) . . ? P4 W6 P3 63.35(14) . . ? O2 C6 W1 174.9(18) . . ? O3 C7 W1 177(2) . . ? O4 C8 W1 178.0(16) . . ? O5 C9 W1 176.4(18) . . ? O6 C10 W2 177.2(16) . . ? O7 C11 W2 176(3) . . ? O8 C12 W2 178(2) . . ? O9 C13 W2 176.7(19) . . ? O10 C14 W2 177.7(16) . . ? O11 C15 W3 175(2) . . ? O12 C16 W3 177.0(17) . . ? O13 C17 W3 176.4(18) . . ? O14 C18 W3 176.7(19) . . ? C20 C19 P4 131.6(13) . . ? C20 C19 P3 129.2(13) . . ? P4 C19 P3 95.4(9) . . ? C20 C19 W6 130.5(12) . . ? P4 C19 W6 73.7(6) . . ? P3 C19 W6 73.3(6) . . ? C22 C21 P4 132.7(13) . . ? C22 C21 P3 129.5(13) . . ? P4 C21 P3 95.3(8) . . ? C22 C21 W6 128.3(11) . . ? P4 C21 W6 73.1(6) . . ? P3 C21 W6 73.1(6) . . ? O15 C23 W4 177(2) . . ? O16 C24 W4 176.3(17) . . ? O17 C25 W4 177(2) . . ? O18 C26 W4 174(3) . . ? O19 C27 W4 173(2) . . ? O20 C28 W5 175.2(19) . . ? O21 C29 W5 177.2(19) . . ? O22 C30 W5 179(3) . . ? O23 C31 W5 175.1(19) . . ? O24 C32 W5 177.3(17) . . ? O25 C33 W6 177.8(19) . . ? O26 C34 W6 177(2) . . ? O27 C35 W6 178(2) . . ? O28 C36 W6 173.9(19) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.552 _refine_diff_density_min -1.850 _refine_diff_density_rms 0.320