# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Dodds, Deborah' 'Floure, Joelle' 'Garland, Michael' 'Haddow, Mairi' 'Leonard, Thomas' 'McMullin, Claire' 'Orpen, A.' 'Pringle, Paul G.' _publ_contact_author_name 'Pringle, Paul G.' _publ_contact_author_email paul.pringle@bristol.ac.uk _publ_section_title ; Diphosphanes derived from phobane and phosphatrioxa- adamantane: similarities, differences and anomalies. ; # Attachment '- Diphosphanes.cif' data_1a _database_code_depnum_ccdc_archive 'CCDC 815349' #TrackingRef '- Diphosphanes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H32 O6.84 P2' _chemical_formula_sum 'C20 H32 O6.84 P2' _chemical_formula_weight 443.77 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.019(3) _cell_length_b 8.4223(19) _cell_length_c 20.509(5) _cell_angle_alpha 90.00 _cell_angle_beta 107.483(12) _cell_angle_gamma 90.00 _cell_volume 2144.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 21876 _cell_measurement_theta_min 2.92 _cell_measurement_theta_max 30.19 _exptl_crystal_description nuget _exptl_crystal_colour colourless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 946.4 _exptl_absorpt_coefficient_mu 0.241 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9676 _exptl_absorpt_correction_T_max 0.9759 _exptl_absorpt_process_details 'SADABS 2008/2 (Sheldrick, G.M., 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.366 _diffrn_detector_type 'Bruker-AXS SMART APEX' _diffrn_measurement_details 'frames, 0.3\% width' _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Bruker-AXS Kappa' _diffrn_measurement_method '\w & \f scans' _diffrn_measurement_specimen_support ; glass fibre ; _diffrn_radiation_collimation '0.5 mm double pinhole' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe X-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71074 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 40 _diffrn_source_power 2 _diffrn_source_size '0.4 x 8 mm fine focus' _diffrn_source_target Mo _diffrn_source_type 'Bruker-AXS KFF Mo 2K 90\% Ceramic' _diffrn_source_voltage 50 _diffrn_reflns_number 20939 _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_sigmaI/netI 0.0400 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 30.19 _reflns_number_total 3160 _reflns_number_gt 2344 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex II (Bruker-AXS, 2007)' _computing_cell_refinement 'Apex II (Bruker-AXS, 2007)' _computing_data_reduction ; SAINT v7.34A (Bruker-AXS, 2007) & XPREP v2005/4 (Bruker-AXS, 2005) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; P1 is partially oxidised - O4. The occupancy of the oxygen atom in this solution was refined using a free variable to be 41.7%. 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^)+(0.0408P)^2^+1.1795P] 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 3160 _refine_ls_number_parameters 141 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0621 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.0968 _refine_ls_wR_factor_gt 0.0886 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 P1 P 1.03903(3) 0.29679(4) 0.20809(2) 0.02164(11) Uani 1 1 d . . . O1 O 0.94044(7) 0.02232(11) 0.14493(5) 0.0207(2) Uani 1 1 d . . . O2 O 0.96538(8) 0.37996(11) 0.07632(5) 0.0210(2) Uani 1 1 d . . . O3 O 0.89269(7) 0.13191(12) 0.03496(5) 0.0212(2) Uani 1 1 d . . . O4 O 1.13431(19) 0.3831(3) 0.22035(13) 0.0307(9) Uani 0.418(4) 1 d P . . C1 C 1.12178(12) -0.01623(18) 0.21194(8) 0.0262(3) Uani 1 1 d . . . H1A H 1.0974 -0.0431 0.2514 0.039 Uiso 1 1 calc R . . H1B H 1.1935 0.0319 0.2278 0.039 Uiso 1 1 calc R . . H1C H 1.1249 -0.1129 0.1860 0.039 Uiso 1 1 calc R . . C2 C 1.04384(11) 0.09996(17) 0.16658(7) 0.0205(3) Uani 1 1 d . . . C3 C 1.07684(11) 0.14290(17) 0.10322(7) 0.0216(3) Uani 1 1 d . . . H3A H 1.1418 0.2110 0.1168 0.026 Uiso 1 1 calc R . . H3B H 1.0951 0.0448 0.0825 0.026 Uiso 1 1 calc R . . C4 C 0.98684(11) 0.22975(16) 0.05081(8) 0.0206(3) Uani 1 1 d . . . C5 C 1.01090(12) 0.26263(18) -0.01507(8) 0.0250(3) Uani 1 1 d . . . H5A H 0.9472 0.3087 -0.0481 0.037 Uiso 1 1 calc R . . H5B H 1.0301 0.1632 -0.0334 0.037 Uiso 1 1 calc R . . H5C H 1.0712 0.3374 -0.0067 0.037 Uiso 1 1 calc R . . C6 C 0.76439(12) -0.00896(19) 0.07250(8) 0.0273(3) Uani 1 1 d . . . H6A H 0.7879 -0.1094 0.0575 0.041 Uiso 1 1 calc R . . H6B H 0.7072 0.0377 0.0348 0.041 Uiso 1 1 calc R . . H6C H 0.7369 -0.0286 0.1113 0.041 Uiso 1 1 calc R . . C7 C 0.85787(11) 0.10353(17) 0.09370(7) 0.0213(3) Uani 1 1 d . . . C8 C 0.82976(11) 0.26190(17) 0.11929(8) 0.0211(3) Uani 1 1 d . . . H8A H 0.8079 0.2449 0.1610 0.025 Uiso 1 1 calc R . . H8B H 0.7682 0.3101 0.0841 0.025 Uiso 1 1 calc R . . C9 C 0.92552(11) 0.37408(17) 0.13524(7) 0.0198(3) Uani 1 1 d . . . C10 C 0.89705(12) 0.54383(17) 0.14675(8) 0.0254(3) Uani 1 1 d . . . H10A H 0.9614 0.6105 0.1553 0.038 Uiso 1 1 calc R . . H10B H 0.8696 0.5484 0.1863 0.038 Uiso 1 1 calc R . . H10C H 0.8416 0.5825 0.1061 0.038 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 P1 0.02027(19) 0.0218(2) 0.0246(2) 0.00037(15) 0.00945(15) 0.00110(15) O1 0.0162(5) 0.0189(5) 0.0256(5) 0.0020(4) 0.0043(4) -0.0014(4) O2 0.0246(5) 0.0177(5) 0.0236(5) 0.0002(4) 0.0115(4) -0.0008(4) O3 0.0186(5) 0.0220(5) 0.0229(5) -0.0006(4) 0.0064(4) -0.0044(4) O4 0.0200(14) 0.0396(17) 0.0330(16) -0.0092(12) 0.0086(11) -0.0093(11) C1 0.0224(7) 0.0275(8) 0.0288(8) 0.0015(6) 0.0076(6) 0.0067(6) C2 0.0147(6) 0.0214(7) 0.0253(7) -0.0008(6) 0.0055(5) 0.0002(5) C3 0.0176(7) 0.0203(7) 0.0279(8) -0.0035(6) 0.0084(6) -0.0017(5) C4 0.0203(7) 0.0173(7) 0.0255(7) -0.0024(6) 0.0088(6) -0.0037(5) C5 0.0274(8) 0.0242(8) 0.0254(8) -0.0033(6) 0.0112(6) -0.0050(6) C6 0.0218(7) 0.0280(8) 0.0312(8) -0.0006(6) 0.0068(6) -0.0064(6) C7 0.0172(7) 0.0233(7) 0.0227(7) 0.0027(6) 0.0048(6) -0.0008(5) C8 0.0168(7) 0.0226(7) 0.0239(7) 0.0045(6) 0.0060(6) 0.0016(5) C9 0.0204(7) 0.0189(7) 0.0221(7) 0.0017(6) 0.0097(6) 0.0003(5) C10 0.0312(8) 0.0211(7) 0.0270(8) 0.0026(6) 0.0132(7) 0.0039(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 O4 1.394(2) . ? P1 C2 1.8732(15) . ? P1 C9 1.8743(15) . ? P1 P1 2.2447(9) 2_755 ? O1 C7 1.4314(17) . ? O1 C2 1.4413(16) . ? O2 C4 1.4284(17) . ? O2 C9 1.4523(16) . ? O3 C7 1.4291(17) . ? O3 C4 1.4309(16) . ? C1 C2 1.512(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.529(2) . ? C3 C4 1.519(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.502(2) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.500(2) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.518(2) . ? C8 C9 1.5194(19) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.513(2) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 P1 C2 113.21(12) . . ? O4 P1 C9 114.11(12) . . ? C2 P1 C9 94.08(6) . . ? O4 P1 P1 116.42(11) . 2_755 ? C2 P1 P1 115.64(4) . 2_755 ? C9 P1 P1 100.40(5) . 2_755 ? C7 O1 C2 115.81(10) . . ? C4 O2 C9 115.64(10) . . ? C7 O3 C4 111.83(10) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C1 106.74(12) . . ? O1 C2 C3 108.68(11) . . ? C1 C2 C3 111.59(11) . . ? O1 C2 P1 112.70(9) . . ? C1 C2 P1 113.65(10) . . ? C3 C2 P1 103.48(9) . . ? C4 C3 C2 111.18(11) . . ? C4 C3 H3A 109.4 . . ? C2 C3 H3A 109.4 . . ? C4 C3 H3B 109.4 . . ? C2 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? O2 C4 O3 110.17(10) . . ? O2 C4 C5 106.43(11) . . ? O3 C4 C5 107.33(11) . . ? O2 C4 C3 111.19(11) . . ? O3 C4 C3 108.03(11) . . ? C5 C4 C3 113.61(12) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O3 C7 O1 109.89(11) . . ? O3 C7 C6 107.25(12) . . ? O1 C7 C6 106.02(12) . . ? O3 C7 C8 108.36(11) . . ? O1 C7 C8 111.83(11) . . ? C6 C7 C8 113.36(12) . . ? C7 C8 C9 110.70(11) . . ? C7 C8 H8A 109.5 . . ? C9 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? O2 C9 C10 105.25(11) . . ? O2 C9 C8 108.49(11) . . ? C10 C9 C8 113.42(12) . . ? O2 C9 P1 106.37(9) . . ? C10 C9 P1 112.04(10) . . ? C8 C9 P1 110.80(10) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 O1 C2 C1 -171.60(11) . . . . ? C7 O1 C2 C3 -51.12(15) . . . . ? C7 O1 C2 P1 62.97(13) . . . . ? O4 P1 C2 O1 -171.33(14) . . . . ? C9 P1 C2 O1 -52.89(10) . . . . ? P1 P1 C2 O1 50.70(11) 2_755 . . . ? O4 P1 C2 C1 67.08(16) . . . . ? C9 P1 C2 C1 -174.49(10) . . . . ? P1 P1 C2 C1 -70.90(11) 2_755 . . . ? O4 P1 C2 C3 -54.12(15) . . . . ? C9 P1 C2 C3 64.31(9) . . . . ? P1 P1 C2 C3 167.90(7) 2_755 . . . ? O1 C2 C3 C4 50.17(15) . . . . ? C1 C2 C3 C4 167.60(12) . . . . ? P1 C2 C3 C4 -69.82(12) . . . . ? C9 O2 C4 O3 55.80(15) . . . . ? C9 O2 C4 C5 171.85(11) . . . . ? C9 O2 C4 C3 -63.94(14) . . . . ? C7 O3 C4 O2 -60.02(14) . . . . ? C7 O3 C4 C5 -175.51(11) . . . . ? C7 O3 C4 C3 61.62(14) . . . . ? C2 C3 C4 O2 64.95(14) . . . . ? C2 C3 C4 O3 -56.06(14) . . . . ? C2 C3 C4 C5 -175.01(12) . . . . ? C4 O3 C7 O1 -61.14(14) . . . . ? C4 O3 C7 C6 -175.96(11) . . . . ? C4 O3 C7 C8 61.32(13) . . . . ? C2 O1 C7 O3 56.46(15) . . . . ? C2 O1 C7 C6 172.05(11) . . . . ? C2 O1 C7 C8 -63.93(14) . . . . ? O3 C7 C8 C9 -57.16(14) . . . . ? O1 C7 C8 C9 64.12(15) . . . . ? C6 C7 C8 C9 -176.09(12) . . . . ? C4 O2 C9 C10 -173.51(11) . . . . ? C4 O2 C9 C8 -51.79(14) . . . . ? C4 O2 C9 P1 67.45(12) . . . . ? C7 C8 C9 O2 51.40(14) . . . . ? C7 C8 C9 C10 167.97(12) . . . . ? C7 C8 C9 P1 -65.02(13) . . . . ? O4 P1 C9 O2 54.87(15) . . . . ? C2 P1 C9 O2 -62.82(9) . . . . ? P1 P1 C9 O2 -179.83(7) 2_755 . . . ? O4 P1 C9 C10 -59.63(16) . . . . ? C2 P1 C9 C10 -177.32(10) . . . . ? P1 P1 C9 C10 65.67(10) 2_755 . . . ? O4 P1 C9 C8 172.60(14) . . . . ? C2 P1 C9 C8 54.90(10) . . . . ? P1 P1 C9 C8 -62.11(10) 2_755 . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.19 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.377 _refine_diff_density_min -0.268 _refine_diff_density_rms 0.057 data_1b _database_code_depnum_ccdc_archive 'CCDC 815350' #TrackingRef '- Diphosphanes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H32 O8 P2' _chemical_formula_sum 'C20 H32 O8 P2' _chemical_formula_weight 462.40 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 12.0015(10) _cell_length_b 12.7265(11) _cell_length_c 14.6537(13) _cell_angle_alpha 90.00 _cell_angle_beta 104.510(2) _cell_angle_gamma 90.00 _cell_volume 2166.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7122 _cell_measurement_theta_min 2.69 _cell_measurement_theta_max 27.51 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.417 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 0.246 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.952 _exptl_absorpt_correction_T_max 0.976 _exptl_absorpt_process_details 'SADABS V2.10' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.2 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6949 _diffrn_reflns_av_R_equivalents 0.0223 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 27.50 _reflns_number_total 2494 _reflns_number_gt 1955 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0596P)^2^+0.1581P] 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 2494 _refine_ls_number_parameters 140 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0483 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.1036 _refine_ls_wR_factor_gt 0.0996 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 1.04711(4) 0.23534(3) 0.32957(3) 0.02049(14) Uani 1 1 d . . . O1 O 0.92707(9) 0.40075(9) 0.36923(8) 0.0213(3) Uani 1 1 d . . . O2 O 0.99686(10) 0.17249(9) 0.48819(8) 0.0238(3) Uani 1 1 d . . . O3 O 0.89705(10) 0.32661(9) 0.50904(8) 0.0230(3) Uani 1 1 d . . . O4 O 1.16249(11) 0.18608(10) 0.34713(9) 0.0312(3) Uani 1 1 d . . . C1 C 1.11785(15) 0.44773(13) 0.35689(13) 0.0265(4) Uani 1 1 d . . . H1A H 1.0895 0.4592 0.2889 0.040 Uiso 1 1 calc R . . H1B H 1.1982 0.4243 0.3711 0.040 Uiso 1 1 calc R . . H1C H 1.1129 0.5135 0.3904 0.040 Uiso 1 1 calc R . . C2 C 1.04512(13) 0.36442(13) 0.38830(12) 0.0213(4) Uani 1 1 d . . . C3 C 1.08955(14) 0.34365(13) 0.49397(12) 0.0244(4) Uani 1 1 d . . . H3A H 1.1655 0.3087 0.5061 0.029 Uiso 1 1 calc R . . H3B H 1.0997 0.4114 0.5283 0.029 Uiso 1 1 calc R . . C4 C 1.00710(14) 0.27515(13) 0.53014(12) 0.0238(4) Uani 1 1 d . . . C5 C 1.04411(17) 0.25878(16) 0.63565(12) 0.0327(4) Uani 1 1 d . . . H5A H 1.0495 0.3269 0.6676 0.049 Uiso 1 1 calc R . . H5B H 1.1194 0.2241 0.6523 0.049 Uiso 1 1 calc R . . H5C H 0.9874 0.2147 0.6554 0.049 Uiso 1 1 calc R . . C6 C 0.74072(14) 0.40129(14) 0.39496(13) 0.0263(4) Uani 1 1 d . . . H6A H 0.6882 0.3659 0.4265 0.039 Uiso 1 1 calc R . . H6B H 0.7044 0.4067 0.3273 0.039 Uiso 1 1 calc R . . H6C H 0.7582 0.4718 0.4215 0.039 Uiso 1 1 calc R . . C7 C 0.85065(14) 0.33883(13) 0.40968(11) 0.0209(3) Uani 1 1 d . . . C8 C 0.83158(14) 0.22954(12) 0.36609(12) 0.0206(3) Uani 1 1 d . . . H8A H 0.8006 0.2356 0.2970 0.025 Uiso 1 1 calc R . . H8B H 0.7745 0.1912 0.3919 0.025 Uiso 1 1 calc R . . C9 C 0.94469(14) 0.16854(12) 0.38740(11) 0.0210(3) Uani 1 1 d . . . C10 C 0.93121(16) 0.05278(13) 0.36208(13) 0.0275(4) Uani 1 1 d . . . H10A H 1.0073 0.0199 0.3740 0.041 Uiso 1 1 calc R . . H10B H 0.8917 0.0453 0.2952 0.041 Uiso 1 1 calc R . . H10C H 0.8859 0.0184 0.4006 0.041 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 P1 0.0184(2) 0.0188(2) 0.0248(2) -0.00210(17) 0.00648(17) -0.00138(16) O1 0.0186(6) 0.0214(5) 0.0256(6) -0.0002(5) 0.0090(5) -0.0010(4) O2 0.0260(6) 0.0231(6) 0.0207(6) 0.0008(5) 0.0026(5) -0.0016(5) O3 0.0211(6) 0.0286(6) 0.0196(6) -0.0033(5) 0.0058(5) -0.0011(5) O4 0.0251(7) 0.0340(7) 0.0338(7) -0.0022(6) 0.0060(5) 0.0033(5) C1 0.0262(9) 0.0239(8) 0.0319(10) -0.0057(7) 0.0119(8) -0.0086(7) C2 0.0174(8) 0.0214(8) 0.0261(9) -0.0050(7) 0.0074(7) -0.0033(6) C3 0.0195(8) 0.0257(8) 0.0276(9) -0.0050(7) 0.0048(7) -0.0040(7) C4 0.0221(9) 0.0278(8) 0.0206(8) -0.0017(7) 0.0035(6) -0.0020(7) C5 0.0315(10) 0.0435(10) 0.0202(9) -0.0012(8) 0.0012(7) -0.0063(8) C6 0.0205(8) 0.0292(9) 0.0299(10) -0.0017(7) 0.0078(7) 0.0008(7) C7 0.0189(8) 0.0252(8) 0.0196(8) -0.0011(6) 0.0067(6) -0.0029(6) C8 0.0193(8) 0.0226(8) 0.0205(8) -0.0014(6) 0.0060(6) -0.0039(6) C9 0.0222(8) 0.0208(7) 0.0203(8) 0.0000(6) 0.0056(6) -0.0040(6) C10 0.0323(10) 0.0195(8) 0.0304(10) 0.0001(7) 0.0070(8) -0.0047(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 O4 1.4827(13) . ? P1 C2 1.8574(16) . ? P1 C9 1.8638(17) . ? P1 P1 2.3229(9) 2_755 ? O1 C7 1.4443(19) . ? O1 C2 1.4494(19) . ? O2 C4 1.436(2) . ? O2 C9 1.453(2) . ? O3 C7 1.4311(19) . ? O3 C4 1.437(2) . ? C1 C2 1.516(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.529(2) . ? C3 C4 1.511(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.512(2) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.509(2) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.524(2) . ? C8 C9 1.527(2) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.518(2) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 P1 C2 114.42(7) . . ? O4 P1 C9 114.96(8) . . ? C2 P1 C9 96.10(7) . . ? O4 P1 P1 111.88(6) . 2_755 ? C2 P1 P1 113.93(5) . 2_755 ? C9 P1 P1 104.23(5) . 2_755 ? C7 O1 C2 115.94(12) . . ? C4 O2 C9 115.81(12) . . ? C7 O3 C4 111.77(12) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C1 109.12(14) . . ? O1 C2 C3 109.05(13) . . ? C1 C2 C3 110.31(13) . . ? O1 C2 P1 108.56(10) . . ? C1 C2 P1 113.74(12) . . ? C3 C2 P1 105.94(11) . . ? C4 C3 C2 111.23(13) . . ? C4 C3 H3A 109.4 . . ? C2 C3 H3A 109.4 . . ? C4 C3 H3B 109.4 . . ? C2 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? O2 C4 O3 110.31(12) . . ? O2 C4 C3 111.60(14) . . ? O3 C4 C3 108.00(14) . . ? O2 C4 C5 106.50(14) . . ? O3 C4 C5 107.55(14) . . ? C3 C4 C5 112.82(14) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O3 C7 O1 110.59(12) . . ? O3 C7 C6 107.82(13) . . ? O1 C7 C6 106.04(13) . . ? O3 C7 C8 107.85(13) . . ? O1 C7 C8 111.73(13) . . ? C6 C7 C8 112.76(13) . . ? C7 C8 C9 110.24(13) . . ? C7 C8 H8A 109.6 . . ? C9 C8 H8A 109.6 . . ? C7 C8 H8B 109.6 . . ? C9 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? O2 C9 C10 105.93(13) . . ? O2 C9 C8 108.96(13) . . ? C10 C9 C8 114.13(13) . . ? O2 C9 P1 106.31(10) . . ? C10 C9 P1 111.93(12) . . ? C8 C9 P1 109.21(11) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 O1 C2 C1 -169.66(13) . . . . ? C7 O1 C2 C3 -49.11(16) . . . . ? C7 O1 C2 P1 65.88(14) . . . . ? O4 P1 C2 O1 -177.14(10) . . . . ? C9 P1 C2 O1 -56.17(12) . . . . ? P1 P1 C2 O1 52.36(12) 2_755 . . . ? O4 P1 C2 C1 61.19(15) . . . . ? C9 P1 C2 C1 -177.85(12) . . . . ? P1 P1 C2 C1 -69.31(13) 2_755 . . . ? O4 P1 C2 C3 -60.14(13) . . . . ? C9 P1 C2 C3 60.83(11) . . . . ? P1 P1 C2 C3 169.36(9) 2_755 . . . ? O1 C2 C3 C4 50.46(17) . . . . ? C1 C2 C3 C4 170.28(14) . . . . ? P1 C2 C3 C4 -66.20(15) . . . . ? C9 O2 C4 O3 54.29(17) . . . . ? C9 O2 C4 C3 -65.77(17) . . . . ? C9 O2 C4 C5 170.71(14) . . . . ? C7 O3 C4 O2 -60.02(16) . . . . ? C7 O3 C4 C3 62.18(16) . . . . ? C7 O3 C4 C5 -175.79(13) . . . . ? C2 C3 C4 O2 63.97(17) . . . . ? C2 C3 C4 O3 -57.44(17) . . . . ? C2 C3 C4 C5 -176.16(15) . . . . ? C4 O3 C7 O1 -59.79(16) . . . . ? C4 O3 C7 C6 -175.31(13) . . . . ? C4 O3 C7 C8 62.65(16) . . . . ? C2 O1 C7 O3 53.82(16) . . . . ? C2 O1 C7 C6 170.44(12) . . . . ? C2 O1 C7 C8 -66.33(17) . . . . ? O3 C7 C8 C9 -58.34(16) . . . . ? O1 C7 C8 C9 63.40(17) . . . . ? C6 C7 C8 C9 -177.27(13) . . . . ? C4 O2 C9 C10 -173.81(13) . . . . ? C4 O2 C9 C8 -50.62(17) . . . . ? C4 O2 C9 P1 66.96(14) . . . . ? C7 C8 C9 O2 51.60(16) . . . . ? C7 C8 C9 C10 169.75(14) . . . . ? C7 C8 C9 P1 -64.13(15) . . . . ? O4 P1 C9 O2 60.68(12) . . . . ? C2 P1 C9 O2 -59.87(11) . . . . ? P1 P1 C9 O2 -176.48(8) 2_755 . . . ? O4 P1 C9 C10 -54.54(14) . . . . ? C2 P1 C9 C10 -175.09(12) . . . . ? P1 P1 C9 C10 68.30(12) 2_755 . . . ? O4 P1 C9 C8 178.10(10) . . . . ? C2 P1 C9 C8 57.54(12) . . . . ? P1 P1 C9 C8 -59.07(11) 2_755 . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.309 _refine_diff_density_min -0.258 _refine_diff_density_rms 0.058 data_2 _database_code_depnum_ccdc_archive 'CCDC 815351' #TrackingRef '- Diphosphanes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H28 P2' _chemical_formula_sum 'C16 H28 P2' _chemical_formula_weight 282.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.5859(7) _cell_length_b 9.9499(11) _cell_length_c 11.4318(12) _cell_angle_alpha 89.916(5) _cell_angle_beta 89.400(5) _cell_angle_gamma 86.605(6) _cell_volume 747.76(14) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7959 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 27.58 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.151 _exptl_crystal_size_mid 0.143 _exptl_crystal_size_min 0.033 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.254 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 308 _exptl_absorpt_coefficient_mu 0.273 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6849 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'SADABS 2008/2 (Sheldrick, G.M., 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.366 _diffrn_detector_type 'Bruker-AXS SMART APEX' _diffrn_measurement_details 'frames, 0.3\% width' _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Bruker-AXS Kappa' _diffrn_measurement_method '\w & \f scans' _diffrn_measurement_specimen_support ; glass fibre ; _diffrn_radiation_collimation '0.5 mm double pinhole' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe X-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71074 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 40 _diffrn_source_power 2 _diffrn_source_size '0.4 x 8 mm fine focus' _diffrn_source_target Mo _diffrn_source_type 'Bruker-AXS KFF Mo 2K 90\% Ceramic' _diffrn_source_voltage 50 _diffrn_reflns_number 15568 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_sigmaI/netI 0.0240 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 27.61 _reflns_number_total 3456 _reflns_number_gt 3097 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex II (Bruker-AXS, 2007)' _computing_cell_refinement 'Apex II (Bruker-AXS, 2007)' _computing_data_reduction ; SAINT v7.34A (Bruker-AXS, 2007) & XPREP v2005/4 (Bruker-AXS, 2005) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; In the final difference map of the crystal structure there is a significant residual peak of 1.81 e-A-3 on P2 which may due to the oxidized species also being present in the solid-state. Attempts to refine this as an oxygen atom in the structure resulted in an occupancy of 0.135, but also an unacceptably short P=O bond distance and hence has been omitted from the model although including the partial oxygen atom improved the R-factor to 0.0303. Despite the monoclinic unit cell dimensions, the structure is triclinic. 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^)+(0.0458P)^2^+0.7673P] 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 3456 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0435 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.1033 _refine_ls_wR_factor_gt 0.1001 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.98038(7) 0.38976(4) -0.00532(4) 0.01412(12) Uani 1 1 d . . . C1 C 1.1961(2) 0.31886(17) 0.08424(15) 0.0155(3) Uani 1 1 d . . . H1 H 1.3209 0.3274 0.0381 0.019 Uiso 1 1 calc R . . C2 C 1.2237(3) 0.39159(18) 0.20100(15) 0.0179(3) Uani 1 1 d . . . H2A H 1.3361 0.3457 0.2418 0.021 Uiso 1 1 calc R . . H2B H 1.2624 0.4822 0.1840 0.021 Uiso 1 1 calc R . . C3 C 1.0388(3) 0.40147(18) 0.28428(15) 0.0188(4) Uani 1 1 d . . . H3A H 1.0302 0.3156 0.3237 0.023 Uiso 1 1 calc R . . H3B H 1.0625 0.4682 0.3436 0.023 Uiso 1 1 calc R . . C4 C 0.8329(3) 0.43838(17) 0.22767(14) 0.0169(3) Uani 1 1 d . . . H4A H 0.8241 0.5345 0.2128 0.020 Uiso 1 1 calc R . . H4B H 0.7265 0.4200 0.2838 0.020 Uiso 1 1 calc R . . C5 C 0.7885(2) 0.36594(17) 0.11300(14) 0.0149(3) Uani 1 1 d . . . H5 H 0.6573 0.4039 0.0847 0.018 Uiso 1 1 calc R . . C6 C 0.7719(3) 0.21227(17) 0.12456(16) 0.0180(3) Uani 1 1 d . . . H6A H 0.6661 0.1960 0.1816 0.022 Uiso 1 1 calc R . . H6B H 0.7286 0.1780 0.0500 0.022 Uiso 1 1 calc R . . C7 C 0.9668(3) 0.13122(17) 0.16083(15) 0.0175(3) Uani 1 1 d . . . H7A H 0.9471 0.0364 0.1488 0.021 Uiso 1 1 calc R . . H7B H 0.9863 0.1444 0.2439 0.021 Uiso 1 1 calc R . . C8 C 1.1625(3) 0.16661(17) 0.09569(16) 0.0179(3) Uani 1 1 d . . . H8A H 1.1605 0.1283 0.0178 0.021 Uiso 1 1 calc R . . H8B H 1.2779 0.1238 0.1360 0.021 Uiso 1 1 calc R . . P2 P 0.53463(7) 0.01403(4) 0.59409(4) 0.01456(12) Uani 1 1 d . . . C9 C 0.7103(2) 0.15374(17) 0.58928(14) 0.0146(3) Uani 1 1 d . . . H9 H 0.8420 0.1164 0.5597 0.017 Uiso 1 1 calc R . . C10 C 0.6398(3) 0.26956(17) 0.50729(14) 0.0158(3) Uani 1 1 d . . . H10A H 0.7374 0.3387 0.5115 0.019 Uiso 1 1 calc R . . H10B H 0.6431 0.2356 0.4277 0.019 Uiso 1 1 calc R . . C11 C 0.4270(3) 0.33547(17) 0.53194(15) 0.0158(3) Uani 1 1 d . . . H11A H 0.3855 0.3880 0.4638 0.019 Uiso 1 1 calc R . . H11B H 0.4372 0.3979 0.5964 0.019 Uiso 1 1 calc R . . C12 C 0.2576(2) 0.24083(17) 0.56172(15) 0.0154(3) Uani 1 1 d . . . H12A H 0.2102 0.2039 0.4891 0.019 Uiso 1 1 calc R . . H12B H 0.1445 0.2943 0.5962 0.019 Uiso 1 1 calc R . . C13 C 0.3126(2) 0.12288(16) 0.64492(14) 0.0139(3) Uani 1 1 d . . . H13 H 0.1953 0.0668 0.6489 0.017 Uiso 1 1 calc R . . C14 C 0.3622(3) 0.16342(17) 0.77151(14) 0.0155(3) Uani 1 1 d . . . H14A H 0.2443 0.2133 0.8045 0.019 Uiso 1 1 calc R . . H14B H 0.3852 0.0821 0.8175 0.019 Uiso 1 1 calc R . . C15 C 0.5474(3) 0.24868(17) 0.78392(14) 0.0156(3) Uani 1 1 d . . . H15A H 0.5789 0.2553 0.8663 0.019 Uiso 1 1 calc R . . H15B H 0.5109 0.3389 0.7561 0.019 Uiso 1 1 calc R . . C16 C 0.7400(3) 0.19528(17) 0.71819(15) 0.0161(3) Uani 1 1 d . . . H16A H 0.7982 0.1178 0.7603 0.019 Uiso 1 1 calc R . . H16B H 0.8382 0.2641 0.7198 0.019 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 P1 0.0170(2) 0.0134(2) 0.0123(2) 0.00233(15) 0.00014(15) -0.00374(16) C1 0.0117(7) 0.0169(8) 0.0181(8) 0.0016(6) 0.0033(6) -0.0019(6) C2 0.0145(8) 0.0187(8) 0.0205(8) 0.0001(6) -0.0045(6) -0.0013(6) C3 0.0226(9) 0.0194(9) 0.0140(8) 0.0005(6) -0.0017(6) 0.0015(7) C4 0.0170(8) 0.0176(8) 0.0157(8) 0.0029(6) 0.0046(6) 0.0018(6) C5 0.0102(7) 0.0161(8) 0.0184(8) 0.0066(6) -0.0004(6) -0.0008(6) C6 0.0149(8) 0.0176(8) 0.0221(8) 0.0067(6) -0.0009(6) -0.0058(6) C7 0.0187(8) 0.0140(8) 0.0201(8) 0.0045(6) -0.0011(6) -0.0029(6) C8 0.0171(8) 0.0150(8) 0.0212(8) 0.0027(6) 0.0008(6) 0.0014(6) P2 0.0183(2) 0.0122(2) 0.0132(2) -0.00005(15) -0.00098(15) -0.00038(16) C9 0.0112(7) 0.0168(8) 0.0156(8) -0.0013(6) 0.0007(6) -0.0002(6) C10 0.0165(8) 0.0160(8) 0.0152(8) 0.0020(6) 0.0026(6) -0.0048(6) C11 0.0193(8) 0.0128(8) 0.0153(8) 0.0029(6) 0.0004(6) -0.0008(6) C12 0.0119(7) 0.0169(8) 0.0173(8) 0.0015(6) 0.0008(6) 0.0010(6) C13 0.0128(7) 0.0147(8) 0.0144(7) 0.0008(6) 0.0011(6) -0.0037(6) C14 0.0167(8) 0.0170(8) 0.0129(7) 0.0008(6) 0.0024(6) -0.0023(6) C15 0.0169(8) 0.0170(8) 0.0129(7) -0.0012(6) -0.0008(6) -0.0008(6) C16 0.0137(8) 0.0181(8) 0.0167(8) -0.0003(6) -0.0021(6) -0.0013(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C1 1.8640(18) . ? P1 C5 1.8657(17) . ? P1 P1 2.2277(9) 2_765 ? C1 C2 1.537(2) . ? C1 C8 1.549(2) . ? C1 H1 0.9800 . ? C2 C3 1.536(2) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.534(2) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.536(2) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.545(2) . ? C5 H5 0.9800 . ? C6 C7 1.535(2) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.540(2) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? P2 C13 1.8561(17) . ? P2 C9 1.8610(17) . ? P2 P2 2.2252(8) 2_656 ? C9 C10 1.538(2) . ? C9 C16 1.548(2) . ? C9 H9 0.9800 . ? C10 C11 1.536(2) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.537(2) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.538(2) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.546(2) . ? C13 H13 0.9800 . ? C14 C15 1.534(2) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.535(2) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 P1 C5 93.39(7) . . ? C1 P1 P1 102.15(6) . 2_765 ? C5 P1 P1 101.70(6) . 2_765 ? C2 C1 C8 114.66(14) . . ? C2 C1 P1 114.52(12) . . ? C8 C1 P1 105.40(11) . . ? C2 C1 H1 107.3 . . ? C8 C1 H1 107.3 . . ? P1 C1 H1 107.3 . . ? C3 C2 C1 116.56(14) . . ? C3 C2 H2A 108.2 . . ? C1 C2 H2A 108.2 . . ? C3 C2 H2B 108.2 . . ? C1 C2 H2B 108.2 . . ? H2A C2 H2B 107.3 . . ? C4 C3 C2 115.98(14) . . ? C4 C3 H3A 108.3 . . ? C2 C3 H3A 108.3 . . ? C4 C3 H3B 108.3 . . ? C2 C3 H3B 108.3 . . ? H3A C3 H3B 107.4 . . ? C3 C4 C5 116.52(14) . . ? C3 C4 H4A 108.2 . . ? C5 C4 H4A 108.2 . . ? C3 C4 H4B 108.2 . . ? C5 C4 H4B 108.2 . . ? H4A C4 H4B 107.3 . . ? C4 C5 C6 114.82(14) . . ? C4 C5 P1 113.95(11) . . ? C6 C5 P1 105.90(11) . . ? C4 C5 H5 107.3 . . ? C6 C5 H5 107.3 . . ? P1 C5 H5 107.3 . . ? C7 C6 C5 115.90(14) . . ? C7 C6 H6A 108.3 . . ? C5 C6 H6A 108.3 . . ? C7 C6 H6B 108.3 . . ? C5 C6 H6B 108.3 . . ? H6A C6 H6B 107.4 . . ? C6 C7 C8 115.64(14) . . ? C6 C7 H7A 108.4 . . ? C8 C7 H7A 108.4 . . ? C6 C7 H7B 108.4 . . ? C8 C7 H7B 108.4 . . ? H7A C7 H7B 107.4 . . ? C7 C8 C1 115.61(14) . . ? C7 C8 H8A 108.4 . . ? C1 C8 H8A 108.4 . . ? C7 C8 H8B 108.4 . . ? C1 C8 H8B 108.4 . . ? H8A C8 H8B 107.4 . . ? C13 P2 C9 94.24(7) . . ? C13 P2 P2 102.07(6) . 2_656 ? C9 P2 P2 102.33(6) . 2_656 ? C10 C9 C16 114.85(14) . . ? C10 C9 P2 113.56(11) . . ? C16 C9 P2 105.79(11) . . ? C10 C9 H9 107.4 . . ? C16 C9 H9 107.4 . . ? P2 C9 H9 107.4 . . ? C11 C10 C9 116.15(13) . . ? C11 C10 H10A 108.2 . . ? C9 C10 H10A 108.2 . . ? C11 C10 H10B 108.2 . . ? C9 C10 H10B 108.2 . . ? H10A C10 H10B 107.4 . . ? C10 C11 C12 116.92(14) . . ? C10 C11 H11A 108.1 . . ? C12 C11 H11A 108.1 . . ? C10 C11 H11B 108.1 . . ? C12 C11 H11B 108.1 . . ? H11A C11 H11B 107.3 . . ? C11 C12 C13 116.90(14) . . ? C11 C12 H12A 108.1 . . ? C13 C12 H12A 108.1 . . ? C11 C12 H12B 108.1 . . ? C13 C12 H12B 108.1 . . ? H12A C12 H12B 107.3 . . ? C12 C13 C14 115.24(14) . . ? C12 C13 P2 113.43(11) . . ? C14 C13 P2 105.53(11) . . ? C12 C13 H13 107.4 . . ? C14 C13 H13 107.4 . . ? P2 C13 H13 107.4 . . ? C15 C14 C13 115.26(13) . . ? C15 C14 H14A 108.5 . . ? C13 C14 H14A 108.5 . . ? C15 C14 H14B 108.5 . . ? C13 C14 H14B 108.5 . . ? H14A C14 H14B 107.5 . . ? C14 C15 C16 115.28(14) . . ? C14 C15 H15A 108.5 . . ? C16 C15 H15A 108.5 . . ? C14 C15 H15B 108.5 . . ? C16 C15 H15B 108.5 . . ? H15A C15 H15B 107.5 . . ? C15 C16 C9 115.90(14) . . ? C15 C16 H16A 108.3 . . ? C9 C16 H16A 108.3 . . ? C15 C16 H16B 108.3 . . ? C9 C16 H16B 108.3 . . ? H16A C16 H16B 107.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 P1 C1 C2 -57.37(13) . . . . ? P1 P1 C1 C2 45.37(12) 2_765 . . . ? C5 P1 C1 C8 69.59(12) . . . . ? P1 P1 C1 C8 172.34(10) 2_765 . . . ? C8 C1 C2 C3 -65.9(2) . . . . ? P1 C1 C2 C3 56.20(18) . . . . ? C1 C2 C3 C4 -43.3(2) . . . . ? C2 C3 C4 C5 44.1(2) . . . . ? C3 C4 C5 C6 64.73(19) . . . . ? C3 C4 C5 P1 -57.66(17) . . . . ? C1 P1 C5 C4 57.90(13) . . . . ? P1 P1 C5 C4 -45.26(12) 2_765 . . . ? C1 P1 C5 C6 -69.26(12) . . . . ? P1 P1 C5 C6 -172.42(10) 2_765 . . . ? C4 C5 C6 C7 -64.53(19) . . . . ? P1 C5 C6 C7 62.11(17) . . . . ? C5 C6 C7 C8 -45.9(2) . . . . ? C6 C7 C8 C1 46.5(2) . . . . ? C2 C1 C8 C7 63.8(2) . . . . ? P1 C1 C8 C7 -63.08(16) . . . . ? C13 P2 C9 C10 -58.89(12) . . . . ? P2 P2 C9 C10 44.46(12) 2_656 . . . ? C13 P2 C9 C16 67.97(12) . . . . ? P2 P2 C9 C16 171.32(10) 2_656 . . . ? C16 C9 C10 C11 -65.38(19) . . . . ? P2 C9 C10 C11 56.58(17) . . . . ? C9 C10 C11 C12 -42.4(2) . . . . ? C10 C11 C12 C13 42.0(2) . . . . ? C11 C12 C13 C14 66.24(19) . . . . ? C11 C12 C13 P2 -55.56(17) . . . . ? C9 P2 C13 C12 58.07(13) . . . . ? P2 P2 C13 C12 -45.51(12) 2_656 . . . ? C9 P2 C13 C14 -69.00(11) . . . . ? P2 P2 C13 C14 -172.58(9) 2_656 . . . ? C12 C13 C14 C15 -62.19(19) . . . . ? P2 C13 C14 C15 63.77(16) . . . . ? C13 C14 C15 C16 -48.5(2) . . . . ? C14 C15 C16 C9 47.7(2) . . . . ? C10 C9 C16 C15 64.22(19) . . . . ? P2 C9 C16 C15 -61.86(16) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.61 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.809 _refine_diff_density_min -0.206 _refine_diff_density_rms 0.064 data_3 _database_code_depnum_ccdc_archive 'CCDC 815352' #TrackingRef '- Diphosphanes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H30 O3 P2' _chemical_formula_sum 'C18 H30 O3 P2' _chemical_formula_weight 356.36 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.9995(5) _cell_length_b 10.3237(2) _cell_length_c 8.6944(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.5160(10) _cell_angle_gamma 90.00 _cell_volume 1793.39(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 30294 _cell_measurement_theta_min 2.84 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.410 _exptl_crystal_size_mid 0.191 _exptl_crystal_size_min 0.094 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.320 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 0.255 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7020 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'SADABS 2008/2 (Sheldrick, G.M., 2008)' _diffrn_ambient_temperature 100 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.366 _diffrn_detector_type 'Bruker-AXS SMART APEX' _diffrn_measurement_details 'frames, 0.3\% width' _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Bruker-AXS Kappa' _diffrn_measurement_method '\w & \f scans' _diffrn_measurement_specimen_support ; glass fibre ; _diffrn_radiation_collimation '0.5 mm double pinhole' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe X-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71074 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 40 _diffrn_source_power 2 _diffrn_source_size '0.4 x 8 mm fine focus' _diffrn_source_target Mo _diffrn_source_type 'Bruker-AXS KFF Mo 2K 90\% Ceramic' _diffrn_source_voltage 50 _diffrn_reflns_number 29347 _diffrn_reflns_av_R_equivalents 0.0302 _diffrn_reflns_av_sigmaI/netI 0.0193 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.20 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4112 _reflns_number_gt 3603 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex II (Bruker-AXS, 2007)' _computing_cell_refinement 'Apex II (Bruker-AXS, 2007)' _computing_data_reduction ; SAINT v7.34A (Bruker-AXS, 2007) & XPREP v2005/4 (Bruker-AXS, 2005) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Six low angle disagreeable reflections omitted: 2 0 0, 3 0 0, 1 0 0, 1 1 0, 2 1 0 and 0 1 1 . 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^)+(0.0434P)^2^+0.7600P] 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 4112 _refine_ls_number_parameters 212 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0356 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0841 _refine_ls_wR_factor_gt 0.0807 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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 P1 P 0.265041(15) 1.06877(3) 0.46569(4) 0.01213(9) Uani 1 1 d . . . P2 P 0.204681(15) 0.93580(3) 0.31216(4) 0.01368(9) Uani 1 1 d . . . O1 O 0.36792(4) 0.90391(8) 0.37124(9) 0.01183(18) Uani 1 1 d . . . O2 O 0.34430(4) 1.03841(8) 0.71849(10) 0.01311(18) Uani 1 1 d . . . O3 O 0.42569(4) 0.90622(8) 0.61217(10) 0.01241(18) Uani 1 1 d . . . C1 C 0.34974(6) 1.08998(12) 0.21621(14) 0.0157(2) Uani 1 1 d . . . H1A H 0.3944 1.0856 0.1804 0.024 Uiso 1 1 calc R . . H1B H 0.3347 1.1783 0.2138 0.024 Uiso 1 1 calc R . . H1C H 0.3205 1.0382 0.1509 0.024 Uiso 1 1 calc R . . C2 C 0.34919(6) 1.03924(11) 0.38001(14) 0.0119(2) Uani 1 1 d . . . C3 C 0.40036(6) 1.10781(12) 0.48777(14) 0.0129(2) Uani 1 1 d . . . H3A H 0.4436 1.1096 0.4413 0.015 Uiso 1 1 calc R . . H3B H 0.3864 1.1965 0.5043 0.015 Uiso 1 1 calc R . . C4 C 0.40624(6) 1.03645(12) 0.64127(14) 0.0128(2) Uani 1 1 d . . . C5 C 0.45843(6) 1.09260(12) 0.75277(15) 0.0158(2) Uani 1 1 d . . . H5A H 0.4596 1.0435 0.8466 0.024 Uiso 1 1 calc R . . H5B H 0.4475 1.1811 0.7743 0.024 Uiso 1 1 calc R . . H5C H 0.5015 1.0889 0.7083 0.024 Uiso 1 1 calc R . . C6 C 0.40616(6) 0.70771(12) 0.48600(14) 0.0147(2) Uani 1 1 d . . . H6A H 0.3741 0.6570 0.4267 0.022 Uiso 1 1 calc R . . H6B H 0.4167 0.6651 0.5821 0.022 Uiso 1 1 calc R . . H6C H 0.4461 0.7172 0.4298 0.022 Uiso 1 1 calc R . . C7 C 0.37713(6) 0.83924(11) 0.51629(13) 0.0118(2) Uani 1 1 d . . . C8 C 0.31198(6) 0.83306(11) 0.60064(14) 0.0125(2) Uani 1 1 d . . . H8A H 0.2777 0.7913 0.5356 0.015 Uiso 1 1 calc R . . H8B H 0.3186 0.7818 0.6935 0.015 Uiso 1 1 calc R . . C9 C 0.28899(6) 0.96882(12) 0.64248(14) 0.0128(2) Uani 1 1 d . . . C10 C 0.23522(6) 0.96775(13) 0.76009(14) 0.0163(3) Uani 1 1 d . . . H10A H 0.2524 0.9274 0.8531 0.024 Uiso 1 1 calc R . . H10B H 0.1971 0.9201 0.7199 0.024 Uiso 1 1 calc R . . H10C H 0.2221 1.0551 0.7817 0.024 Uiso 1 1 calc R . . C11 C 0.12597(6) 0.90750(12) 0.41479(15) 0.0159(3) Uani 1 1 d . . . H11 H 0.1369 0.8480 0.5000 0.019 Uiso 1 1 calc R . . C12 C 0.07864(6) 0.83423(13) 0.29893(15) 0.0193(3) Uani 1 1 d . . . H12A H 0.0997 0.7528 0.2738 0.023 Uiso 1 1 calc R . . H12B H 0.0378 0.8138 0.3501 0.023 Uiso 1 1 calc R . . C13 C 0.05927(7) 0.90456(14) 0.14704(15) 0.0201(3) Uani 1 1 d . . . H13A H 0.0395 0.8419 0.0755 0.024 Uiso 1 1 calc R . . H13B H 0.0252 0.9684 0.1674 0.024 Uiso 1 1 calc R . . C14 C 0.11684(7) 0.97293(14) 0.06885(15) 0.0207(3) Uani 1 1 d . . . H14A H 0.0979 1.0288 -0.0115 0.025 Uiso 1 1 calc R . . H14B H 0.1436 0.9078 0.0196 0.025 Uiso 1 1 calc R . . C15 C 0.16361(7) 1.05502(13) 0.17590(15) 0.0193(3) Uani 1 1 d . . . H15 H 0.1986 1.0908 0.1128 0.023 Uiso 1 1 calc R . . C16 C 0.12953(7) 1.16971(13) 0.25425(17) 0.0257(3) Uani 1 1 d . . . H16A H 0.1641 1.2212 0.3069 0.031 Uiso 1 1 calc R . . H16B H 0.1087 1.2238 0.1744 0.031 Uiso 1 1 calc R . . C17 C 0.07649(7) 1.13698(14) 0.37007(17) 0.0259(3) Uani 1 1 d . . . H17A H 0.0666 1.2147 0.4274 0.031 Uiso 1 1 calc R . . H17B H 0.0357 1.1112 0.3136 0.031 Uiso 1 1 calc R . . C18 C 0.09623(6) 1.02970(14) 0.48439(16) 0.0208(3) Uani 1 1 d . . . H18A H 0.0569 1.0051 0.5388 0.025 Uiso 1 1 calc R . . H18B H 0.1286 1.0647 0.5597 0.025 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 P1 0.01103(16) 0.01247(16) 0.01286(16) 0.00052(11) 0.00026(11) 0.00032(11) P2 0.01203(16) 0.01451(16) 0.01446(17) -0.00071(12) -0.00003(12) 0.00011(11) O1 0.0141(4) 0.0102(4) 0.0112(4) 0.0004(3) 0.0008(3) 0.0012(3) O2 0.0110(4) 0.0160(4) 0.0124(4) -0.0024(3) 0.0010(3) -0.0011(3) O3 0.0113(4) 0.0117(4) 0.0141(4) -0.0019(3) -0.0014(3) -0.0006(3) C1 0.0172(6) 0.0160(6) 0.0141(6) 0.0022(5) 0.0019(5) -0.0011(5) C2 0.0119(5) 0.0102(5) 0.0135(6) 0.0003(4) 0.0006(4) 0.0005(4) C3 0.0124(5) 0.0112(5) 0.0151(6) -0.0006(4) 0.0016(4) -0.0013(4) C4 0.0105(5) 0.0129(6) 0.0149(6) -0.0016(4) 0.0009(4) -0.0001(4) C5 0.0142(6) 0.0167(6) 0.0165(6) -0.0030(5) -0.0012(5) -0.0012(5) C6 0.0164(6) 0.0122(6) 0.0153(6) -0.0002(4) -0.0009(4) 0.0015(4) C7 0.0128(5) 0.0120(6) 0.0105(6) 0.0007(4) -0.0012(4) -0.0007(4) C8 0.0126(5) 0.0126(6) 0.0122(6) 0.0016(4) -0.0004(4) -0.0019(4) C9 0.0110(5) 0.0147(6) 0.0125(6) 0.0003(5) -0.0001(4) -0.0010(4) C10 0.0141(6) 0.0207(6) 0.0143(6) 0.0018(5) 0.0025(5) -0.0003(5) C11 0.0138(6) 0.0186(6) 0.0153(6) 0.0015(5) 0.0005(5) -0.0010(5) C12 0.0167(6) 0.0204(6) 0.0208(7) -0.0005(5) 0.0006(5) -0.0061(5) C13 0.0161(6) 0.0252(7) 0.0186(6) -0.0030(5) -0.0028(5) -0.0025(5) C14 0.0196(6) 0.0255(7) 0.0165(6) 0.0032(5) -0.0033(5) -0.0037(5) C15 0.0195(6) 0.0210(7) 0.0172(6) 0.0051(5) -0.0030(5) -0.0049(5) C16 0.0293(7) 0.0163(6) 0.0301(8) 0.0048(6) -0.0125(6) 0.0007(6) C17 0.0238(7) 0.0243(7) 0.0287(8) -0.0084(6) -0.0087(6) 0.0105(6) C18 0.0140(6) 0.0277(7) 0.0206(7) -0.0052(5) -0.0002(5) 0.0033(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C2 1.8947(12) . ? P1 C9 1.8953(12) . ? P1 P2 2.2321(4) . ? P2 C11 1.8663(13) . ? P2 C15 1.8728(13) . ? O1 C7 1.4317(14) . ? O1 C2 1.4494(14) . ? O2 C4 1.4347(14) . ? O2 C9 1.4534(14) . ? O3 C4 1.4254(14) . ? O3 C7 1.4300(14) . ? C1 C2 1.5178(17) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.5304(16) . ? C3 C4 1.5244(17) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.5088(17) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.5046(16) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.5244(16) . ? C8 C9 1.5240(16) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.5161(16) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C18 1.5306(18) . ? C11 C12 1.5490(18) . ? C11 H11 0.9800 . ? C12 C13 1.5415(19) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.5345(18) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.5437(18) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.540(2) . ? C15 H15 0.9800 . ? C16 C17 1.532(2) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.528(2) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 P1 C9 91.95(5) . . ? C2 P1 P2 97.60(4) . . ? C9 P1 P2 105.13(4) . . ? C11 P2 C15 92.84(6) . . ? C11 P2 P1 104.82(4) . . ? C15 P2 P1 100.65(4) . . ? C7 O1 C2 115.26(9) . . ? C4 O2 C9 115.83(9) . . ? C4 O3 C7 112.07(9) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C1 105.71(9) . . ? O1 C2 C3 108.09(9) . . ? C1 C2 C3 112.49(10) . . ? O1 C2 P1 114.32(8) . . ? C1 C2 P1 110.89(8) . . ? C3 C2 P1 105.46(8) . . ? C4 C3 C2 109.65(10) . . ? C4 C3 H3A 109.7 . . ? C2 C3 H3A 109.7 . . ? C4 C3 H3B 109.7 . . ? C2 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? O3 C4 O2 110.14(9) . . ? O3 C4 C5 106.85(9) . . ? O2 C4 C5 106.32(10) . . ? O3 C4 C3 108.16(9) . . ? O2 C4 C3 111.59(9) . . ? C5 C4 C3 113.67(10) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O3 C7 O1 110.23(9) . . ? O3 C7 C6 106.32(9) . . ? O1 C7 C6 107.60(9) . . ? O3 C7 C8 108.23(9) . . ? O1 C7 C8 111.33(9) . . ? C6 C7 C8 113.01(10) . . ? C9 C8 C7 110.45(9) . . ? C9 C8 H8A 109.6 . . ? C7 C8 H8A 109.6 . . ? C9 C8 H8B 109.6 . . ? C7 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? O2 C9 C10 104.19(9) . . ? O2 C9 C8 109.37(9) . . ? C10 C9 C8 112.62(10) . . ? O2 C9 P1 105.06(8) . . ? C10 C9 P1 112.92(8) . . ? C8 C9 P1 112.04(8) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C18 C11 C12 115.00(11) . . ? C18 C11 P2 114.24(9) . . ? C12 C11 P2 105.65(9) . . ? C18 C11 H11 107.2 . . ? C12 C11 H11 107.2 . . ? P2 C11 H11 107.2 . . ? C13 C12 C11 116.78(11) . . ? C13 C12 H12A 108.1 . . ? C11 C12 H12A 108.1 . . ? C13 C12 H12B 108.1 . . ? C11 C12 H12B 108.1 . . ? H12A C12 H12B 107.3 . . ? C14 C13 C12 115.53(11) . . ? C14 C13 H13A 108.4 . . ? C12 C13 H13A 108.4 . . ? C14 C13 H13B 108.4 . . ? C12 C13 H13B 108.4 . . ? H13A C13 H13B 107.5 . . ? C13 C14 C15 115.60(11) . . ? C13 C14 H14A 108.4 . . ? C15 C14 H14A 108.4 . . ? C13 C14 H14B 108.4 . . ? C15 C14 H14B 108.4 . . ? H14A C14 H14B 107.4 . . ? C16 C15 C14 114.87(11) . . ? C16 C15 P2 114.58(9) . . ? C14 C15 P2 104.95(9) . . ? C16 C15 H15 107.3 . . ? C14 C15 H15 107.3 . . ? P2 C15 H15 107.3 . . ? C17 C16 C15 116.99(11) . . ? C17 C16 H16A 108.0 . . ? C15 C16 H16A 108.0 . . ? C17 C16 H16B 108.0 . . ? C15 C16 H16B 108.0 . . ? H16A C16 H16B 107.3 . . ? C18 C17 C16 114.88(11) . . ? C18 C17 H17A 108.5 . . ? C16 C17 H17A 108.5 . . ? C18 C17 H17B 108.5 . . ? C16 C17 H17B 108.5 . . ? H17A C17 H17B 107.5 . . ? C17 C18 C11 115.72(11) . . ? C17 C18 H18A 108.4 . . ? C11 C18 H18A 108.4 . . ? C17 C18 H18B 108.4 . . ? C11 C18 H18B 108.4 . . ? H18A C18 H18B 107.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 P1 P2 C11 162.00(6) . . . . ? C9 P1 P2 C11 67.89(6) . . . . ? C2 P1 P2 C15 -102.15(6) . . . . ? C9 P1 P2 C15 163.74(6) . . . . ? C7 O1 C2 C1 174.04(9) . . . . ? C7 O1 C2 C3 53.38(12) . . . . ? C7 O1 C2 P1 -63.71(11) . . . . ? C9 P1 C2 O1 52.62(9) . . . . ? P2 P1 C2 O1 -52.93(8) . . . . ? C9 P1 C2 C1 171.99(9) . . . . ? P2 P1 C2 C1 66.45(8) . . . . ? C9 P1 C2 C3 -65.98(8) . . . . ? P2 P1 C2 C3 -171.52(7) . . . . ? O1 C2 C3 C4 -53.35(12) . . . . ? C1 C2 C3 C4 -169.68(10) . . . . ? P1 C2 C3 C4 69.33(10) . . . . ? C7 O3 C4 O2 60.53(12) . . . . ? C7 O3 C4 C5 175.61(9) . . . . ? C7 O3 C4 C3 -61.66(11) . . . . ? C9 O2 C4 O3 -54.66(12) . . . . ? C9 O2 C4 C5 -170.07(9) . . . . ? C9 O2 C4 C3 65.47(12) . . . . ? C2 C3 C4 O3 58.37(12) . . . . ? C2 C3 C4 O2 -62.92(12) . . . . ? C2 C3 C4 C5 176.85(10) . . . . ? C4 O3 C7 O1 59.68(12) . . . . ? C4 O3 C7 C6 176.01(9) . . . . ? C4 O3 C7 C8 -62.29(12) . . . . ? C2 O1 C7 O3 -56.06(12) . . . . ? C2 O1 C7 C6 -171.60(9) . . . . ? C2 O1 C7 C8 64.06(12) . . . . ? O3 C7 C8 C9 56.68(12) . . . . ? O1 C7 C8 C9 -64.62(12) . . . . ? C6 C7 C8 C9 174.15(10) . . . . ? C4 O2 C9 C10 170.71(9) . . . . ? C4 O2 C9 C8 50.09(13) . . . . ? C4 O2 C9 P1 -70.34(10) . . . . ? C7 C8 C9 O2 -50.06(12) . . . . ? C7 C8 C9 C10 -165.40(10) . . . . ? C7 C8 C9 P1 66.01(11) . . . . ? C2 P1 C9 O2 64.07(8) . . . . ? P2 P1 C9 O2 162.49(6) . . . . ? C2 P1 C9 C10 176.99(9) . . . . ? P2 P1 C9 C10 -84.59(9) . . . . ? C2 P1 C9 C8 -54.57(9) . . . . ? P2 P1 C9 C8 43.84(8) . . . . ? C15 P2 C11 C18 -58.26(10) . . . . ? P1 P2 C11 C18 43.54(10) . . . . ? C15 P2 C11 C12 69.15(9) . . . . ? P1 P2 C11 C12 170.95(7) . . . . ? C18 C11 C12 C13 66.13(15) . . . . ? P2 C11 C12 C13 -60.81(13) . . . . ? C11 C12 C13 C14 43.99(17) . . . . ? C12 C13 C14 C15 -45.84(17) . . . . ? C13 C14 C15 C16 -62.39(16) . . . . ? C13 C14 C15 P2 64.35(13) . . . . ? C11 P2 C15 C16 55.78(10) . . . . ? P1 P2 C15 C16 -49.88(10) . . . . ? C11 P2 C15 C14 -71.14(9) . . . . ? P1 P2 C15 C14 -176.79(8) . . . . ? C14 C15 C16 C17 65.57(15) . . . . ? P2 C15 C16 C17 -56.07(14) . . . . ? C15 C16 C17 C18 45.44(17) . . . . ? C16 C17 C18 C11 -47.44(16) . . . . ? C12 C11 C18 C17 -61.83(15) . . . . ? P2 C11 C18 C17 60.61(14) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.357 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.075 data_4a _database_code_depnum_ccdc_archive 'CCDC 815353' #TrackingRef '- Diphosphanes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H26 O3 P2' _chemical_formula_sum 'C22 H26 O3 P2' _chemical_formula_weight 400.37 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c a 21' _symmetry_space_group_name_Hall 'P 2c -2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 25.664(5) _cell_length_b 11.194(2) _cell_length_c 7.1808(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2062.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5999 _cell_measurement_theta_min 2.415 _cell_measurement_theta_max 26.408 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.289 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 0.230 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.882983 _exptl_absorpt_correction_T_max 0.970000 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 8.5 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 22827 _diffrn_reflns_av_R_equivalents 0.0392 _diffrn_reflns_av_sigmaI/netI 0.0315 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4751 _reflns_number_gt 4557 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART V5.054 (Bruker, 1998)' _computing_cell_refinement 'Bruker SMART V5.054 (Bruker, 1998)' _computing_data_reduction 'Bruker SAINT V6.0 (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V6.1 (Bruker AXS, 2000)' _computing_publication_material 'Bruker SHELXTL V6.1 (Bruker AXS, 2000)' _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^)+(0.0483P)^2^+0.2897P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), 2182 Friedel pairs' _refine_ls_abs_structure_Flack -0.01(7) _refine_ls_number_reflns 4751 _refine_ls_number_parameters 249 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0357 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0834 _refine_ls_wR_factor_gt 0.0825 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.121276(16) 0.16116(4) 1.01752(6) 0.01325(10) Uani 1 1 d . . . P2 P 0.085669(16) 0.21534(4) 0.74612(7) 0.01484(10) Uani 1 1 d . . . O1 O 0.19686(5) -0.00058(11) 1.08801(17) 0.0158(3) Uani 1 1 d . . . O2 O 0.07705(4) -0.05674(11) 0.91730(17) 0.0141(3) Uani 1 1 d . . . O3 O 0.14982(5) -0.17204(10) 1.00024(18) 0.0159(2) Uani 1 1 d . . . C1 C 0.22377(7) 0.15013(16) 0.8797(3) 0.0178(4) Uani 1 1 d . . . H1A H 0.2314 0.2040 0.9837 0.027 Uiso 1 1 calc R . . H1B H 0.2147 0.1972 0.7693 0.027 Uiso 1 1 calc R . . H1C H 0.2545 0.1011 0.8530 0.027 Uiso 1 1 calc R . . C2 C 0.17844(7) 0.06992(15) 0.9311(2) 0.0135(3) Uani 1 1 d . . . C3 C 0.16284(6) -0.01714(14) 0.7772(2) 0.0140(3) Uani 1 1 d . . . H3A H 0.1467 0.0274 0.6729 0.017 Uiso 1 1 calc R . . H3B H 0.1942 -0.0583 0.7292 0.017 Uiso 1 1 calc R . . C4 C 0.12434(7) -0.10904(16) 0.8521(2) 0.0148(3) Uani 1 1 d . . . C5 C 0.10797(7) -0.20140(15) 0.7110(3) 0.0182(4) Uani 1 1 d . . . H5A H 0.0849 -0.2599 0.7705 0.027 Uiso 1 1 calc R . . H5B H 0.1389 -0.2422 0.6624 0.027 Uiso 1 1 calc R . . H5C H 0.0894 -0.1622 0.6085 0.027 Uiso 1 1 calc R . . C6 C 0.19369(7) -0.16725(16) 1.2873(3) 0.0207(4) Uani 1 1 d . . . H6A H 0.1718 -0.2320 1.3353 0.031 Uiso 1 1 calc R . . H6B H 0.2050 -0.1163 1.3906 0.031 Uiso 1 1 calc R . . H6C H 0.2243 -0.2012 1.2252 0.031 Uiso 1 1 calc R . . C7 C 0.16292(7) -0.09373(15) 1.1496(2) 0.0152(3) Uani 1 1 d . . . C8 C 0.11236(7) -0.04130(16) 1.2278(2) 0.0163(3) Uani 1 1 d . . . H8A H 0.0906 -0.1062 1.2802 0.020 Uiso 1 1 calc R . . H8B H 0.1206 0.0155 1.3294 0.020 Uiso 1 1 calc R . . C9 C 0.08221(7) 0.02324(15) 1.0743(2) 0.0141(3) Uani 1 1 d . . . C10 C 0.02710(7) 0.05362(16) 1.1346(3) 0.0194(4) Uani 1 1 d . . . H10A H 0.0088 0.0930 1.0319 0.029 Uiso 1 1 calc R . . H10B H 0.0283 0.1073 1.2423 0.029 Uiso 1 1 calc R . . H10C H 0.0087 -0.0199 1.1687 0.029 Uiso 1 1 calc R . . C11 C 0.02761(7) 0.29771(14) 0.8227(3) 0.0162(4) Uani 1 1 d . . . C12 C 0.02241(7) 0.36113(15) 0.9896(3) 0.0185(4) Uani 1 1 d . . . H12 H 0.0504 0.3623 1.0763 0.022 Uiso 1 1 calc R . . C13 C -0.02327(7) 0.42231(15) 1.0294(3) 0.0232(4) Uani 1 1 d . . . H13 H -0.0264 0.4650 1.1432 0.028 Uiso 1 1 calc R . . C14 C -0.06428(7) 0.42134(16) 0.9040(3) 0.0246(4) Uani 1 1 d . . . H14 H -0.0953 0.4643 0.9311 0.029 Uiso 1 1 calc R . . C15 C -0.06015(7) 0.35751(15) 0.7384(3) 0.0229(4) Uani 1 1 d . . . H15 H -0.0884 0.3561 0.6527 0.028 Uiso 1 1 calc R . . C16 C -0.01433(7) 0.29561(15) 0.6989(3) 0.0189(4) Uani 1 1 d . . . H16 H -0.0116 0.2514 0.5864 0.023 Uiso 1 1 calc R . . C17 C 0.13134(7) 0.33757(15) 0.6882(3) 0.0178(4) Uani 1 1 d . . . C18 C 0.14275(7) 0.43327(16) 0.8067(3) 0.0201(4) Uani 1 1 d . . . H18 H 0.1258 0.4393 0.9240 0.024 Uiso 1 1 calc R . . C19 C 0.17880(7) 0.51976(17) 0.7536(3) 0.0266(4) Uani 1 1 d . . . H19 H 0.1862 0.5849 0.8342 0.032 Uiso 1 1 calc R . . C20 C 0.20393(8) 0.51090(19) 0.5836(3) 0.0309(5) Uani 1 1 d . . . H20 H 0.2287 0.5697 0.5480 0.037 Uiso 1 1 calc R . . C21 C 0.19307(8) 0.4166(2) 0.4655(3) 0.0310(5) Uani 1 1 d . . . H21 H 0.2106 0.4105 0.3493 0.037 Uiso 1 1 calc R . . C22 C 0.15652(7) 0.33048(17) 0.5163(3) 0.0238(4) Uani 1 1 d . . . H22 H 0.1487 0.2667 0.4336 0.029 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 P1 0.0155(2) 0.01229(19) 0.01200(19) -0.00131(18) 0.00154(18) -0.00070(16) P2 0.0164(2) 0.01405(19) 0.0141(2) -0.00022(19) 0.00047(18) 0.00276(16) O1 0.0162(6) 0.0173(6) 0.0140(6) 0.0038(5) -0.0029(5) -0.0020(5) O2 0.0140(6) 0.0140(6) 0.0144(6) -0.0023(5) -0.0002(5) -0.0006(4) O3 0.0203(6) 0.0126(5) 0.0149(6) 0.0007(5) -0.0026(5) 0.0012(5) C1 0.0149(8) 0.0199(9) 0.0186(9) 0.0024(7) -0.0004(7) -0.0008(7) C2 0.0138(8) 0.0145(8) 0.0121(8) 0.0005(7) -0.0013(7) 0.0010(6) C3 0.0158(8) 0.0143(7) 0.0119(8) -0.0009(6) -0.0005(6) 0.0042(6) C4 0.0163(8) 0.0144(8) 0.0136(8) -0.0003(7) -0.0011(7) 0.0024(6) C5 0.0234(9) 0.0151(8) 0.0161(10) -0.0033(7) -0.0039(7) 0.0012(7) C6 0.0227(9) 0.0215(9) 0.0178(9) 0.0046(7) -0.0038(7) -0.0016(7) C7 0.0187(8) 0.0158(8) 0.0111(8) 0.0015(7) -0.0032(7) -0.0024(7) C8 0.0207(8) 0.0165(8) 0.0116(8) 0.0015(7) 0.0019(7) -0.0032(6) C9 0.0156(8) 0.0125(7) 0.0141(8) 0.0006(6) 0.0029(6) -0.0025(6) C10 0.0163(8) 0.0204(9) 0.0216(10) 0.0011(7) 0.0057(7) -0.0011(7) C11 0.0149(8) 0.0111(8) 0.0228(9) 0.0014(7) 0.0026(7) 0.0003(6) C12 0.0182(8) 0.0156(7) 0.0216(10) -0.0031(7) 0.0012(7) -0.0016(7) C13 0.0230(9) 0.0135(8) 0.0331(11) -0.0060(8) 0.0096(9) -0.0026(7) C14 0.0168(8) 0.0138(8) 0.0430(12) 0.0022(8) 0.0090(9) 0.0015(7) C15 0.0149(8) 0.0172(8) 0.0367(11) 0.0045(9) -0.0024(9) -0.0025(6) C16 0.0206(9) 0.0131(8) 0.0230(10) 0.0020(7) -0.0010(7) -0.0022(7) C17 0.0156(8) 0.0167(8) 0.0210(9) 0.0062(7) 0.0010(7) 0.0050(6) C18 0.0185(9) 0.0190(9) 0.0227(9) 0.0037(7) -0.0019(7) 0.0021(7) C19 0.0206(9) 0.0213(9) 0.0378(11) 0.0074(10) -0.0073(9) 0.0014(7) C20 0.0175(9) 0.0284(10) 0.0469(13) 0.0207(10) 0.0025(9) 0.0020(8) C21 0.0213(10) 0.0353(11) 0.0365(12) 0.0167(10) 0.0115(9) 0.0105(8) C22 0.0231(9) 0.0234(8) 0.0249(9) 0.0053(8) 0.0043(9) 0.0104(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C9 1.8854(17) . ? P1 C2 1.8922(17) . ? P1 P2 2.2363(7) . ? P2 C11 1.8365(18) . ? P2 C17 1.8490(19) . ? O1 C7 1.429(2) . ? O1 C2 1.455(2) . ? O2 C4 1.426(2) . ? O2 C9 1.446(2) . ? O3 C7 1.426(2) . ? O3 C4 1.434(2) . ? C1 C2 1.515(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.527(2) . ? C3 C4 1.524(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.507(2) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.509(2) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.531(2) . ? C8 C9 1.529(2) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.518(2) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C16 1.396(3) . ? C11 C12 1.399(3) . ? C12 C13 1.388(3) . ? C12 H12 0.9500 . ? C13 C14 1.385(3) . ? C13 H13 0.9500 . ? C14 C15 1.391(3) . ? C14 H14 0.9500 . ? C15 C16 1.394(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C22 1.396(3) . ? C17 C18 1.399(3) . ? C18 C19 1.392(3) . ? C18 H18 0.9500 . ? C19 C20 1.385(3) . ? C19 H19 0.9500 . ? C20 C21 1.382(3) . ? C20 H20 0.9500 . ? C21 C22 1.394(3) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? 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 C9 P1 C2 92.36(8) . . ? C9 P1 P2 101.14(6) . . ? C2 P1 P2 100.21(6) . . ? C11 P2 C17 102.13(8) . . ? C11 P2 P1 101.93(6) . . ? C17 P2 P1 97.91(6) . . ? C7 O1 C2 115.96(12) . . ? C4 O2 C9 115.61(12) . . ? C7 O3 C4 111.31(12) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C1 105.10(13) . . ? O1 C2 C3 107.44(13) . . ? C1 C2 C3 113.79(14) . . ? O1 C2 P1 106.90(11) . . ? C1 C2 P1 110.81(12) . . ? C3 C2 P1 112.25(11) . . ? C4 C3 C2 110.20(13) . . ? C4 C3 H3A 109.6 . . ? C2 C3 H3A 109.6 . . ? C4 C3 H3B 109.6 . . ? C2 C3 H3B 109.6 . . ? H3A C3 H3B 108.1 . . ? O2 C4 O3 110.26(13) . . ? O2 C4 C5 105.37(14) . . ? O3 C4 C5 106.76(14) . . ? O2 C4 C3 112.97(14) . . ? O3 C4 C3 107.34(13) . . ? C5 C4 C3 113.98(14) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O3 C7 O1 111.06(13) . . ? O3 C7 C6 106.31(14) . . ? O1 C7 C6 106.37(14) . . ? O3 C7 C8 108.17(14) . . ? O1 C7 C8 110.52(14) . . ? C6 C7 C8 114.35(14) . . ? C9 C8 C7 110.22(14) . . ? C9 C8 H8A 109.6 . . ? C7 C8 H8A 109.6 . . ? C9 C8 H8B 109.6 . . ? C7 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? O2 C9 C10 106.03(14) . . ? O2 C9 C8 108.43(13) . . ? C10 C9 C8 111.82(15) . . ? O2 C9 P1 112.78(11) . . ? C10 C9 P1 111.95(12) . . ? C8 C9 P1 105.89(12) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C16 C11 C12 118.70(16) . . ? C16 C11 P2 115.25(14) . . ? C12 C11 P2 126.05(14) . . ? C13 C12 C11 120.50(18) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C14 C13 C12 120.26(19) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 120.13(17) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C14 C15 C16 119.54(18) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C15 C16 C11 120.85(18) . . ? C15 C16 H16 119.6 . . ? C11 C16 H16 119.6 . . ? C22 C17 C18 119.00(17) . . ? C22 C17 P2 116.77(15) . . ? C18 C17 P2 124.22(15) . . ? C19 C18 C17 120.31(19) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C20 C19 C18 120.1(2) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C21 C20 C19 120.11(19) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C20 C21 C22 120.2(2) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C21 C22 C17 120.2(2) . . ? C21 C22 H22 119.9 . . ? C17 C22 H22 119.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 P1 P2 C11 82.52(8) . . . . ? C2 P1 P2 C11 177.00(8) . . . . ? C9 P1 P2 C17 -173.23(8) . . . . ? C2 P1 P2 C17 -78.75(8) . . . . ? C7 O1 C2 C1 -173.13(14) . . . . ? C7 O1 C2 C3 -51.62(17) . . . . ? C7 O1 C2 P1 69.06(14) . . . . ? C9 P1 C2 O1 -61.86(11) . . . . ? P2 P1 C2 O1 -163.62(9) . . . . ? C9 P1 C2 C1 -175.86(13) . . . . ? P2 P1 C2 C1 82.38(12) . . . . ? C9 P1 C2 C3 55.70(12) . . . . ? P2 P1 C2 C3 -46.07(12) . . . . ? O1 C2 C3 C4 53.52(17) . . . . ? C1 C2 C3 C4 169.43(14) . . . . ? P1 C2 C3 C4 -63.71(15) . . . . ? C9 O2 C4 O3 56.63(18) . . . . ? C9 O2 C4 C5 171.47(13) . . . . ? C9 O2 C4 C3 -63.47(17) . . . . ? C7 O3 C4 O2 -60.93(17) . . . . ? C7 O3 C4 C5 -174.90(13) . . . . ? C7 O3 C4 C3 62.50(17) . . . . ? C2 C3 C4 O2 61.58(17) . . . . ? C2 C3 C4 O3 -60.17(16) . . . . ? C2 C3 C4 C5 -178.18(14) . . . . ? C4 O3 C7 O1 -59.50(17) . . . . ? C4 O3 C7 C6 -174.81(13) . . . . ? C4 O3 C7 C8 61.95(17) . . . . ? C2 O1 C7 O3 54.83(18) . . . . ? C2 O1 C7 C6 170.10(14) . . . . ? C2 O1 C7 C8 -65.24(17) . . . . ? O3 C7 C8 C9 -57.47(17) . . . . ? O1 C7 C8 C9 64.31(17) . . . . ? C6 C7 C8 C9 -175.70(14) . . . . ? C4 O2 C9 C10 -172.40(14) . . . . ? C4 O2 C9 C8 -52.18(18) . . . . ? C4 O2 C9 P1 64.75(16) . . . . ? C7 C8 C9 O2 51.42(17) . . . . ? C7 C8 C9 C10 167.96(14) . . . . ? C7 C8 C9 P1 -69.86(15) . . . . ? C2 P1 C9 O2 -54.49(12) . . . . ? P2 P1 C9 O2 46.40(12) . . . . ? C2 P1 C9 C10 -173.97(13) . . . . ? P2 P1 C9 C10 -73.08(13) . . . . ? C2 P1 C9 C8 63.93(12) . . . . ? P2 P1 C9 C8 164.83(10) . . . . ? C17 P2 C11 C16 107.67(14) . . . . ? P1 P2 C11 C16 -151.42(12) . . . . ? C17 P2 C11 C12 -71.86(17) . . . . ? P1 P2 C11 C12 29.05(16) . . . . ? C16 C11 C12 C13 -1.1(3) . . . . ? P2 C11 C12 C13 178.45(14) . . . . ? C11 C12 C13 C14 -0.1(3) . . . . ? C12 C13 C14 C15 0.9(3) . . . . ? C13 C14 C15 C16 -0.6(3) . . . . ? C14 C15 C16 C11 -0.6(3) . . . . ? C12 C11 C16 C15 1.4(3) . . . . ? P2 C11 C16 C15 -178.18(14) . . . . ? C11 P2 C17 C22 -131.15(14) . . . . ? P1 P2 C17 C22 124.77(13) . . . . ? C11 P2 C17 C18 50.43(17) . . . . ? P1 P2 C17 C18 -53.65(15) . . . . ? C22 C17 C18 C19 -0.2(3) . . . . ? P2 C17 C18 C19 178.22(14) . . . . ? C17 C18 C19 C20 -0.6(3) . . . . ? C18 C19 C20 C21 0.4(3) . . . . ? C19 C20 C21 C22 0.5(3) . . . . ? C20 C21 C22 C17 -1.2(3) . . . . ? C18 C17 C22 C21 1.0(3) . . . . ? P2 C17 C22 C21 -177.47(14) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.455 _refine_diff_density_min -0.200 _refine_diff_density_rms 0.055 data_5a _database_code_depnum_ccdc_archive 'CCDC 815354' #TrackingRef '- Diphosphanes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H24 P2' _chemical_formula_sum 'C20 H24 P2' _chemical_formula_weight 326.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 8.7796(3) _cell_length_b 12.3250(4) _cell_length_c 16.0889(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1740.96(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 11533 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 27.57 _exptl_crystal_description nugget _exptl_crystal_colour colourless _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.089 _exptl_crystal_size_min 0.067 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.245 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 0.245 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6353 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'SADABS 2008/2 (Sheldrick, G.M., 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.366 _diffrn_detector_type 'Bruker-AXS SMART APEX' _diffrn_measurement_details 'frames, 0.3\% width' _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Bruker-AXS Kappa' _diffrn_measurement_method '\w & \f scans' _diffrn_measurement_specimen_support ; glass fibre ; _diffrn_radiation_collimation '0.5 mm double pinhole' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe X-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71074 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 40 _diffrn_source_power 2 _diffrn_source_size '0.4 x 8 mm fine focus' _diffrn_source_target Mo _diffrn_source_type 'Bruker-AXS KFF Mo 2K 90\% Ceramic' _diffrn_source_voltage 50 _diffrn_reflns_number 11481 _diffrn_reflns_av_R_equivalents 0.0487 _diffrn_reflns_av_sigmaI/netI 0.0582 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 27.57 _reflns_number_total 3999 _reflns_number_gt 3510 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex II (Bruker-AXS, 2007)' _computing_cell_refinement 'Apex II (Bruker-AXS, 2007)' _computing_data_reduction ; SAINT v7.34A (Bruker-AXS, 2007) & XPREP v2005/4 (Bruker-AXS, 2005) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; One low angle disagreeable reflection omitted: 0 1 1. 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^)+(0.0427P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), 1710 Friedel Pairs' _refine_ls_abs_structure_Flack -0.18(10) _refine_ls_number_reflns 3999 _refine_ls_number_parameters 200 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.0905 _refine_ls_wR_factor_gt 0.0848 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 P1 P 0.35989(6) 0.36900(4) 0.82608(4) 0.01711(13) Uani 1 1 d . . . P2 P 0.10839(6) 0.34601(4) 0.83263(4) 0.01596(13) Uani 1 1 d . . . C1 C 0.4313(3) 0.27652(18) 0.90936(14) 0.0173(5) Uani 1 1 d . . . H1 H 0.4054 0.3106 0.9640 0.021 Uiso 1 1 calc R . . C2 C 0.6059(3) 0.27838(19) 0.90084(15) 0.0217(5) Uani 1 1 d . . . H2A H 0.6411 0.3541 0.9082 0.026 Uiso 1 1 calc R . . H2B H 0.6499 0.2349 0.9467 0.026 Uiso 1 1 calc R . . C3 C 0.6700(2) 0.23566(19) 0.81887(14) 0.0227(5) Uani 1 1 d . . . H3A H 0.6639 0.1555 0.8196 0.027 Uiso 1 1 calc R . . H3B H 0.7791 0.2555 0.8158 0.027 Uiso 1 1 calc R . . C4 C 0.5915(3) 0.2764(2) 0.73985(14) 0.0232(5) Uani 1 1 d . . . H4A H 0.6270 0.2318 0.6925 0.028 Uiso 1 1 calc R . . H4B H 0.6250 0.3519 0.7295 0.028 Uiso 1 1 calc R . . C5 C 0.4148(3) 0.27432(19) 0.74108(13) 0.0181(5) Uani 1 1 d . . . H5 H 0.3789 0.3070 0.6877 0.022 Uiso 1 1 calc R . . C6 C 0.3452(3) 0.16033(18) 0.74719(13) 0.0211(5) Uani 1 1 d . . . H6A H 0.3844 0.1166 0.7002 0.025 Uiso 1 1 calc R . . H6B H 0.2336 0.1670 0.7398 0.025 Uiso 1 1 calc R . . C7 C 0.3749(3) 0.09729(16) 0.82795(14) 0.0210(5) Uani 1 1 d . . . H7A H 0.3034 0.0352 0.8303 0.025 Uiso 1 1 calc R . . H7B H 0.4793 0.0672 0.8257 0.025 Uiso 1 1 calc R . . C8 C 0.3585(3) 0.16263(17) 0.90835(13) 0.0193(5) Uani 1 1 d . . . H8A H 0.4039 0.1198 0.9542 0.023 Uiso 1 1 calc R . . H8B H 0.2486 0.1706 0.9205 0.023 Uiso 1 1 calc R . . C9 C 0.0596(2) 0.46210(18) 0.89928(14) 0.0165(5) Uani 1 1 d . . . C10 C -0.0837(3) 0.51024(18) 0.89133(14) 0.0195(5) Uani 1 1 d . . . H10 H -0.1496 0.4887 0.8475 0.023 Uiso 1 1 calc R . . C11 C -0.1303(3) 0.58937(19) 0.94718(13) 0.0232(5) Uani 1 1 d . . . H11 H -0.2272 0.6226 0.9405 0.028 Uiso 1 1 calc R . . C12 C -0.0372(3) 0.62049(19) 1.01254(15) 0.0249(5) Uani 1 1 d . . . H12 H -0.0707 0.6734 1.0514 0.030 Uiso 1 1 calc R . . C13 C 0.1057(3) 0.57340(19) 1.02062(14) 0.0254(5) Uani 1 1 d . . . H13 H 0.1708 0.5945 1.0649 0.031 Uiso 1 1 calc R . . C14 C 0.1536(3) 0.49550(19) 0.96410(14) 0.0208(5) Uani 1 1 d . . . H14 H 0.2520 0.4644 0.9697 0.025 Uiso 1 1 calc R . . C15 C 0.0599(2) 0.39909(18) 0.72950(14) 0.0168(5) Uani 1 1 d . . . C16 C -0.0040(2) 0.32695(18) 0.67162(15) 0.0200(5) Uani 1 1 d . . . H16 H -0.0186 0.2530 0.6862 0.024 Uiso 1 1 calc R . . C17 C -0.0460(3) 0.3632(2) 0.59287(14) 0.0227(5) Uani 1 1 d . . . H17 H -0.0895 0.3140 0.5541 0.027 Uiso 1 1 calc R . . C18 C -0.0248(3) 0.4702(2) 0.57096(15) 0.0217(5) Uani 1 1 d . . . H18 H -0.0534 0.4946 0.5172 0.026 Uiso 1 1 calc R . . C19 C 0.0388(3) 0.54258(19) 0.62774(14) 0.0195(5) Uani 1 1 d . . . H19 H 0.0530 0.6165 0.6128 0.023 Uiso 1 1 calc R . . C20 C 0.0810(2) 0.50665(19) 0.70566(13) 0.0183(5) Uani 1 1 d . . . H20 H 0.1254 0.5563 0.7438 0.022 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 P1 0.0136(2) 0.0169(3) 0.0209(3) 0.0019(3) 0.0001(2) 0.0002(2) P2 0.0131(2) 0.0166(3) 0.0182(3) 0.0013(2) -0.0005(2) -0.0002(2) C1 0.0168(11) 0.0214(11) 0.0136(11) -0.0005(9) 0.0002(9) 0.0022(9) C2 0.0177(12) 0.0226(12) 0.0247(13) 0.0027(10) -0.0043(10) -0.0006(10) C3 0.0125(10) 0.0256(11) 0.0299(14) 0.0028(11) 0.0002(10) 0.0020(9) C4 0.0172(11) 0.0294(13) 0.0229(13) 0.0030(10) 0.0080(10) 0.0043(11) C5 0.0163(11) 0.0243(11) 0.0138(11) 0.0038(9) 0.0007(9) 0.0047(10) C6 0.0180(11) 0.0247(12) 0.0206(12) -0.0045(10) -0.0008(9) 0.0013(11) C7 0.0195(10) 0.0176(10) 0.0258(12) -0.0023(10) 0.0011(11) -0.0005(9) C8 0.0178(11) 0.0213(11) 0.0187(12) 0.0053(9) 0.0002(9) 0.0024(10) C9 0.0167(11) 0.0173(11) 0.0154(11) 0.0031(9) 0.0032(9) -0.0002(9) C10 0.0169(11) 0.0231(12) 0.0185(12) 0.0045(9) 0.0010(10) -0.0009(10) C11 0.0216(12) 0.0266(12) 0.0213(13) 0.0063(10) 0.0057(10) 0.0054(10) C12 0.0315(13) 0.0228(12) 0.0205(12) 0.0001(10) 0.0075(11) 0.0046(11) C13 0.0274(13) 0.0304(13) 0.0185(12) -0.0024(10) -0.0003(11) -0.0004(11) C14 0.0187(11) 0.0217(11) 0.0221(13) -0.0007(10) -0.0003(10) 0.0008(10) C15 0.0100(10) 0.0224(12) 0.0182(12) -0.0011(9) 0.0009(9) 0.0003(8) C16 0.0165(10) 0.0175(10) 0.0259(13) 0.0000(11) 0.0003(10) 0.0012(8) C17 0.0225(12) 0.0240(12) 0.0217(13) -0.0060(10) -0.0039(10) 0.0030(11) C18 0.0181(12) 0.0300(13) 0.0171(12) 0.0017(10) -0.0008(10) 0.0037(10) C19 0.0178(11) 0.0194(11) 0.0212(13) 0.0029(10) 0.0027(10) 0.0004(10) C20 0.0148(11) 0.0214(11) 0.0187(12) -0.0019(9) 0.0001(9) -0.0006(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C5 1.861(2) . ? P1 C1 1.867(2) . ? P1 P2 2.2286(7) . ? P2 C15 1.834(2) . ? P2 C9 1.839(2) . ? C1 C2 1.540(3) . ? C1 C8 1.542(3) . ? C1 H1 1.0000 . ? C2 C3 1.527(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.531(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.552(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.535(3) . ? C5 H5 1.0000 . ? C6 C7 1.536(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.530(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C14 1.392(3) . ? C9 C10 1.397(3) . ? C10 C11 1.388(3) . ? C10 H10 0.9500 . ? C11 C12 1.386(3) . ? C11 H11 0.9500 . ? C12 C13 1.388(3) . ? C12 H12 0.9500 . ? C13 C14 1.388(3) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C20 1.392(3) . ? C15 C16 1.404(3) . ? C16 C17 1.393(3) . ? C16 H16 0.9500 . ? C17 C18 1.377(3) . ? C17 H17 0.9500 . ? C18 C19 1.394(3) . ? C18 H18 0.9500 . ? C19 C20 1.380(3) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? 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 C5 P1 C1 93.30(10) . . ? C5 P1 P2 102.22(8) . . ? C1 P1 P2 102.77(8) . . ? C15 P2 C9 101.30(10) . . ? C15 P2 P1 98.16(7) . . ? C9 P2 P1 99.17(7) . . ? C2 C1 C8 115.14(18) . . ? C2 C1 P1 105.15(15) . . ? C8 C1 P1 114.15(15) . . ? C2 C1 H1 107.3 . . ? C8 C1 H1 107.3 . . ? P1 C1 H1 107.3 . . ? C3 C2 C1 116.00(19) . . ? C3 C2 H2A 108.3 . . ? C1 C2 H2A 108.3 . . ? C3 C2 H2B 108.3 . . ? C1 C2 H2B 108.3 . . ? H2A C2 H2B 107.4 . . ? C2 C3 C4 116.01(18) . . ? C2 C3 H3A 108.3 . . ? C4 C3 H3A 108.3 . . ? C2 C3 H3B 108.3 . . ? C4 C3 H3B 108.3 . . ? H3A C3 H3B 107.4 . . ? C3 C4 C5 115.70(19) . . ? C3 C4 H4A 108.4 . . ? C5 C4 H4A 108.4 . . ? C3 C4 H4B 108.4 . . ? C5 C4 H4B 108.4 . . ? H4A C4 H4B 107.4 . . ? C6 C5 C4 114.48(19) . . ? C6 C5 P1 115.05(15) . . ? C4 C5 P1 104.95(16) . . ? C6 C5 H5 107.3 . . ? C4 C5 H5 107.3 . . ? P1 C5 H5 107.3 . . ? C5 C6 C7 116.70(18) . . ? C5 C6 H6A 108.1 . . ? C7 C6 H6A 108.1 . . ? C5 C6 H6B 108.1 . . ? C7 C6 H6B 108.1 . . ? H6A C6 H6B 107.3 . . ? C8 C7 C6 115.65(17) . . ? C8 C7 H7A 108.4 . . ? C6 C7 H7A 108.4 . . ? C8 C7 H7B 108.4 . . ? C6 C7 H7B 108.4 . . ? H7A C7 H7B 107.4 . . ? C7 C8 C1 116.69(18) . . ? C7 C8 H8A 108.1 . . ? C1 C8 H8A 108.1 . . ? C7 C8 H8B 108.1 . . ? C1 C8 H8B 108.1 . . ? H8A C8 H8B 107.3 . . ? C14 C9 C10 118.5(2) . . ? C14 C9 P2 121.95(17) . . ? C10 C9 P2 119.13(18) . . ? C11 C10 C9 120.3(2) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C12 C11 C10 120.8(2) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C11 C12 C13 119.2(2) . . ? C11 C12 H12 120.4 . . ? C13 C12 H12 120.4 . . ? C14 C13 C12 120.1(2) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C9 121.1(2) . . ? C13 C14 H14 119.5 . . ? C9 C14 H14 119.5 . . ? C20 C15 C16 118.3(2) . . ? C20 C15 P2 123.91(17) . . ? C16 C15 P2 117.83(17) . . ? C17 C16 C15 120.4(2) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C18 C17 C16 120.3(2) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C19 120.0(2) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C20 C19 C18 119.8(2) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C19 C20 C15 121.3(2) . . ? C19 C20 H20 119.3 . . ? C15 C20 H20 119.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 P1 P2 C15 -64.86(11) . . . . ? C1 P1 P2 C15 -161.14(10) . . . . ? C5 P1 P2 C9 -167.78(10) . . . . ? C1 P1 P2 C9 95.93(11) . . . . ? C5 P1 C1 C2 70.02(15) . . . . ? P2 P1 C1 C2 173.35(13) . . . . ? C5 P1 C1 C8 -57.11(17) . . . . ? P2 P1 C1 C8 46.22(16) . . . . ? C8 C1 C2 C3 64.0(3) . . . . ? P1 C1 C2 C3 -62.5(2) . . . . ? C1 C2 C3 C4 46.0(3) . . . . ? C2 C3 C4 C5 -45.9(3) . . . . ? C3 C4 C5 C6 -64.4(3) . . . . ? C3 C4 C5 P1 62.7(2) . . . . ? C1 P1 C5 C6 56.81(17) . . . . ? P2 P1 C5 C6 -47.02(17) . . . . ? C1 P1 C5 C4 -69.93(15) . . . . ? P2 P1 C5 C4 -173.76(13) . . . . ? C4 C5 C6 C7 65.5(3) . . . . ? P1 C5 C6 C7 -56.2(2) . . . . ? C5 C6 C7 C8 43.5(3) . . . . ? C6 C7 C8 C1 -44.4(3) . . . . ? C2 C1 C8 C7 -64.2(2) . . . . ? P1 C1 C8 C7 57.5(2) . . . . ? C15 P2 C9 C14 -136.79(19) . . . . ? P1 P2 C9 C14 -36.48(19) . . . . ? C15 P2 C9 C10 51.0(2) . . . . ? P1 P2 C9 C10 151.32(17) . . . . ? C14 C9 C10 C11 -0.1(3) . . . . ? P2 C9 C10 C11 172.40(16) . . . . ? C9 C10 C11 C12 -1.3(3) . . . . ? C10 C11 C12 C13 1.5(3) . . . . ? C11 C12 C13 C14 -0.5(4) . . . . ? C12 C13 C14 C9 -0.8(4) . . . . ? C10 C9 C14 C13 1.1(3) . . . . ? P2 C9 C14 C13 -171.15(18) . . . . ? C9 P2 C15 C20 36.0(2) . . . . ? P1 P2 C15 C20 -65.14(19) . . . . ? C9 P2 C15 C16 -143.26(17) . . . . ? P1 P2 C15 C16 115.63(16) . . . . ? C20 C15 C16 C17 -0.6(3) . . . . ? P2 C15 C16 C17 178.67(16) . . . . ? C15 C16 C17 C18 0.2(3) . . . . ? C16 C17 C18 C19 -0.1(3) . . . . ? C17 C18 C19 C20 0.4(3) . . . . ? C18 C19 C20 C15 -0.8(3) . . . . ? C16 C15 C20 C19 0.9(3) . . . . ? P2 C15 C20 C19 -178.36(16) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.340 _refine_diff_density_min -0.311 _refine_diff_density_rms 0.054 data_7c _database_code_depnum_ccdc_archive 'CCDC 815355' #TrackingRef '- Diphosphanes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H44 Cl2 O7 P2 Pt, C7 H8' _chemical_formula_sum 'C35 H52 Cl2 O7 P2 Pt' _chemical_formula_weight 912.70 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.051(3) _cell_length_b 12.288(3) _cell_length_c 15.346(4) _cell_angle_alpha 66.679(6) _cell_angle_beta 85.658(9) _cell_angle_gamma 80.770(11) _cell_volume 1888.7(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 16339 _cell_measurement_theta_min 2.346 _cell_measurement_theta_max 27.504 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.605 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 3.986 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.18 _exptl_absorpt_correction_T_max 0.45 _exptl_absorpt_process_details 'SADABS V2.10' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 8.2 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 20066 _diffrn_reflns_av_R_equivalents 0.0508 _diffrn_reflns_av_sigmaI/netI 0.0452 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 27.51 _reflns_number_total 8550 _reflns_number_gt 8157 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART V5.054 (Bruker, 1998)' _computing_cell_refinement 'Bruker SMART V5.054 (Bruker, 1998)' _computing_data_reduction 'Bruker SAINT V6.02 (Bruker, 1999)' _computing_structure_solution 'SHELXS V6.12 (Bruker 2001)' _computing_structure_refinement 'SHELXL V6.12 (Bruker 2001)' _computing_molecular_graphics 'Bruker SHELXTL V6.14 (Bruker AXS, 2003)' _computing_publication_material 'Bruker SHELXTL V6.14 (Bruker AXS, 2003)' _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^)+(0.0359P)^2^+0.6354P] 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 8550 _refine_ls_number_parameters 431 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0239 _refine_ls_R_factor_gt 0.0222 _refine_ls_wR_factor_ref 0.0697 _refine_ls_wR_factor_gt 0.0629 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.110 _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 0.577838(7) 0.554407(8) 0.680355(6) 0.01627(4) Uani 1 1 d . . . Cl1 Cl 0.41612(6) 0.47569(7) 0.64611(6) 0.02796(16) Uani 1 1 d . . . Cl2 Cl 0.43791(6) 0.72634(7) 0.66680(6) 0.02887(16) Uani 1 1 d . . . P1 P 0.71500(6) 0.39145(6) 0.70742(5) 0.01557(13) Uani 1 1 d . . . P2 P 0.72135(6) 0.63979(7) 0.71244(5) 0.01654(14) Uani 1 1 d . . . O1 O 0.57380(16) 0.22102(18) 0.74350(13) 0.0205(4) Uani 1 1 d . . . O2 O 0.86097(16) 0.22938(17) 0.65793(13) 0.0188(4) Uani 1 1 d . . . O3 O 0.71631(17) 0.09501(18) 0.68964(14) 0.0220(4) Uani 1 1 d . . . O4 O 0.99411(17) 0.2464(2) 0.84195(15) 0.0276(5) Uani 1 1 d . . . O5 O 1.05956(16) 0.36872(18) 0.69914(14) 0.0234(4) Uani 1 1 d . . . O6 O 1.0261(2) 0.5096(2) 0.84270(17) 0.0393(6) Uani 1 1 d . . . O7 O 1.02607(17) 0.6401(2) 0.69060(16) 0.0295(5) Uani 1 1 d . . . C1 C 0.5999(3) 0.2609(3) 0.8796(2) 0.0272(6) Uani 1 1 d . . . H1A H 0.5309 0.3229 0.8598 0.041 Uiso 1 1 calc R . . H1B H 0.6561 0.2821 0.9130 0.041 Uiso 1 1 calc R . . H1C H 0.5723 0.1870 0.9207 0.041 Uiso 1 1 calc R . . C2 C 0.6640(2) 0.2460(2) 0.79322(18) 0.0190(5) Uani 1 1 d . . . C3 C 0.7695(2) 0.1433(3) 0.81696(19) 0.0212(5) Uani 1 1 d . . . H3A H 0.7421 0.0707 0.8630 0.025 Uiso 1 1 calc R . . H3B H 0.8357 0.1614 0.8446 0.025 Uiso 1 1 calc R . . C4 C 0.8154(2) 0.1241(3) 0.72690(19) 0.0200(5) Uani 1 1 d . . . C5 C 0.9215(3) 0.0234(3) 0.7443(2) 0.0268(6) Uani 1 1 d . . . H5A H 0.9004 -0.0475 0.7952 0.040 Uiso 1 1 calc R . . H5B H 0.9927 0.0461 0.7611 0.040 Uiso 1 1 calc R . . H5C H 0.9386 0.0077 0.6878 0.040 Uiso 1 1 calc R . . C6 C 0.5099(3) 0.1499(3) 0.6356(2) 0.0283(6) Uani 1 1 d . . . H6A H 0.5312 0.1337 0.5796 0.042 Uiso 1 1 calc R . . H6B H 0.4399 0.2110 0.6231 0.042 Uiso 1 1 calc R . . H6C H 0.4908 0.0782 0.6865 0.042 Uiso 1 1 calc R . . C7 C 0.6166(2) 0.1918(3) 0.66307(19) 0.0208(5) Uani 1 1 d . . . C8 C 0.6608(2) 0.2983(3) 0.58256(19) 0.0195(5) Uani 1 1 d . . . H8A H 0.5952 0.3654 0.5641 0.023 Uiso 1 1 calc R . . H8B H 0.6834 0.2778 0.5280 0.023 Uiso 1 1 calc R . . C9 C 0.7709(2) 0.3336(2) 0.61356(18) 0.0175(5) Uani 1 1 d . . . C10 C 0.8352(2) 0.4220(3) 0.53170(19) 0.0229(6) Uani 1 1 d . . . H10A H 0.9024 0.4427 0.5553 0.034 Uiso 1 1 calc R . . H10B H 0.7783 0.4929 0.5006 0.034 Uiso 1 1 calc R . . H10C H 0.8655 0.3865 0.4873 0.034 Uiso 1 1 calc R . . C11 C 0.8586(2) 0.4210(3) 0.74398(18) 0.0179(5) Uani 1 1 d . . . C12 C 0.8612(2) 0.5287(3) 0.74229(19) 0.0196(5) Uani 1 1 d . . . C13 C 0.9763(2) 0.3313(3) 0.7688(2) 0.0205(5) Uani 1 1 d . . . C14 C 1.1801(3) 0.2967(3) 0.7196(3) 0.0344(8) Uani 1 1 d . . . H14A H 1.2153 0.3052 0.7714 0.052 Uiso 1 1 calc R . . H14B H 1.2322 0.3232 0.6645 0.052 Uiso 1 1 calc R . . H14C H 1.1721 0.2141 0.7363 0.052 Uiso 1 1 calc R . . C15 C 0.9805(2) 0.5579(3) 0.7662(2) 0.0229(6) Uani 1 1 d . . . C16 C 1.1456(3) 0.6686(3) 0.7022(3) 0.0387(8) Uani 1 1 d . . . H16A H 1.1404 0.6985 0.7517 0.058 Uiso 1 1 calc R . . H16B H 1.1701 0.7284 0.6438 0.058 Uiso 1 1 calc R . . H16C H 1.2050 0.5977 0.7188 0.058 Uiso 1 1 calc R . . C17 C 0.7732(2) 0.7704(2) 0.61571(19) 0.0189(5) Uani 1 1 d . . . H17 H 0.8444 0.7883 0.6393 0.023 Uiso 1 1 calc R . . C18 C 0.8186(3) 0.7385(3) 0.5304(2) 0.0255(6) Uani 1 1 d . . . H18A H 0.8782 0.6664 0.5513 0.031 Uiso 1 1 calc R . . H18B H 0.7503 0.7231 0.5030 0.031 Uiso 1 1 calc R . . C19 C 0.8775(3) 0.8415(3) 0.4554(2) 0.0316(7) Uani 1 1 d . . . H19A H 0.9032 0.8214 0.4011 0.038 Uiso 1 1 calc R . . H19B H 0.9497 0.8525 0.4815 0.038 Uiso 1 1 calc R . . C20 C 0.7874(3) 0.9583(3) 0.4233(2) 0.0348(7) Uani 1 1 d . . . H20A H 0.8283 1.0230 0.3787 0.042 Uiso 1 1 calc R . . H20B H 0.7192 0.9501 0.3911 0.042 Uiso 1 1 calc R . . C21 C 0.7391(3) 0.9886(3) 0.5084(2) 0.0334(7) Uani 1 1 d . . . H21A H 0.6792 1.0604 0.4869 0.040 Uiso 1 1 calc R . . H21B H 0.8063 1.0048 0.5365 0.040 Uiso 1 1 calc R . . C22 C 0.6796(3) 0.8859(3) 0.5838(2) 0.0269(6) Uani 1 1 d . . . H22A H 0.6083 0.8735 0.5576 0.032 Uiso 1 1 calc R . . H22B H 0.6531 0.9062 0.6379 0.032 Uiso 1 1 calc R . . C23 C 0.6833(2) 0.6755(3) 0.81793(19) 0.0201(5) Uani 1 1 d . . . H23 H 0.6026 0.7249 0.8066 0.024 Uiso 1 1 calc R . . C24 C 0.7706(3) 0.7487(3) 0.8369(2) 0.0319(7) Uani 1 1 d . . . H24A H 0.8528 0.7044 0.8464 0.038 Uiso 1 1 calc R . . H24B H 0.7727 0.8234 0.7822 0.038 Uiso 1 1 calc R . . C25 C 0.7288(3) 0.7752(3) 0.9247(2) 0.0343(7) Uani 1 1 d . . . H25A H 0.7883 0.8167 0.9378 0.041 Uiso 1 1 calc R . . H25B H 0.6509 0.8275 0.9120 0.041 Uiso 1 1 calc R . . C26 C 0.7150(3) 0.6612(4) 1.0113(2) 0.0376(8) Uani 1 1 d . . . H26A H 0.7945 0.6123 1.0278 0.045 Uiso 1 1 calc R . . H26B H 0.6846 0.6816 1.0646 0.045 Uiso 1 1 calc R . . C27 C 0.6275(3) 0.5905(3) 0.9923(2) 0.0364(8) Uani 1 1 d . . . H27A H 0.5461 0.6365 0.9818 0.044 Uiso 1 1 calc R . . H27B H 0.6234 0.5167 1.0475 0.044 Uiso 1 1 calc R . . C28 C 0.6682(3) 0.5606(3) 0.9050(2) 0.0309(7) Uani 1 1 d . . . H28A H 0.7454 0.5072 0.9179 0.037 Uiso 1 1 calc R . . H28B H 0.6075 0.5201 0.8922 0.037 Uiso 1 1 calc R . . C29 C 0.1770(3) 0.8146(4) 0.9176(2) 0.0431(9) Uani 1 1 d . . . C30 C 0.2868(3) 0.8060(4) 0.8669(3) 0.0472(10) Uani 1 1 d . . . H30 H 0.3092 0.7417 0.8488 0.057 Uiso 1 1 calc R . . C31 C 0.3609(4) 0.8933(4) 0.8443(3) 0.0501(10) Uani 1 1 d . . . H31 H 0.4335 0.8873 0.8105 0.060 Uiso 1 1 calc R . . C32 C 0.3299(4) 0.9906(4) 0.8708(3) 0.0562(11) Uani 1 1 d . . . H32 H 0.3816 1.0484 0.8553 0.067 Uiso 1 1 calc R . . C33 C 0.2230(4) 1.0001(4) 0.9194(3) 0.0563(12) Uani 1 1 d . . . H33 H 0.2012 1.0652 0.9368 0.068 Uiso 1 1 calc R . . C34 C 0.1468(3) 0.9132(4) 0.9432(2) 0.0452(10) Uani 1 1 d . . . H34 H 0.0744 0.9204 0.9767 0.054 Uiso 1 1 calc R . . C35 C 0.0954(4) 0.7200(5) 0.9437(3) 0.0606(12) Uani 1 1 d . . . H35A H 0.0735 0.6950 1.0098 0.091 Uiso 1 1 calc R . . H35B H 0.1378 0.6526 0.9317 0.091 Uiso 1 1 calc R . . H35C H 0.0225 0.7516 0.9063 0.091 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 0.01257(6) 0.01780(8) 0.01899(6) -0.00761(5) -0.00096(4) -0.00224(4) Cl1 0.0182(3) 0.0282(4) 0.0403(4) -0.0147(3) -0.0067(3) -0.0047(3) Cl2 0.0171(3) 0.0259(4) 0.0451(4) -0.0167(3) -0.0035(3) 0.0021(3) P1 0.0151(3) 0.0166(4) 0.0157(3) -0.0068(3) -0.0003(2) -0.0030(2) P2 0.0149(3) 0.0166(4) 0.0195(3) -0.0083(3) -0.0007(2) -0.0027(2) O1 0.0199(8) 0.0230(11) 0.0218(9) -0.0105(8) 0.0018(7) -0.0080(7) O2 0.0184(8) 0.0154(10) 0.0219(9) -0.0064(8) 0.0008(7) -0.0030(7) O3 0.0219(9) 0.0189(11) 0.0293(10) -0.0132(8) -0.0012(8) -0.0041(8) O4 0.0228(9) 0.0255(12) 0.0276(10) -0.0034(9) -0.0051(8) -0.0004(8) O5 0.0153(8) 0.0235(11) 0.0284(10) -0.0080(9) 0.0021(7) -0.0015(8) O6 0.0331(11) 0.0470(16) 0.0367(13) -0.0096(12) -0.0149(10) -0.0136(11) O7 0.0186(9) 0.0335(13) 0.0371(12) -0.0118(10) -0.0004(8) -0.0111(8) C1 0.0313(14) 0.0302(17) 0.0203(13) -0.0103(12) 0.0065(11) -0.0070(12) C2 0.0213(11) 0.0185(14) 0.0173(12) -0.0057(10) 0.0001(9) -0.0068(10) C3 0.0235(12) 0.0188(14) 0.0198(12) -0.0052(11) -0.0009(10) -0.0050(10) C4 0.0217(12) 0.0182(14) 0.0212(12) -0.0076(11) 0.0001(10) -0.0067(10) C5 0.0252(13) 0.0192(15) 0.0330(15) -0.0079(12) -0.0009(11) -0.0010(11) C6 0.0250(13) 0.0321(18) 0.0330(15) -0.0161(14) -0.0007(11) -0.0094(12) C7 0.0205(12) 0.0223(15) 0.0227(13) -0.0121(11) 0.0006(10) -0.0036(10) C8 0.0205(11) 0.0218(15) 0.0191(12) -0.0100(11) -0.0011(10) -0.0054(10) C9 0.0173(11) 0.0184(14) 0.0173(11) -0.0078(10) -0.0006(9) -0.0018(10) C10 0.0243(12) 0.0238(15) 0.0191(12) -0.0062(11) 0.0028(10) -0.0057(11) C11 0.0135(10) 0.0218(14) 0.0142(11) -0.0034(10) 0.0003(9) -0.0010(10) C12 0.0142(11) 0.0266(15) 0.0195(12) -0.0102(11) 0.0009(9) -0.0046(10) C13 0.0178(11) 0.0204(15) 0.0250(13) -0.0103(11) -0.0012(10) -0.0033(10) C14 0.0170(12) 0.037(2) 0.0450(19) -0.0134(16) 0.0012(12) 0.0014(12) C15 0.0169(11) 0.0218(15) 0.0350(15) -0.0166(12) -0.0024(11) -0.0015(10) C16 0.0217(13) 0.045(2) 0.057(2) -0.0242(18) 0.0039(14) -0.0173(14) C17 0.0174(11) 0.0169(14) 0.0235(13) -0.0087(11) 0.0011(10) -0.0034(10) C18 0.0292(14) 0.0226(16) 0.0262(14) -0.0109(12) 0.0044(11) -0.0067(11) C19 0.0362(15) 0.0293(18) 0.0277(15) -0.0101(13) 0.0108(12) -0.0082(13) C20 0.0404(17) 0.0320(19) 0.0253(15) -0.0039(13) 0.0043(13) -0.0073(14) C21 0.0389(16) 0.0207(16) 0.0337(16) -0.0052(13) 0.0044(13) -0.0014(13) C22 0.0272(13) 0.0206(15) 0.0276(14) -0.0063(12) 0.0030(11) 0.0018(11) C23 0.0203(11) 0.0221(15) 0.0216(12) -0.0124(11) 0.0002(10) -0.0035(10) C24 0.0372(16) 0.0376(19) 0.0317(15) -0.0215(14) 0.0051(13) -0.0174(14) C25 0.0377(16) 0.042(2) 0.0374(17) -0.0280(16) 0.0031(13) -0.0143(14) C26 0.0398(17) 0.053(2) 0.0249(15) -0.0208(16) 0.0000(13) -0.0068(16) C27 0.0428(18) 0.044(2) 0.0261(15) -0.0165(15) 0.0115(13) -0.0136(16) C28 0.0400(16) 0.0302(18) 0.0258(14) -0.0131(13) 0.0081(13) -0.0121(14) C29 0.0423(18) 0.054(3) 0.0254(16) -0.0095(16) -0.0101(14) 0.0046(17) C30 0.047(2) 0.055(3) 0.0315(17) -0.0149(18) -0.0029(15) 0.0116(19) C31 0.048(2) 0.048(3) 0.042(2) -0.0119(19) 0.0007(17) 0.0102(19) C32 0.058(2) 0.048(3) 0.048(2) -0.006(2) -0.0082(19) 0.004(2) C33 0.077(3) 0.048(3) 0.0343(19) -0.0134(19) -0.0123(19) 0.014(2) C34 0.0444(19) 0.056(3) 0.0240(15) -0.0120(16) -0.0055(14) 0.0168(18) C35 0.058(2) 0.074(3) 0.052(2) -0.025(2) -0.011(2) -0.010(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P2 2.2180(8) . ? Pt1 P1 2.2233(9) . ? Pt1 Cl1 2.3463(8) . ? Pt1 Cl2 2.3559(9) . ? P1 C11 1.856(3) . ? P1 C9 1.870(3) . ? P1 C2 1.895(3) . ? P2 C17 1.841(3) . ? P2 C23 1.841(3) . ? P2 C12 1.843(3) . ? O1 C2 1.439(3) . ? O1 C7 1.444(3) . ? O2 C4 1.446(3) . ? O2 C9 1.448(3) . ? O3 C4 1.426(3) . ? O3 C7 1.435(3) . ? O4 C13 1.195(3) . ? O5 C13 1.342(3) . ? O5 C14 1.456(3) . ? O6 C15 1.195(4) . ? O7 C15 1.329(4) . ? O7 C16 1.461(3) . ? C1 C2 1.517(4) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.521(4) . ? C3 C4 1.529(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.516(4) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.508(4) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.520(4) . ? C8 C9 1.522(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.515(4) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.319(4) . ? C11 C13 1.528(4) . ? C12 C15 1.525(4) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.538(4) . ? C17 C22 1.543(4) . ? C17 H17 0.9800 . ? C18 C19 1.532(4) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.533(5) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.532(5) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.535(4) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.533(4) . ? C23 C28 1.535(4) . ? C23 H23 0.9800 . ? C24 C25 1.529(4) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.522(5) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.512(5) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.541(4) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C34 1.400(6) . ? C29 C30 1.403(5) . ? C29 C35 1.496(6) . ? C30 C31 1.373(6) . ? C30 H30 0.9300 . ? C31 C32 1.395(6) . ? C31 H31 0.9300 . ? C32 C33 1.363(6) . ? C32 H32 0.9300 . ? C33 C34 1.384(6) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? 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 P2 Pt1 P1 88.35(3) . . ? P2 Pt1 Cl1 176.00(2) . . ? P1 Pt1 Cl1 95.62(3) . . ? P2 Pt1 Cl2 88.01(3) . . ? P1 Pt1 Cl2 174.15(2) . . ? Cl1 Pt1 Cl2 87.99(3) . . ? C11 P1 C9 102.33(11) . . ? C11 P1 C2 112.84(12) . . ? C9 P1 C2 95.13(12) . . ? C11 P1 Pt1 107.18(10) . . ? C9 P1 Pt1 123.09(9) . . ? C2 P1 Pt1 115.48(9) . . ? C17 P2 C23 109.28(13) . . ? C17 P2 C12 103.16(12) . . ? C23 P2 C12 105.85(12) . . ? C17 P2 Pt1 117.84(9) . . ? C23 P2 Pt1 112.59(9) . . ? C12 P2 Pt1 107.00(10) . . ? C2 O1 C7 116.89(19) . . ? C4 O2 C9 116.72(19) . . ? C4 O3 C7 111.2(2) . . ? C13 O5 C14 114.1(2) . . ? C15 O7 C16 116.2(2) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C1 106.8(2) . . ? O1 C2 C3 107.7(2) . . ? C1 C2 C3 113.9(2) . . ? O1 C2 P1 105.59(17) . . ? C1 C2 P1 111.1(2) . . ? C3 C2 P1 111.23(18) . . ? C2 C3 C4 109.8(2) . . ? C2 C3 H3A 109.7 . . ? C4 C3 H3A 109.7 . . ? C2 C3 H3B 109.7 . . ? C4 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? O3 C4 O2 111.1(2) . . ? O3 C4 C5 108.2(2) . . ? O2 C4 C5 105.3(2) . . ? O3 C4 C3 108.0(2) . . ? O2 C4 C3 111.1(2) . . ? C5 C4 C3 113.2(2) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O3 C7 O1 110.5(2) . . ? O3 C7 C6 108.4(2) . . ? O1 C7 C6 105.6(2) . . ? O3 C7 C8 108.1(2) . . ? O1 C7 C8 111.5(2) . . ? C6 C7 C8 112.8(2) . . ? C7 C8 C9 110.3(2) . . ? C7 C8 H8A 109.6 . . ? C9 C8 H8A 109.6 . . ? C7 C8 H8B 109.6 . . ? C9 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? O2 C9 C10 107.0(2) . . ? O2 C9 C8 110.5(2) . . ? C10 C9 C8 112.9(2) . . ? O2 C9 P1 106.44(16) . . ? C10 C9 P1 112.9(2) . . ? C8 C9 P1 106.94(17) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C13 118.2(2) . . ? C12 C11 P1 117.7(2) . . ? C13 C11 P1 123.9(2) . . ? C11 C12 C15 118.9(2) . . ? C11 C12 P2 119.6(2) . . ? C15 C12 P2 121.6(2) . . ? O4 C13 O5 125.4(2) . . ? O4 C13 C11 125.2(2) . . ? O5 C13 C11 109.2(2) . . ? O5 C14 H14A 109.5 . . ? O5 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O5 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O6 C15 O7 125.9(3) . . ? O6 C15 C12 123.1(3) . . ? O7 C15 C12 110.9(2) . . ? O7 C16 H16A 109.5 . . ? O7 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O7 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C22 110.5(2) . . ? C18 C17 P2 110.26(19) . . ? C22 C17 P2 115.59(18) . . ? C18 C17 H17 106.7 . . ? C22 C17 H17 106.7 . . ? P2 C17 H17 106.7 . . ? C19 C18 C17 110.2(2) . . ? C19 C18 H18A 109.6 . . ? C17 C18 H18A 109.6 . . ? C19 C18 H18B 109.6 . . ? C17 C18 H18B 109.6 . . ? H18A C18 H18B 108.1 . . ? C18 C19 C20 111.1(2) . . ? C18 C19 H19A 109.4 . . ? C20 C19 H19A 109.4 . . ? C18 C19 H19B 109.4 . . ? C20 C19 H19B 109.4 . . ? H19A C19 H19B 108.0 . . ? C21 C20 C19 110.7(3) . . ? C21 C20 H20A 109.5 . . ? C19 C20 H20A 109.5 . . ? C21 C20 H20B 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 108.1 . . ? C20 C21 C22 111.6(3) . . ? C20 C21 H21A 109.3 . . ? C22 C21 H21A 109.3 . . ? C20 C21 H21B 109.3 . . ? C22 C21 H21B 109.3 . . ? H21A C21 H21B 108.0 . . ? C21 C22 C17 109.5(2) . . ? C21 C22 H22A 109.8 . . ? C17 C22 H22A 109.8 . . ? C21 C22 H22B 109.8 . . ? C17 C22 H22B 109.8 . . ? H22A C22 H22B 108.2 . . ? C24 C23 C28 111.9(2) . . ? C24 C23 P2 115.22(19) . . ? C28 C23 P2 109.9(2) . . ? C24 C23 H23 106.4 . . ? C28 C23 H23 106.4 . . ? P2 C23 H23 106.4 . . ? C25 C24 C23 110.7(2) . . ? C25 C24 H24A 109.5 . . ? C23 C24 H24A 109.5 . . ? C25 C24 H24B 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 108.1 . . ? C26 C25 C24 111.7(3) . . ? C26 C25 H25A 109.3 . . ? C24 C25 H25A 109.3 . . ? C26 C25 H25B 109.3 . . ? C24 C25 H25B 109.3 . . ? H25A C25 H25B 107.9 . . ? C27 C26 C25 111.1(3) . . ? C27 C26 H26A 109.4 . . ? C25 C26 H26A 109.4 . . ? C27 C26 H26B 109.4 . . ? C25 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C26 C27 C28 111.6(3) . . ? C26 C27 H27A 109.3 . . ? C28 C27 H27A 109.3 . . ? C26 C27 H27B 109.3 . . ? C28 C27 H27B 109.3 . . ? H27A C27 H27B 108.0 . . ? C23 C28 C27 110.3(3) . . ? C23 C28 H28A 109.6 . . ? C27 C28 H28A 109.6 . . ? C23 C28 H28B 109.6 . . ? C27 C28 H28B 109.6 . . ? H28A C28 H28B 108.1 . . ? C34 C29 C30 118.2(4) . . ? C34 C29 C35 121.3(4) . . ? C30 C29 C35 120.4(4) . . ? C31 C30 C29 119.6(4) . . ? C31 C30 H30 120.2 . . ? C29 C30 H30 120.2 . . ? C30 C31 C32 121.5(4) . . ? C30 C31 H31 119.3 . . ? C32 C31 H31 119.3 . . ? C33 C32 C31 119.4(5) . . ? C33 C32 H32 120.3 . . ? C31 C32 H32 120.3 . . ? C32 C33 C34 120.2(4) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C33 C34 C29 121.1(4) . . ? C33 C34 H34 119.4 . . ? C29 C34 H34 119.4 . . ? C29 C35 H35A 109.5 . . ? C29 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C29 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 Pt1 P1 C11 2.29(8) . . . . ? Cl1 Pt1 P1 C11 -177.16(9) . . . . ? P2 Pt1 P1 C9 -115.63(10) . . . . ? Cl1 Pt1 P1 C9 64.91(11) . . . . ? P2 Pt1 P1 C2 128.98(10) . . . . ? Cl1 Pt1 P1 C2 -50.48(10) . . . . ? P1 Pt1 P2 C17 114.88(10) . . . . ? Cl2 Pt1 P2 C17 -69.69(10) . . . . ? P1 Pt1 P2 C23 -116.51(10) . . . . ? Cl2 Pt1 P2 C23 58.92(10) . . . . ? P1 Pt1 P2 C12 -0.63(9) . . . . ? Cl2 Pt1 P2 C12 174.80(9) . . . . ? C7 O1 C2 C1 -174.1(2) . . . . ? C7 O1 C2 C3 -51.4(3) . . . . ? C7 O1 C2 P1 67.5(2) . . . . ? C11 P1 C2 O1 -165.15(16) . . . . ? C9 P1 C2 O1 -59.45(18) . . . . ? Pt1 P1 C2 O1 71.09(18) . . . . ? C11 P1 C2 C1 79.4(2) . . . . ? C9 P1 C2 C1 -174.92(19) . . . . ? Pt1 P1 C2 C1 -44.4(2) . . . . ? C11 P1 C2 C3 -48.6(2) . . . . ? C9 P1 C2 C3 57.1(2) . . . . ? Pt1 P1 C2 C3 -172.36(15) . . . . ? O1 C2 C3 C4 53.4(3) . . . . ? C1 C2 C3 C4 171.7(2) . . . . ? P1 C2 C3 C4 -61.8(3) . . . . ? C7 O3 C4 O2 -59.5(3) . . . . ? C7 O3 C4 C5 -174.6(2) . . . . ? C7 O3 C4 C3 62.6(3) . . . . ? C9 O2 C4 O3 50.6(3) . . . . ? C9 O2 C4 C5 167.5(2) . . . . ? C9 O2 C4 C3 -69.6(3) . . . . ? C2 C3 C4 O3 -60.7(3) . . . . ? C2 C3 C4 O2 61.4(3) . . . . ? C2 C3 C4 C5 179.6(2) . . . . ? C4 O3 C7 O1 -58.1(3) . . . . ? C4 O3 C7 C6 -173.3(2) . . . . ? C4 O3 C7 C8 64.2(3) . . . . ? C2 O1 C7 O3 53.7(3) . . . . ? C2 O1 C7 C6 170.6(2) . . . . ? C2 O1 C7 C8 -66.6(3) . . . . ? O3 C7 C8 C9 -58.3(3) . . . . ? O1 C7 C8 C9 63.3(3) . . . . ? C6 C7 C8 C9 -178.1(2) . . . . ? C4 O2 C9 C10 -168.9(2) . . . . ? C4 O2 C9 C8 -45.6(3) . . . . ? C4 O2 C9 P1 70.1(2) . . . . ? C7 C8 C9 O2 48.6(3) . . . . ? C7 C8 C9 C10 168.4(2) . . . . ? C7 C8 C9 P1 -66.8(2) . . . . ? C11 P1 C9 O2 58.20(19) . . . . ? C2 P1 C9 O2 -56.54(18) . . . . ? Pt1 P1 C9 O2 178.43(11) . . . . ? C11 P1 C9 C10 -58.9(2) . . . . ? C2 P1 C9 C10 -173.63(19) . . . . ? Pt1 P1 C9 C10 61.3(2) . . . . ? C11 P1 C9 C8 176.31(18) . . . . ? C2 P1 C9 C8 61.57(19) . . . . ? Pt1 P1 C9 C8 -63.5(2) . . . . ? C9 P1 C11 C12 126.4(2) . . . . ? C2 P1 C11 C12 -132.6(2) . . . . ? Pt1 P1 C11 C12 -4.4(2) . . . . ? C9 P1 C11 C13 -49.0(2) . . . . ? C2 P1 C11 C13 52.0(2) . . . . ? Pt1 P1 C11 C13 -179.75(18) . . . . ? C13 C11 C12 C15 -0.7(4) . . . . ? P1 C11 C12 C15 -176.32(19) . . . . ? C13 C11 C12 P2 179.90(18) . . . . ? P1 C11 C12 P2 4.2(3) . . . . ? C17 P2 C12 C11 -127.0(2) . . . . ? C23 P2 C12 C11 118.2(2) . . . . ? Pt1 P2 C12 C11 -2.1(2) . . . . ? C17 P2 C12 C15 53.6(2) . . . . ? C23 P2 C12 C15 -61.2(2) . . . . ? Pt1 P2 C12 C15 178.52(19) . . . . ? C14 O5 C13 O4 -0.8(4) . . . . ? C14 O5 C13 C11 173.9(2) . . . . ? C12 C11 C13 O4 107.3(3) . . . . ? P1 C11 C13 O4 -77.3(4) . . . . ? C12 C11 C13 O5 -67.4(3) . . . . ? P1 C11 C13 O5 107.9(2) . . . . ? C16 O7 C15 O6 3.2(4) . . . . ? C16 O7 C15 C12 -175.1(2) . . . . ? C11 C12 C15 O6 -64.9(4) . . . . ? P2 C12 C15 O6 114.5(3) . . . . ? C11 C12 C15 O7 113.4(3) . . . . ? P2 C12 C15 O7 -67.1(3) . . . . ? C23 P2 C17 C18 173.94(18) . . . . ? C12 P2 C17 C18 61.7(2) . . . . ? Pt1 P2 C17 C18 -55.9(2) . . . . ? C23 P2 C17 C22 -59.9(2) . . . . ? C12 P2 C17 C22 -172.1(2) . . . . ? Pt1 P2 C17 C22 70.3(2) . . . . ? C22 C17 C18 C19 58.5(3) . . . . ? P2 C17 C18 C19 -172.5(2) . . . . ? C17 C18 C19 C20 -57.2(3) . . . . ? C18 C19 C20 C21 55.8(4) . . . . ? C19 C20 C21 C22 -56.1(4) . . . . ? C20 C21 C22 C17 57.0(4) . . . . ? C18 C17 C22 C21 -58.1(3) . . . . ? P2 C17 C22 C21 175.8(2) . . . . ? C17 P2 C23 C24 -39.7(2) . . . . ? C12 P2 C23 C24 70.8(2) . . . . ? Pt1 P2 C23 C24 -172.68(19) . . . . ? C17 P2 C23 C28 -167.24(19) . . . . ? C12 P2 C23 C28 -56.8(2) . . . . ? Pt1 P2 C23 C28 59.8(2) . . . . ? C28 C23 C24 C25 -54.7(3) . . . . ? P2 C23 C24 C25 178.8(2) . . . . ? C23 C24 C25 C26 55.1(4) . . . . ? C24 C25 C26 C27 -56.3(4) . . . . ? C25 C26 C27 C28 56.4(4) . . . . ? C24 C23 C28 C27 54.6(3) . . . . ? P2 C23 C28 C27 -176.1(2) . . . . ? C26 C27 C28 C23 -55.4(4) . . . . ? C34 C29 C30 C31 0.2(5) . . . . ? C35 C29 C30 C31 -179.5(4) . . . . ? C29 C30 C31 C32 0.2(6) . . . . ? C30 C31 C32 C33 -0.6(6) . . . . ? C31 C32 C33 C34 0.7(6) . . . . ? C32 C33 C34 C29 -0.4(6) . . . . ? C30 C29 C34 C33 -0.1(5) . . . . ? C35 C29 C34 C33 179.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.102 _refine_diff_density_min -1.533 _refine_diff_density_rms 0.121