# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Weigand, Jan' _publ_contact_author_email jweigand@uni-muenster.de _publ_section_title ; Zwitterionic and cationic P5-Clusters from four membered phosphorus nitrogen metal heterocycles ; loop_ _publ_author_name J.Weigand M.Holthausen C.Richter A.Hepp # Attachment 'jjw0065.cif' #============================================================================== data_jjw0065 _database_code_depnum_ccdc_archive 'CCDC 783481' #TrackingRef 'jjw0065.cif' _audit_update_record ; 2010-07-06 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C6 H18 Al Cl2 N2 P5 Si2), C6 H4 F ' _chemical_formula_sum 'C18 H40 Al2 Cl4 F N4 P10 Si4' _chemical_formula_weight 949.36 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.3117(6) _cell_length_b 20.619(2) _cell_length_c 16.9567(17) _cell_angle_alpha 90.00 _cell_angle_beta 95.643(2) _cell_angle_gamma 90.00 _cell_volume 2196.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 1 _cell_measurement_theta_max 22.5 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.436 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 970 _exptl_absorpt_coefficient_mu 0.808 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9164 _exptl_absorpt_correction_T_max 0.9840 _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. SADABS reports ratio of Tmin/Tmax = 0.830979 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23512 _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_sigmaI/netI 0.0231 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 28.70 _reflns_number_total 5677 _reflns_number_gt 4781 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2(Bruker AXS, 2007)' _computing_cell_refinement 'APEX2(Bruker AXS, 2007)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2007 )' _computing_structure_solution ; SHELXS-97 , G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122 ; _computing_structure_refinement ; SHELXL-97, G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122 ; _computing_molecular_graphics ; ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Hydrogen atoms of disordered solvent molecule refined with geometrical restraints (DFIX), a common isotropic thermal displacement parameter is used . ; _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^+0.5342P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5677 _refine_ls_number_parameters 210 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0387 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0811 _refine_ls_wR_factor_gt 0.0767 _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 C1 C 0.1647(3) 0.05184(10) 0.09847(13) 0.0412(5) Uani 1 1 d . . . H1A H 0.1065 0.0455 0.1494 0.062 Uiso 1 1 calc R . . H1B H 0.1731 0.0099 0.0717 0.062 Uiso 1 1 calc R . . H1C H 0.0719 0.0811 0.0653 0.062 Uiso 1 1 calc R . . C2 C 0.6110(3) 0.03265(8) 0.18003(11) 0.0336(4) Uani 1 1 d . . . H2A H 0.7442 0.0551 0.1976 0.050 Uiso 1 1 calc R . . H2B H 0.6423 -0.0062 0.1500 0.050 Uiso 1 1 calc R . . H2C H 0.5388 0.0201 0.2263 0.050 Uiso 1 1 calc R . . C3 C 0.5485(3) 0.10178(9) 0.02008(10) 0.0350(4) Uani 1 1 d . . . H3A H 0.4565 0.1317 -0.0125 0.052 Uiso 1 1 calc R . . H3B H 0.5575 0.0605 -0.0079 0.052 Uiso 1 1 calc R . . H3C H 0.6911 0.1206 0.0303 0.052 Uiso 1 1 calc R . . C4 C 0.1017(3) 0.35114(11) 0.29474(15) 0.0480(5) Uani 1 1 d . . . H4A H 0.0186 0.3503 0.2428 0.072 Uiso 1 1 calc R . . H4B H 0.0834 0.3932 0.3201 0.072 Uiso 1 1 calc R . . H4C H 0.0522 0.3166 0.3281 0.072 Uiso 1 1 calc R . . C5 C 0.4882(4) 0.40428(9) 0.22059(12) 0.0410(5) Uani 1 1 d . . . H5A H 0.6366 0.3954 0.2119 0.061 Uiso 1 1 calc R . . H5B H 0.4796 0.4459 0.2481 0.061 Uiso 1 1 calc R . . H5C H 0.4014 0.4062 0.1694 0.061 Uiso 1 1 calc R . . C6 C 0.5416(3) 0.33632(10) 0.38108(11) 0.0388(4) Uani 1 1 d . . . H6A H 0.4770 0.3049 0.4148 0.058 Uiso 1 1 calc R . . H6B H 0.5403 0.3794 0.4054 0.058 Uiso 1 1 calc R . . H6C H 0.6888 0.3235 0.3753 0.058 Uiso 1 1 calc R . . N2 N 0.4203(2) 0.26723(6) 0.22891(8) 0.0212(3) Uani 1 1 d . . . Al1 Al 0.50474(7) 0.24752(2) 0.12821(3) 0.01951(10) Uani 1 1 d . . . Si1 Si 0.43536(7) 0.08774(2) 0.11571(3) 0.02170(10) Uani 1 1 d . . . Si2 Si 0.38739(7) 0.33851(2) 0.28200(3) 0.02414(10) Uani 1 1 d . . . P1 P 0.36355(6) 0.191656(19) 0.24330(2) 0.01899(9) Uani 1 1 d . . . P2 P 0.05319(7) 0.16870(2) 0.28390(3) 0.03072(11) Uani 1 1 d . . . P3 P 0.51564(8) 0.14330(2) 0.34859(3) 0.02928(11) Uani 1 1 d . . . P4 P 0.22111(9) 0.08255(3) 0.34063(3) 0.03841(13) Uani 1 1 d . . . P5 P 0.22687(9) 0.17303(3) 0.40581(3) 0.04035(13) Uani 1 1 d . . . Cl1 Cl 0.32289(6) 0.28856(2) 0.02893(2) 0.03141(10) Uani 1 1 d . . . Cl2 Cl 0.83337(6) 0.25801(2) 0.11416(3) 0.03498(11) Uani 1 1 d . . . N1 N 0.4229(2) 0.16406(6) 0.15856(7) 0.0209(3) Uani 1 1 d . . . F1 F 0.7001(6) 0.47290(16) 0.07624(19) 0.0672(8) Uiso 0.50 1 d P A -1 C7 C 0.8667(9) 0.4865(3) 0.0348(3) 0.0453(13) Uiso 0.50 1 d P A -1 C8 C 0.9714(8) 0.4425(2) 0.0514(3) 0.0382(11) Uiso 0.50 1 d PD A -1 H8 H 0.975(8) 0.4036(15) 0.085(3) 0.046 Uiso 0.50 1 d PD B -1 C9 C 0.7991(8) 0.5383(2) 0.0066(3) 0.0315(9) Uiso 0.50 1 d PD A -1 H9 H 0.672(5) 0.5632(19) 0.016(3) 0.038 Uiso 0.50 1 d PD C -1 C10 C 0.8077(10) 0.4835(3) 0.0487(3) 0.0456(13) Uiso 0.50 1 d P A -1 C11 C 1.0378(8) 0.44384(19) 0.0367(3) 0.0287(8) Uiso 0.50 1 d PD A -1 H11 H 1.025(8) 0.4036(12) 0.067(3) 0.034 Uiso 0.50 1 d PD D -1 C12 C 0.8598(8) 0.5452(2) -0.0103(3) 0.0346(9) Uiso 0.50 1 d PD A -1 H12 H 0.724(4) 0.568(2) -0.007(3) 0.041 Uiso 0.50 1 d PD E -1 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 C1 0.0285(9) 0.0448(11) 0.0499(12) -0.0174(9) 0.0017(8) -0.0072(8) C2 0.0349(9) 0.0246(8) 0.0411(10) 0.0035(7) 0.0029(8) 0.0073(7) C3 0.0416(10) 0.0385(10) 0.0260(9) -0.0069(7) 0.0095(7) 0.0071(8) C4 0.0313(10) 0.0499(12) 0.0618(14) -0.0243(11) 0.0008(9) 0.0105(9) C5 0.0562(13) 0.0221(8) 0.0423(11) 0.0019(8) -0.0062(9) -0.0041(8) C6 0.0421(11) 0.0435(11) 0.0289(9) -0.0078(8) -0.0060(8) -0.0013(9) N2 0.0265(7) 0.0173(6) 0.0206(6) -0.0007(5) 0.0067(5) -0.0009(5) Al1 0.0207(2) 0.0204(2) 0.0178(2) 0.00287(17) 0.00401(17) 0.00033(17) Si1 0.0218(2) 0.0203(2) 0.0231(2) -0.00402(16) 0.00214(16) 0.00099(16) Si2 0.0247(2) 0.0210(2) 0.0259(2) -0.00604(17) -0.00110(17) 0.00194(16) P1 0.02321(19) 0.01855(18) 0.01571(17) 0.00057(14) 0.00448(14) -0.00067(14) P2 0.0275(2) 0.0374(3) 0.0285(2) 0.00553(18) 0.00882(17) -0.00475(18) P3 0.0344(2) 0.0344(2) 0.0188(2) 0.00563(17) 0.00087(17) -0.00096(18) P4 0.0482(3) 0.0335(3) 0.0336(3) 0.0131(2) 0.0044(2) -0.0104(2) P5 0.0472(3) 0.0548(3) 0.0212(2) -0.0006(2) 0.0138(2) -0.0034(2) Cl1 0.0282(2) 0.0383(2) 0.0273(2) 0.01248(17) 0.00043(15) 0.00348(17) Cl2 0.02120(19) 0.0500(3) 0.0342(2) 0.00828(19) 0.00517(16) -0.00232(17) N1 0.0282(7) 0.0183(6) 0.0170(6) 0.0006(5) 0.0054(5) 0.0010(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 C1 Si1 1.8581(19) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 Si1 1.8629(18) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 Si1 1.8576(18) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 Si2 1.855(2) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 Si2 1.860(2) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 Si2 1.8575(19) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? N2 P1 1.6227(13) . ? N2 Si2 1.7465(13) . ? N2 Al1 1.8826(14) . ? Al1 N1 1.8828(13) . ? Al1 Cl1 2.1184(6) . ? Al1 Cl2 2.1220(6) . ? Al1 P1 2.5043(6) . ? Si1 N1 1.7384(13) . ? P1 N1 1.6232(13) . ? P1 P3 2.1831(6) . ? P1 P2 2.1910(6) . ? P2 P4 2.2369(7) . ? P2 P5 2.2445(7) . ? P3 P5 2.2332(7) . ? P3 P4 2.2347(7) . ? P4 P5 2.1671(8) . ? F1 C10 0.889(6) . ? F1 C7 1.350(6) . ? F1 C8 1.909(6) . ? C7 C8 1.141(7) . ? C7 C9 1.229(7) . ? C7 C11 1.391(7) . ? C7 C12 1.429(7) . ? C8 C11 0.509(5) . ? C8 C10 1.333(7) . ? C8 H8 0.9800(10) . ? C8 H11 0.90(2) . ? C9 C12 0.520(5) . ? C9 C10 1.334(7) . ? C9 H9 0.9800(10) . ? C9 H12 0.79(2) . ? C10 C12 1.669(8) . ? C10 C11 1.697(8) . ? C11 H8 1.254(19) . ? C11 H11 0.9800(10) . ? C12 H12 0.9800(10) . ? 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 Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si2 C4 H4A 109.5 . . ? Si2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? P1 N2 Si2 133.75(8) . . ? P1 N2 Al1 90.88(6) . . ? Si2 N2 Al1 135.05(8) . . ? N2 Al1 N1 80.77(6) . . ? N2 Al1 Cl1 117.06(5) . . ? N1 Al1 Cl1 116.14(5) . . ? N2 Al1 Cl2 116.55(5) . . ? N1 Al1 Cl2 114.91(5) . . ? Cl1 Al1 Cl2 109.23(3) . . ? N2 Al1 P1 40.38(4) . . ? N1 Al1 P1 40.40(4) . . ? Cl1 Al1 P1 126.62(3) . . ? Cl2 Al1 P1 124.13(2) . . ? N1 Si1 C3 105.11(8) . . ? N1 Si1 C1 110.36(8) . . ? C3 Si1 C1 110.55(9) . . ? N1 Si1 C2 110.86(8) . . ? C3 Si1 C2 110.39(9) . . ? C1 Si1 C2 109.51(10) . . ? N2 Si2 C4 110.13(8) . . ? N2 Si2 C6 111.56(8) . . ? C4 Si2 C6 109.08(10) . . ? N2 Si2 C5 105.10(8) . . ? C4 Si2 C5 110.65(11) . . ? C6 Si2 C5 110.27(9) . . ? N2 P1 N1 97.47(7) . . ? N2 P1 P3 118.41(5) . . ? N1 P1 P3 116.27(5) . . ? N2 P1 P2 118.17(5) . . ? N1 P1 P2 119.59(5) . . ? P3 P1 P2 88.81(2) . . ? N2 P1 Al1 48.74(5) . . ? N1 P1 Al1 48.74(5) . . ? P3 P1 Al1 133.30(2) . . ? P2 P1 Al1 137.89(2) . . ? P1 P2 P4 84.62(2) . . ? P1 P2 P5 84.84(2) . . ? P4 P2 P5 57.84(2) . . ? P1 P3 P5 85.29(2) . . ? P1 P3 P4 84.86(2) . . ? P5 P3 P4 58.03(2) . . ? P5 P4 P3 60.95(2) . . ? P5 P4 P2 61.26(2) . . ? P3 P4 P2 86.39(2) . . ? P4 P5 P3 61.02(2) . . ? P4 P5 P2 60.91(2) . . ? P3 P5 P2 86.24(2) . . ? P1 N1 Si1 135.32(8) . . ? P1 N1 Al1 90.86(6) . . ? Si1 N1 Al1 133.50(8) . . ? C10 F1 C7 2.4(5) . . ? C10 F1 C8 38.5(4) . . ? C7 F1 C8 36.1(3) . . ? C8 C7 C9 163.2(7) . . ? C8 C7 F1 99.7(5) . . ? C9 C7 F1 97.2(5) . . ? C8 C7 C11 20.3(3) . . ? C9 C7 C11 142.9(6) . . ? F1 C7 C11 119.9(5) . . ? C8 C7 C12 142.3(6) . . ? C9 C7 C12 20.8(3) . . ? F1 C7 C12 118.0(5) . . ? C11 C7 C12 122.0(5) . . ? C11 C8 C7 108.7(10) . . ? C11 C8 C10 128.4(10) . . ? C7 C8 C10 19.7(4) . . ? C11 C8 F1 152.9(9) . . ? C7 C8 F1 44.2(4) . . ? C10 C8 F1 24.5(3) . . ? C11 C8 H8 111(3) . . ? C7 C8 H8 141(3) . . ? C10 C8 H8 121(3) . . ? F1 C8 H8 96(3) . . ? C11 C8 H11 83(2) . . ? C7 C8 H11 167(3) . . ? C10 C8 H11 148(3) . . ? F1 C8 H11 123(3) . . ? H8 C8 H11 28(4) . . ? C12 C9 C7 101.9(9) . . ? C12 C9 C10 122.2(9) . . ? C7 C9 C10 20.3(3) . . ? C12 C9 H9 128(3) . . ? C7 C9 H9 130(3) . . ? C10 C9 H9 110(3) . . ? C12 C9 H12 95(3) . . ? C7 C9 H12 163(3) . . ? C10 C9 H12 143(3) . . ? H9 C9 H12 34(4) . . ? F1 C10 C8 117.0(6) . . ? F1 C10 C9 119.9(6) . . ? C8 C10 C9 123.1(6) . . ? F1 C10 C12 135.1(6) . . ? C8 C10 C12 107.9(5) . . ? C9 C10 C12 15.3(3) . . ? F1 C10 C11 130.6(6) . . ? C8 C10 C11 13.6(3) . . ? C9 C10 C11 109.5(5) . . ? C12 C10 C11 94.3(4) . . ? C8 C11 C7 51.0(8) . . ? C8 C11 C10 38.0(8) . . ? C7 C11 C10 13.0(3) . . ? C8 C11 H8 47(2) . . ? C7 C11 H8 98(2) . . ? C10 C11 H8 85(2) . . ? C8 C11 H11 66(3) . . ? C7 C11 H11 116(3) . . ? C10 C11 H11 103(3) . . ? H8 C11 H11 19(4) . . ? C9 C12 C7 57.3(8) . . ? C9 C12 C10 42.5(7) . . ? C7 C12 C10 14.8(3) . . ? C9 C12 H9 34.9(19) . . ? C7 C12 H9 92.0(18) . . ? C10 C12 H9 77.3(17) . . ? C9 C12 H12 54(3) . . ? C7 C12 H12 111(3) . . ? C10 C12 H12 96(3) . . ? H9 C12 H12 20(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.547 _refine_diff_density_min -0.257 _refine_diff_density_rms 0.067 # Attachment 'jjw0066.cif' #============================================================================== data_jjw0066 _database_code_depnum_ccdc_archive 'CCDC 783482' #TrackingRef 'jjw0066.cif' _audit_update_record ; 2010-07-06 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H18 Cl2 N2 P5 Si3, Cl4 Ga' _chemical_formula_sum 'C6 H18 Cl6 Ga N2 P5 Si3' _chemical_formula_weight 639.76 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 '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 9.3085(6) _cell_length_b 9.8158(7) _cell_length_c 14.7125(10) _cell_angle_alpha 87.5680(10) _cell_angle_beta 80.7320(10) _cell_angle_gamma 71.5780(10) _cell_volume 1258.70(15) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 1 _cell_measurement_theta_max 22.5 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.688 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 636 _exptl_absorpt_coefficient_mu 2.188 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7074 _exptl_absorpt_correction_T_max 0.9176 _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. SADABS reports ratio of Tmin/Tmax = 0.725860 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13664 _diffrn_reflns_av_R_equivalents 0.0188 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 28.70 _reflns_number_total 6480 _reflns_number_gt 5661 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2(Bruker AXS, 2007)' _computing_cell_refinement 'APEX2(Bruker AXS, 2007)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2007 )' _computing_structure_solution ; SHELXS-97 , G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122 ; _computing_structure_refinement ; SHELXL-97, G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122 ; _computing_molecular_graphics ; ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0331P)^2^+0.2524P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6480 _refine_ls_number_parameters 214 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0253 _refine_ls_wR_factor_ref 0.0650 _refine_ls_wR_factor_gt 0.0623 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 C1 C 1.1161(2) 0.7836(2) 0.34088(14) 0.0394(5) Uani 1 1 d . . . H1A H 1.1409 0.6831 0.3601 0.059 Uiso 1 1 calc R . . H1B H 1.1726 0.8319 0.3718 0.059 Uiso 1 1 calc R . . H1C H 1.1452 0.7878 0.2740 0.059 Uiso 1 1 calc R . . C2 C 0.8482(3) 1.0552(2) 0.32150(16) 0.0416(5) Uani 1 1 d . . . H2A H 0.8839 1.0482 0.2549 0.062 Uiso 1 1 calc R . . H2B H 0.8931 1.1179 0.3494 0.062 Uiso 1 1 calc R . . H2C H 0.7362 1.0954 0.3331 0.062 Uiso 1 1 calc R . . C3 C 0.8455(3) 0.8782(3) 0.49840(13) 0.0435(5) Uani 1 1 d . . . H3A H 0.7337 0.9198 0.5121 0.065 Uiso 1 1 calc R . . H3B H 0.8935 0.9367 0.5278 0.065 Uiso 1 1 calc R . . H3C H 0.8764 0.7802 0.5222 0.065 Uiso 1 1 calc R . . C4 C 0.7607(2) 0.3694(2) 0.13969(15) 0.0354(4) Uani 1 1 d . . . H4A H 0.7989 0.4167 0.0855 0.053 Uiso 1 1 calc R . . H4B H 0.7179 0.2982 0.1201 0.053 Uiso 1 1 calc R . . H4C H 0.8452 0.3214 0.1735 0.053 Uiso 1 1 calc R . . C5 C 0.4672(2) 0.6250(2) 0.14973(14) 0.0344(4) Uani 1 1 d . . . H5A H 0.4052 0.7092 0.1876 0.052 Uiso 1 1 calc R . . H5B H 0.4005 0.5734 0.1330 0.052 Uiso 1 1 calc R . . H5C H 0.5203 0.6561 0.0937 0.052 Uiso 1 1 calc R . . C6 C 0.5193(2) 0.4254(2) 0.31583(14) 0.0369(4) Uani 1 1 d . . . H6A H 0.5974 0.3732 0.3530 0.055 Uiso 1 1 calc R . . H6B H 0.4721 0.3590 0.2945 0.055 Uiso 1 1 calc R . . H6C H 0.4405 0.5019 0.3532 0.055 Uiso 1 1 calc R . . N1 N 0.80945(15) 0.76825(15) 0.32911(9) 0.0221(3) Uani 1 1 d . . . N2 N 0.70011(15) 0.61250(15) 0.26622(9) 0.0227(3) Uani 1 1 d . . . Si2 Si 0.90733(5) 0.87452(5) 0.37259(3) 0.02442(10) Uani 1 1 d . . . Si3 Si 0.60954(5) 0.50513(5) 0.21538(3) 0.02279(10) Uani 1 1 d . . . P1 P 0.80423(5) 0.71709(4) 0.22343(3) 0.01937(9) Uani 1 1 d . . . P2 P 1.02139(5) 0.62549(5) 0.13546(3) 0.02522(10) Uani 1 1 d . . . P3 P 0.71905(5) 0.87010(5) 0.11819(3) 0.02633(10) Uani 1 1 d . . . P4 P 0.87560(5) 0.69365(5) 0.02378(3) 0.02742(10) Uani 1 1 d . . . P5 P 0.96880(6) 0.84548(5) 0.07463(3) 0.03119(11) Uani 1 1 d . . . Cl1 Cl 0.81544(6) 0.49800(5) 0.45510(3) 0.03698(11) Uani 1 1 d . . . Cl2 Cl 0.49982(5) 0.75667(5) 0.45393(3) 0.03564(11) Uani 1 1 d . . . Cl3 Cl 0.88900(6) 0.68056(6) 0.72832(4) 0.04776(14) Uani 1 1 d . . . Cl4 Cl 0.56614(6) 0.74036(6) 0.90422(3) 0.03908(12) Uani 1 1 d . . . Cl5 Cl 0.54968(5) 0.96666(6) 0.70829(3) 0.03825(11) Uani 1 1 d . . . Cl6 Cl 0.77400(7) 0.98651(6) 0.87728(4) 0.04868(14) Uani 1 1 d . . . Ga1 Ga 0.69538(2) 0.84249(2) 0.803908(13) 0.02538(6) Uani 1 1 d . . . Si1 Si 0.70412(5) 0.65891(5) 0.37761(3) 0.02264(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0253(9) 0.0528(12) 0.0393(11) -0.0043(9) -0.0072(8) -0.0092(9) C2 0.0453(12) 0.0286(10) 0.0548(13) 0.0029(9) -0.0165(10) -0.0133(9) C3 0.0525(13) 0.0582(14) 0.0242(9) -0.0104(9) -0.0011(9) -0.0246(11) C4 0.0267(9) 0.0322(10) 0.0469(11) -0.0110(8) -0.0001(8) -0.0101(8) C5 0.0273(9) 0.0404(11) 0.0371(10) 0.0083(8) -0.0082(8) -0.0122(8) C6 0.0426(11) 0.0390(11) 0.0336(10) 0.0056(8) -0.0001(8) -0.0229(9) N1 0.0253(7) 0.0255(7) 0.0152(6) 0.0005(5) -0.0010(5) -0.0085(6) N2 0.0246(7) 0.0254(7) 0.0189(6) 0.0019(5) -0.0005(5) -0.0107(6) Si2 0.0237(2) 0.0282(2) 0.0210(2) -0.00327(18) -0.00381(17) -0.00708(18) Si3 0.0199(2) 0.0248(2) 0.0238(2) 0.00079(18) -0.00047(17) -0.00869(17) P1 0.02043(19) 0.02084(19) 0.01592(18) 0.00114(15) -0.00109(15) -0.00615(15) P2 0.0204(2) 0.0292(2) 0.0221(2) 0.00070(17) -0.00021(16) -0.00376(17) P3 0.0272(2) 0.0254(2) 0.0198(2) 0.00266(16) -0.00112(17) -0.00062(17) P4 0.0282(2) 0.0325(2) 0.0187(2) -0.00418(17) -0.00229(17) -0.00562(18) P5 0.0350(3) 0.0326(2) 0.0287(2) 0.00601(19) -0.00024(19) -0.0174(2) Cl1 0.0381(2) 0.0356(2) 0.0296(2) 0.01190(18) -0.00587(18) -0.00202(19) Cl2 0.0289(2) 0.0412(3) 0.0266(2) 0.00475(18) 0.00655(17) -0.00245(19) Cl3 0.0359(3) 0.0430(3) 0.0469(3) 0.0097(2) 0.0032(2) 0.0063(2) Cl4 0.0428(3) 0.0559(3) 0.0289(2) 0.0108(2) -0.00703(19) -0.0306(2) Cl5 0.0303(2) 0.0479(3) 0.0252(2) 0.00670(19) -0.00542(17) 0.0035(2) Cl6 0.0655(4) 0.0413(3) 0.0562(3) 0.0162(2) -0.0311(3) -0.0321(3) Ga1 0.02259(10) 0.02845(10) 0.02504(10) 0.00717(8) -0.00560(7) -0.00787(8) Si1 0.0235(2) 0.0250(2) 0.0173(2) 0.00367(17) -0.00089(17) -0.00615(18) _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 C1 Si2 1.8545(19) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 Si2 1.848(2) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 Si2 1.846(2) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 Si3 1.8523(19) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 Si3 1.8448(18) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 Si3 1.8491(19) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? N1 P1 1.6667(14) . ? N1 Si1 1.7312(14) . ? N1 Si2 1.7812(14) . ? N2 P1 1.6634(14) . ? N2 Si1 1.7287(14) . ? N2 Si3 1.7924(14) . ? P1 P2 2.1626(6) . ? P1 P3 2.1741(6) . ? P1 Si1 2.4260(6) . ? P2 P5 2.2388(7) . ? P2 P4 2.2450(6) . ? P3 P4 2.2383(6) . ? P3 P5 2.2476(7) . ? P4 P5 2.1573(7) . ? Cl1 Si1 2.0154(6) . ? Cl2 Si1 2.0121(6) . ? Cl3 Ga1 2.1692(5) . ? Cl4 Ga1 2.1669(5) . ? Cl5 Ga1 2.1744(5) . ? Cl6 Ga1 2.1765(5) . ? 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 Si2 C1 H1A 109.5 . . ? Si2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si2 C2 H2A 109.5 . . ? Si2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si2 C3 H3A 109.5 . . ? Si2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si3 C4 H4A 109.5 . . ? Si3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si3 C5 H5A 109.5 . . ? Si3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si3 C6 H6A 109.5 . . ? Si3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? P1 N1 Si1 91.10(7) . . ? P1 N1 Si2 133.38(8) . . ? Si1 N1 Si2 135.06(8) . . ? P1 N2 Si1 91.30(7) . . ? P1 N2 Si3 133.71(8) . . ? Si1 N2 Si3 134.86(8) . . ? N1 Si2 C3 104.33(8) . . ? N1 Si2 C2 108.50(8) . . ? C3 Si2 C2 112.30(11) . . ? N1 Si2 C1 107.84(8) . . ? C3 Si2 C1 111.93(10) . . ? C2 Si2 C1 111.53(10) . . ? N2 Si3 C5 108.03(8) . . ? N2 Si3 C6 103.52(8) . . ? C5 Si3 C6 112.38(9) . . ? N2 Si3 C4 107.73(7) . . ? C5 Si3 C4 111.59(10) . . ? C6 Si3 C4 113.04(10) . . ? N2 P1 N1 90.94(7) . . ? N2 P1 P2 119.87(5) . . ? N1 P1 P2 117.23(5) . . ? N2 P1 P3 117.72(5) . . ? N1 P1 P3 122.35(5) . . ? P2 P1 P3 91.54(2) . . ? N2 P1 Si1 45.43(5) . . ? N1 P1 Si1 45.52(5) . . ? P2 P1 Si1 132.26(2) . . ? P3 P1 Si1 136.17(2) . . ? P1 P2 P5 83.74(2) . . ? P1 P2 P4 82.53(2) . . ? P5 P2 P4 57.52(2) . . ? P1 P3 P4 82.43(2) . . ? P1 P3 P5 83.27(2) . . ? P4 P3 P5 57.49(2) . . ? P5 P4 P3 61.47(2) . . ? P5 P4 P2 61.10(2) . . ? P3 P4 P2 87.76(2) . . ? P4 P5 P2 61.39(2) . . ? P4 P5 P3 61.04(2) . . ? P2 P5 P3 87.68(2) . . ? Cl4 Ga1 Cl3 109.79(2) . . ? Cl4 Ga1 Cl5 110.03(2) . . ? Cl3 Ga1 Cl5 109.44(2) . . ? Cl4 Ga1 Cl6 108.12(2) . . ? Cl3 Ga1 Cl6 110.43(3) . . ? Cl5 Ga1 Cl6 109.02(2) . . ? N2 Si1 N1 86.65(6) . . ? N2 Si1 Cl2 116.23(5) . . ? N1 Si1 Cl2 116.71(5) . . ? N2 Si1 Cl1 115.70(5) . . ? N1 Si1 Cl1 114.91(5) . . ? Cl2 Si1 Cl1 106.23(3) . . ? N2 Si1 P1 43.27(5) . . ? N1 Si1 P1 43.39(5) . . ? Cl2 Si1 P1 128.43(3) . . ? Cl1 Si1 P1 125.34(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.480 _refine_diff_density_min -0.337 _refine_diff_density_rms 0.072