# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 #TrackingRef '- ccdc_sub.cif' _publ_contact_author ; Evamarie Hey-Hawkins Structure Determination: L\"onnecke, Peter Institut f\"ur Anorganische Chemie Universit\"at Leipzig Johannisallee 29 04103 Leipzig Bundesrepublik Deutschland ; _publ_contact_author_phone '49 / 341 / 9736151' _publ_contact_author_fax '49 / 341 / 9739319' _publ_contact_author_email hey@uni-leipzig.de _publ_section_title ; Endocyclic P-P bond cleavage in carbaborane-substituted 1,2-diphosphetane -- A new route to secondary phosphinocarbaboranes ; loop_ _publ_author_name _publ_author_address 'Evamarie Hey-Hawkins' ; Institut f\"ur Anorganische Chemie Universit\"at Leipzig Johannisallee 29 04103 Leipzig Germany ; 'Peter Lonnecke' ; Institut f\"ur Anorganische Chemie Universit\"at Leipzig Johannisallee 29 04103 Leipzig Germany ; 'Anika Kreienbrink' ; Institut f\"ur Analytische Chemie Universit\"at Leipzig Linn\'estra\&se 3 04103 Leipzig Germany ; 'Matthias Findeisen' ; Institut f\"ur Anorganische Chemie Universit\"at Leipzig Johannisallee 29 04103 Leipzig Germany ; _publ_requested_category FO _publ_contact_author_name 'Evamarie Hey-Hawkins' #------------------------------------------------------------------------------# # DATA BLOCK # #------------------------------------------------------------------------------# #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2012-03-27 at 12:11:37 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\xray\wingx\files\archive.reqdat # CIF files read : x1433fin x1433 data_x1433fin _database_code_depnum_ccdc_archive 'CCDC 877502' #TrackingRef '- ccdc_sub.cif' _audit_creation_date 2012-03-27T12:11:37-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C6 H21 B10 P' _chemical_formula_weight 232.3 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.6520(4) _cell_length_b 10.6114(3) _cell_length_c 13.2551(6) _cell_angle_alpha 90 _cell_angle_beta 112.994(5) _cell_angle_gamma 90 _cell_volume 1379.22(9) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 2948 _cell_measurement_theta_min 2.8363 _cell_measurement_theta_max 32.5148 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.119 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 488 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.162 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.99677 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.356 _diffrn_orient_matrix_ub_11 -0.026828 _diffrn_orient_matrix_ub_12 0.0508555 _diffrn_orient_matrix_ub_13 -0.0369078 _diffrn_orient_matrix_ub_21 -0.0213347 _diffrn_orient_matrix_ub_22 -0.0427656 _diffrn_orient_matrix_ub_23 -0.0446441 _diffrn_orient_matrix_ub_31 -0.0637179 _diffrn_orient_matrix_ub_32 -0.0070912 _diffrn_orient_matrix_ub_33 0.0047433 _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0649 _diffrn_reflns_av_unetI/netI 0.0678 _diffrn_reflns_number 15173 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 30.51 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 4206 _reflns_number_gt 2993 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_structure_solution ; SIR92 A. Altomare, G. Cascarano, C. Giacovazzo and A. Guagliardi, J. Appl. Crystallogr. 1993, 26, 343-350. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ; ORTEP3 for Windows L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565. ; _computing_publication_material ; WINGX L.J. Farrugia, J. Appl. Cryst., 1999, 32, 837-838. ; #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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. The bond length analysis revealed a disorder of C(1) and B(5) with a ratio of 0.53(2) : 0.47(2). The PH hydrogen atom H(1P)and H(1PF) respectively is disordered as well (Ratio 0.50(2) : 0.50(2)) ; _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^)+(0.0466P)^2^+0.2938P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_number_reflns 4206 _refine_ls_number_parameters 243 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.087 _refine_ls_R_factor_gt 0.0541 _refine_ls_wR_factor_ref 0.1218 _refine_ls_wR_factor_gt 0.1091 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.288 _refine_diff_density_min -0.266 _refine_diff_density_rms 0.054 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 1.05463(4) 0.35482(4) 0.92212(4) 0.02501(13) Uani 1 1 d D . . C1 C 0.78619(19) 0.30662(17) 0.93299(17) 0.0228(4) Uani 0.49(2) 1 d P . . C1F C 0.75699(18) 0.39569(17) 0.81940(15) 0.0225(4) Uani 0.51(2) 1 d P . . C2 C 0.88097(15) 0.28471(14) 0.85712(13) 0.0168(3) Uani 1 1 d . . . C3 C 1.17761(16) 0.26238(15) 0.88333(14) 0.0213(3) Uani 1 1 d . . . C4 C 1.1984(2) 0.12894(18) 0.9299(2) 0.0328(4) Uani 1 1 d . . . C5 C 1.14264(19) 0.26213(19) 0.75980(16) 0.0277(4) Uani 1 1 d . . . C6 C 1.31024(19) 0.3379(2) 0.94035(18) 0.0301(4) Uani 1 1 d . . . B1 B 0.61974(19) 0.34183(18) 0.84610(16) 0.0219(4) Uani 1 1 d . . . B2 B 0.66488(19) 0.18858(18) 0.90321(16) 0.0208(4) Uani 1 1 d . . . B3 B 0.55788(19) 0.20686(19) 0.76222(16) 0.0215(4) Uani 1 1 d . . . B4 B 0.61575(19) 0.34001(18) 0.71044(16) 0.0217(4) Uani 1 1 d . . . B5 B 0.75699(18) 0.39569(17) 0.81940(15) 0.0225(4) Uani 0.49(2) 1 d P . . B5F B 0.78619(19) 0.30662(17) 0.93299(17) 0.0228(4) Uani 0.51(2) 1 d P . . B6 B 0.83326(18) 0.15490(17) 0.91234(15) 0.0176(3) Uani 1 1 d . . . B7 B 0.69021(18) 0.09116(17) 0.80323(16) 0.0191(4) Uani 1 1 d . . . B8 B 0.66002(19) 0.18517(18) 0.68394(16) 0.0202(4) Uani 1 1 d . . . B9 B 0.78371(18) 0.30618(18) 0.71980(15) 0.0186(4) Uani 1 1 d . . . B10 B 0.82871(18) 0.15287(16) 0.77659(15) 0.0174(3) Uani 1 1 d . . . H1P H 1.096(3) 0.331(3) 1.027(2) 0.006(5) Uiso 0.50(2) 1 d PD . . H1PF H 1.044(3) 0.464(2) 0.876(2) 0.006(5) Uiso 0.50(2) 1 d PD . . H1X H 0.5663(19) 0.4069(18) 0.8744(16) 0.029(5) Uiso 1 1 d . . . H2X H 0.6333(18) 0.1541(16) 0.9690(15) 0.022(5) Uiso 1 1 d . . . H3X H 0.4490(19) 0.1831(17) 0.7336(15) 0.025(5) Uiso 1 1 d . . . H4X H 0.552(2) 0.4060(18) 0.6505(17) 0.032(5) Uiso 1 1 d . . . H5X H 0.791(2) 0.4909(19) 0.8316(16) 0.032(5) Uiso 1 1 d . . . H6X H 0.9138(19) 0.1104(17) 0.9815(16) 0.028(5) Uiso 1 1 d . . . H7X H 0.6694(18) -0.0094(17) 0.7982(15) 0.025(5) Uiso 1 1 d . . . H8X H 0.6215(19) 0.1494(16) 0.6014(16) 0.025(5) Uiso 1 1 d . . . H9X H 0.8308(16) 0.3489(15) 0.6700(14) 0.014(4) Uiso 1 1 d . . . H10X H 0.9013(18) 0.0991(16) 0.7582(15) 0.019(4) Uiso 1 1 d . . . H1 H 0.835(2) 0.3508(19) 1.0075(18) 0.034(6) Uiso 1 1 d . . . H4A H 1.116(2) 0.0741(19) 0.8976(17) 0.034(6) Uiso 1 1 d . . . H4B H 1.272(2) 0.090(2) 0.9181(18) 0.045(6) Uiso 1 1 d . . . H4C H 1.223(2) 0.133(2) 1.008(2) 0.043(6) Uiso 1 1 d . . . H5A H 1.062(2) 0.2101(19) 0.7175(17) 0.033(5) Uiso 1 1 d . . . H5B H 1.217(2) 0.2260(19) 0.7446(17) 0.038(6) Uiso 1 1 d . . . H5C H 1.124(2) 0.351(2) 0.7246(18) 0.042(6) Uiso 1 1 d . . . H6A H 1.334(2) 0.346(2) 1.021(2) 0.049(7) Uiso 1 1 d . . . H6B H 1.302(2) 0.425(2) 0.9127(18) 0.042(6) Uiso 1 1 d . . . H6C H 1.382(2) 0.296(2) 0.9271(18) 0.043(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0187(2) 0.0238(2) 0.0320(3) -0.0110(2) 0.00929(19) -0.00529(17) C1 0.0234(9) 0.0204(8) 0.0288(10) -0.0014(7) 0.0148(8) -0.0003(7) C1F 0.0215(9) 0.0241(9) 0.0230(9) -0.0002(7) 0.0099(8) 0.0041(7) C2 0.0177(7) 0.0163(7) 0.0176(8) -0.0002(6) 0.0083(6) 0.0005(6) C3 0.0167(7) 0.0213(8) 0.0254(9) 0.0003(7) 0.0076(7) -0.0007(6) C4 0.0292(10) 0.0230(9) 0.0438(13) 0.0069(9) 0.0115(10) 0.0036(8) C5 0.0245(9) 0.0346(10) 0.0284(10) -0.0041(8) 0.0152(8) -0.0027(8) C6 0.0195(9) 0.0352(11) 0.0343(11) -0.0010(9) 0.0091(8) -0.0063(7) B1 0.0191(9) 0.0267(9) 0.0218(9) -0.0001(8) 0.0100(8) 0.0035(7) B2 0.0202(9) 0.0244(9) 0.0197(9) -0.0012(7) 0.0097(8) -0.0022(7) B3 0.0159(8) 0.0289(10) 0.0210(9) -0.0016(8) 0.0086(8) 0.0000(7) B4 0.0200(9) 0.0269(10) 0.0180(9) 0.0017(7) 0.0072(8) 0.0039(7) B5 0.0215(9) 0.0241(9) 0.0230(9) -0.0002(7) 0.0099(8) 0.0041(7) B5F 0.0234(9) 0.0204(8) 0.0288(10) -0.0014(7) 0.0148(8) -0.0003(7) B6 0.0189(8) 0.0174(8) 0.0164(8) 0.0009(7) 0.0068(7) -0.0015(7) B7 0.0176(8) 0.0213(9) 0.0194(9) -0.0017(7) 0.0082(7) -0.0025(7) B8 0.0182(9) 0.0255(9) 0.0161(9) -0.0028(7) 0.0059(7) -0.0011(7) B9 0.0192(9) 0.0212(8) 0.0148(8) 0.0010(7) 0.0061(7) 0.0016(7) B10 0.0177(8) 0.0159(8) 0.0188(9) -0.0017(7) 0.0074(7) -0.0017(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C3 1.8625(16) . ? P1 C2 1.8635(16) . ? P1 H1P 1.31(2) . ? P1 H1PF 1.29(2) . ? C1 C2 1.696(2) . ? C1 C1F 1.700(3) . ? C1 B2 1.731(3) . ? C1 B1 1.736(3) . ? C1 B6 1.739(3) . ? C1 H1 1.03(2) . ? C1F C2 1.693(2) . ? C1F B1 1.730(3) . ? C1F B4 1.732(3) . ? C1F B9 1.738(3) . ? C1F H5X 1.06(2) . ? C2 B10 1.715(2) . ? C2 B9 1.722(2) . ? C2 B6 1.727(2) . ? C3 C4 1.526(2) . ? C3 C5 1.531(3) . ? C3 C6 1.541(2) . ? C4 H4A 1.00(2) . ? C4 H4B 0.95(2) . ? C4 H4C 0.97(2) . ? C5 H5A 0.99(2) . ? C5 H5B 0.97(2) . ? C5 H5C 1.03(2) . ? C6 H6A 1.00(2) . ? C6 H6B 0.98(2) . ? C6 H6C 0.96(2) . ? B1 B3 1.775(3) . ? B1 B2 1.779(3) . ? B1 B4 1.782(3) . ? B1 H1X 1.053(19) . ? B2 B3 1.779(3) . ? B2 B7 1.782(3) . ? B2 B6 1.786(3) . ? B2 H2X 1.112(18) . ? B3 B4 1.783(3) . ? B3 B7 1.786(3) . ? B3 B8 1.787(3) . ? B3 H3X 1.100(18) . ? B4 B9 1.781(3) . ? B4 B8 1.782(3) . ? B4 H4X 1.08(2) . ? B6 B7 1.775(3) . ? B6 B10 1.781(3) . ? B6 H6X 1.088(19) . ? B7 B10 1.771(2) . ? B7 B8 1.789(3) . ? B7 H7X 1.087(18) . ? B8 B9 1.767(3) . ? B8 B10 1.769(3) . ? B8 H8X 1.076(19) . ? B9 B10 1.778(3) . ? B9 H9X 1.074(16) . ? B10 H10X 1.063(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 P1 C2 109.90(7) . . ? C3 P1 H1P 102.3(13) . . ? C2 P1 H1P 106.0(13) . . ? C3 P1 H1PF 106.5(13) . . ? C2 P1 H1PF 104.5(13) . . ? H1P P1 H1PF 127.0(19) . . ? C2 C1 C1F 59.78(10) . . ? C2 C1 B2 109.25(13) . . ? C1F C1 B2 109.77(15) . . ? C2 C1 B1 109.04(14) . . ? C1F C1 B1 60.45(11) . . ? B2 C1 B1 61.74(11) . . ? C2 C1 B6 60.33(10) . . ? C1F C1 B6 109.84(13) . . ? B2 C1 B6 61.95(10) . . ? B1 C1 B6 112.16(14) . . ? C2 C1 H1 116.1(11) . . ? C1F C1 H1 116.5(11) . . ? B2 C1 H1 126.6(11) . . ? B1 C1 H1 122.4(11) . . ? B6 C1 H1 120.3(11) . . ? C2 C1F C1 60.00(10) . . ? C2 C1F B1 109.51(13) . . ? C1 C1F B1 60.80(11) . . ? C2 C1F B4 109.41(13) . . ? C1 C1F B4 110.34(14) . . ? B1 C1F B4 61.96(11) . . ? C2 C1F B9 60.24(10) . . ? C1 C1F B9 109.96(13) . . ? B1 C1F B9 112.16(14) . . ? B4 C1F B9 61.76(11) . . ? C2 C1F H5X 115.9(11) . . ? C1 C1F H5X 117.3(11) . . ? B1 C1F H5X 123.1(10) . . ? B4 C1F H5X 125.7(11) . . ? B9 C1F H5X 119.3(10) . . ? C1F C2 C1 60.23(10) . . ? C1F C2 B10 110.95(12) . . ? C1 C2 B10 110.92(12) . . ? C1F C2 B9 61.17(10) . . ? C1 C2 B9 110.91(12) . . ? B10 C2 B9 62.30(10) . . ? C1F C2 B6 110.81(12) . . ? C1 C2 B6 61.07(10) . . ? B10 C2 B6 62.32(10) . . ? B9 C2 B6 113.48(12) . . ? C1F C2 P1 112.20(10) . . ? C1 C2 P1 112.60(11) . . ? B10 C2 P1 129.47(10) . . ? B9 C2 P1 120.97(10) . . ? B6 C2 P1 121.73(11) . . ? C4 C3 C5 111.53(16) . . ? C4 C3 C6 108.87(15) . . ? C5 C3 C6 108.60(15) . . ? C4 C3 P1 112.59(13) . . ? C5 C3 P1 113.12(12) . . ? C6 C3 P1 101.53(12) . . ? C3 C4 H4A 113.8(12) . . ? C3 C4 H4B 109.9(14) . . ? H4A C4 H4B 108.4(18) . . ? C3 C4 H4C 109.4(13) . . ? H4A C4 H4C 107.7(17) . . ? H4B C4 H4C 107.5(19) . . ? C3 C5 H5A 113.7(12) . . ? C3 C5 H5B 110.2(13) . . ? H5A C5 H5B 105.0(17) . . ? C3 C5 H5C 113.9(12) . . ? H5A C5 H5C 106.3(17) . . ? H5B C5 H5C 107.1(17) . . ? C3 C6 H6A 111.6(13) . . ? C3 C6 H6B 111.7(13) . . ? H6A C6 H6B 105.7(18) . . ? C3 C6 H6C 108.6(13) . . ? H6A C6 H6C 110.2(19) . . ? H6B C6 H6C 109.0(18) . . ? C1F B1 C1 58.75(10) . . ? C1F B1 B3 105.96(13) . . ? C1 B1 B3 105.96(13) . . ? C1F B1 B2 106.23(13) . . ? C1 B1 B2 58.99(10) . . ? B3 B1 B2 60.09(11) . . ? C1F B1 B4 59.08(11) . . ? C1 B1 B4 106.42(13) . . ? B3 B1 B4 60.16(11) . . ? B2 B1 B4 108.38(13) . . ? C1F B1 H1X 118.3(10) . . ? C1 B1 H1X 117.3(11) . . ? B3 B1 H1X 129.3(10) . . ? B2 B1 H1X 122.8(11) . . ? B4 B1 H1X 124.3(11) . . ? C1 B2 B1 59.28(11) . . ? C1 B2 B3 105.99(13) . . ? B1 B2 B3 59.84(11) . . ? C1 B2 B7 105.83(12) . . ? B1 B2 B7 107.94(13) . . ? B3 B2 B7 60.21(11) . . ? C1 B2 B6 59.26(10) . . ? B1 B2 B6 108.00(13) . . ? B3 B2 B6 107.89(12) . . ? B7 B2 B6 59.64(10) . . ? C1 B2 H2X 119.1(9) . . ? B1 B2 H2X 121.3(9) . . ? B3 B2 H2X 126.4(10) . . ? B7 B2 H2X 124.9(9) . . ? B6 B2 H2X 119.0(9) . . ? B1 B3 B2 60.08(11) . . ? B1 B3 B4 60.13(11) . . ? B2 B3 B4 108.36(13) . . ? B1 B3 B7 107.96(13) . . ? B2 B3 B7 59.99(11) . . ? B4 B3 B7 108.15(12) . . ? B1 B3 B8 107.84(13) . . ? B2 B3 B8 108.08(13) . . ? B4 B3 B8 59.88(11) . . ? B7 B3 B8 60.09(10) . . ? B1 B3 H3X 119.0(10) . . ? B2 B3 H3X 119.6(10) . . ? B4 B3 H3X 121.7(10) . . ? B7 B3 H3X 123.2(10) . . ? B8 B3 H3X 124.7(10) . . ? C1F B4 B9 59.27(10) . . ? C1F B4 B8 105.56(13) . . ? B9 B4 B8 59.46(10) . . ? C1F B4 B1 58.96(11) . . ? B9 B4 B1 107.73(13) . . ? B8 B4 B1 107.76(13) . . ? C1F B4 B3 105.52(14) . . ? B9 B4 B3 107.60(13) . . ? B8 B4 B3 60.19(11) . . ? B1 B4 B3 59.71(11) . . ? C1F B4 H4X 119.1(11) . . ? B9 B4 H4X 120.7(10) . . ? B8 B4 H4X 126.4(10) . . ? B1 B4 H4X 119.7(10) . . ? B3 B4 H4X 125.8(10) . . ? C2 B6 C1 58.60(10) . . ? C2 B6 B7 105.06(12) . . ? C1 B6 B7 105.81(13) . . ? C2 B6 B10 58.52(9) . . ? C1 B6 B10 105.93(13) . . ? B7 B6 B10 59.75(10) . . ? C2 B6 B2 105.41(12) . . ? C1 B6 B2 58.79(10) . . ? B7 B6 B2 60.08(10) . . ? B10 B6 B2 107.68(13) . . ? C2 B6 H6X 115.9(10) . . ? C1 B6 H6X 116.7(10) . . ? B7 B6 H6X 131.6(10) . . ? B10 B6 H6X 123.2(10) . . ? B2 B6 H6X 125.7(10) . . ? B10 B7 B6 60.31(10) . . ? B10 B7 B2 108.28(13) . . ? B6 B7 B2 60.28(10) . . ? B10 B7 B3 107.75(13) . . ? B6 B7 B3 108.08(13) . . ? B2 B7 B3 59.80(11) . . ? B10 B7 B8 59.59(10) . . ? B6 B7 B8 107.96(13) . . ? B2 B7 B8 107.85(13) . . ? B3 B7 B8 59.99(10) . . ? B10 B7 H7X 121.1(9) . . ? B6 B7 H7X 120.9(10) . . ? B2 B7 H7X 121.9(9) . . ? B3 B7 H7X 122.6(10) . . ? B8 B7 H7X 122.1(10) . . ? B9 B8 B10 60.37(10) . . ? B9 B8 B4 60.25(11) . . ? B10 B8 B4 108.48(13) . . ? B9 B8 B3 108.02(13) . . ? B10 B8 B3 107.79(13) . . ? B4 B8 B3 59.92(11) . . ? B9 B8 B7 108.05(13) . . ? B10 B8 B7 59.70(10) . . ? B4 B8 B7 108.06(13) . . ? B3 B8 B7 59.93(11) . . ? B9 B8 H8X 118.5(10) . . ? B10 B8 H8X 121.2(10) . . ? B4 B8 H8X 120.0(10) . . ? B3 B8 H8X 124.0(10) . . ? B7 B8 H8X 124.6(10) . . ? C2 B9 C1F 58.58(10) . . ? C2 B9 B8 105.41(13) . . ? C1F B9 B8 105.99(13) . . ? C2 B9 B10 58.67(10) . . ? C1F B9 B10 106.00(13) . . ? B8 B9 B10 59.88(10) . . ? C2 B9 B4 105.88(12) . . ? C1F B9 B4 58.97(11) . . ? B8 B9 B4 60.30(11) . . ? B10 B9 B4 108.14(13) . . ? C2 B9 H9X 118.3(9) . . ? C1F B9 H9X 119.4(9) . . ? B8 B9 H9X 128.3(9) . . ? B10 B9 H9X 122.2(9) . . ? B4 B9 H9X 124.8(9) . . ? C2 B10 B8 105.59(12) . . ? C2 B10 B7 105.70(12) . . ? B8 B10 B7 60.71(10) . . ? C2 B10 B9 59.04(10) . . ? B8 B10 B9 59.74(10) . . ? B7 B10 B9 108.36(12) . . ? C2 B10 B6 59.16(10) . . ? B8 B10 B6 108.57(12) . . ? B7 B10 B6 59.94(10) . . ? B9 B10 B6 108.25(12) . . ? C2 B10 H10X 119.5(10) . . ? B8 B10 H10X 125.2(10) . . ? B7 B10 H10X 125.7(9) . . ? B9 B10 H10X 119.6(9) . . ? B6 B10 H10X 120.2(10) . . ? # END of CIF #------------------------------------------------------------------------------# # END OF DATA BLOCK # #------------------------------------------------------------------------------# # Attachment '- cif file compound 3.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2012-07-05 at 11:32:17 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\xray\wingx\files\archive.reqdat # CIF files read : x1598fin x1598 data_x1598fin _database_code_depnum_ccdc_archive 'CCDC 891099' #TrackingRef '- cif file compound 3.cif' _audit_creation_date 2012-07-05T11:32:17-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C18 H37 B10 N P2' _chemical_formula_weight 437.53 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca 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' '-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 11.8524(8) _cell_length_b 19.2981(11) _cell_length_c 21.5647(16) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4932.5(6) _cell_formula_units_Z 8 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 1025 _cell_measurement_theta_min 2.8272 _cell_measurement_theta_max 26.5823 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description 'small needles' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.01 _exptl_crystal_density_diffrn 1.178 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1856 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.184 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.9701 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.356 _diffrn_orient_matrix_ub_11 0.020173 _diffrn_orient_matrix_ub_12 -0.0335503 _diffrn_orient_matrix_ub_13 -0.0075519 _diffrn_orient_matrix_ub_21 0.0489114 _diffrn_orient_matrix_ub_22 0.0148842 _diffrn_orient_matrix_ub_23 -0.0134921 _diffrn_orient_matrix_ub_31 0.027977 _diffrn_orient_matrix_ub_32 -0.0018068 _diffrn_orient_matrix_ub_33 0.0290346 _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.272 _diffrn_reflns_av_unetI/netI 0.1633 _diffrn_reflns_number 28712 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 23.26 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 3533 _reflns_number_gt 1734 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_structure_solution ; SIR92 A. Altomare, G. Cascarano, C. Giacovazzo and A. Guagliardi, J. Appl. Crystallogr. 1993, 26, 343-350. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ; ORTEP3 for Windows L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565. ; _computing_publication_material ; WINGX L.J. Farrugia, J. Appl. Cryst., 1999, 32, 837-838. ; #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0753P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 3533 _refine_ls_number_parameters 286 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1788 _refine_ls_R_factor_gt 0.0759 _refine_ls_wR_factor_ref 0.1942 _refine_ls_wR_factor_gt 0.1504 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.701 _refine_diff_density_min -0.291 _refine_diff_density_rms 0.072 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source P P 0.1023 0.0942 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.43296(13) 0.02668(8) 0.65289(7) 0.0310(5) Uani 1 1 d . . . P2 P 0.28158(13) 0.12585(8) 0.52737(8) 0.0285(5) Uani 1 1 d . . . N1 N 0.3326(4) -0.0134(2) 0.5436(2) 0.0326(13) Uani 1 1 d . . . C1 C 0.3925(4) 0.1223(3) 0.6616(3) 0.0274(15) Uani 1 1 d . . . C2 C 0.3416(4) 0.1700(3) 0.5986(3) 0.0243(15) Uani 1 1 d . . . C3 C 0.3084(5) -0.0076(3) 0.6103(3) 0.0334(17) Uani 1 1 d . . . H3A H 0.2881 -0.0538 0.627 0.04 Uiso 1 1 calc R . . H3B H 0.2432 0.0237 0.6167 0.04 Uiso 1 1 calc R . . C4 C 0.3793(5) 0.0503(3) 0.5194(3) 0.0306(16) Uani 1 1 d . . . H4A H 0.3976 0.0438 0.475 0.037 Uiso 1 1 calc R . . H4B H 0.4505 0.0608 0.5415 0.037 Uiso 1 1 calc R . . C5 C 0.4112(5) -0.0185(3) 0.7295(3) 0.0333(16) Uani 1 1 d . . . C6 C 0.4901(5) 0.0105(3) 0.7790(3) 0.0396(18) Uani 1 1 d . . . H6A H 0.4905 -0.0205 0.815 0.059 Uiso 1 1 calc R . . H6B H 0.4638 0.0565 0.7917 0.059 Uiso 1 1 calc R . . H6C H 0.5666 0.0141 0.7621 0.059 Uiso 1 1 calc R . . C7 C 0.2908(5) -0.0220(3) 0.7541(3) 0.0394(17) Uani 1 1 d . . . H7A H 0.2903 -0.0458 0.7942 0.059 Uiso 1 1 calc R . . H7B H 0.2435 -0.0475 0.7246 0.059 Uiso 1 1 calc R . . H7C H 0.2612 0.0251 0.7591 0.059 Uiso 1 1 calc R . . C8 C 0.4511(5) -0.0926(3) 0.7150(3) 0.0447(19) Uani 1 1 d . . . H8A H 0.5299 -0.0914 0.7013 0.067 Uiso 1 1 calc R . . H8B H 0.404 -0.1123 0.6821 0.067 Uiso 1 1 calc R . . H8C H 0.4448 -0.1212 0.7524 0.067 Uiso 1 1 calc R . . C9 C 0.2415(6) -0.0427(3) 0.5083(3) 0.0328(16) Uani 1 1 d . . . C10 C 0.1380(6) -0.0605(3) 0.5333(3) 0.0388(17) Uani 1 1 d . . . H10 H 0.1242 -0.0539 0.5762 0.047 Uiso 1 1 calc R . . C11 C 0.0547(6) -0.0878(3) 0.4958(3) 0.0429(18) Uani 1 1 d . . . H11 H -0.0165 -0.0992 0.5132 0.051 Uiso 1 1 calc R . . C12 C 0.0734(6) -0.0988(3) 0.4339(4) 0.0463(19) Uani 1 1 d . . . H12 H 0.0156 -0.1173 0.4083 0.056 Uiso 1 1 calc R . . C13 C 0.1775(7) -0.0825(3) 0.4093(3) 0.0462(19) Uani 1 1 d . . . H13 H 0.1914 -0.0906 0.3665 0.055 Uiso 1 1 calc R . . C14 C 0.2615(6) -0.0546(3) 0.4456(3) 0.0351(17) Uani 1 1 d . . . H14 H 0.3328 -0.0437 0.428 0.042 Uiso 1 1 calc R . . C15 C 0.3232(5) 0.1776(3) 0.4571(3) 0.0312(16) Uani 1 1 d . . . C16 C 0.4487(5) 0.1892(3) 0.4450(3) 0.0361(17) Uani 1 1 d . . . H16A H 0.4586 0.2122 0.4049 0.054 Uiso 1 1 calc R . . H16B H 0.4879 0.1445 0.4446 0.054 Uiso 1 1 calc R . . H16C H 0.4803 0.2185 0.4779 0.054 Uiso 1 1 calc R . . C17 C 0.2743(5) 0.1333(3) 0.4032(3) 0.0391(17) Uani 1 1 d . . . H17A H 0.2841 0.1581 0.3639 0.059 Uiso 1 1 calc R . . H17B H 0.1937 0.125 0.4105 0.059 Uiso 1 1 calc R . . H17C H 0.3141 0.0888 0.4013 0.059 Uiso 1 1 calc R . . C18 C 0.2568(5) 0.2461(3) 0.4561(3) 0.0370(17) Uani 1 1 d . . . H18A H 0.2849 0.2767 0.4889 0.055 Uiso 1 1 calc R . . H18B H 0.1766 0.2366 0.463 0.055 Uiso 1 1 calc R . . H18C H 0.2666 0.2686 0.4157 0.055 Uiso 1 1 calc R . . B1 B 0.3484(6) 0.1597(4) 0.7278(3) 0.0330(19) Uani 1 1 d . . . H1 H 0.3296 0.1295 0.7709 0.04 Uiso 1 1 calc R . . B2 B 0.4873(6) 0.1705(3) 0.7004(3) 0.0295(19) Uani 1 1 d . . . H2 H 0.5621 0.1477 0.7247 0.035 Uiso 1 1 calc R . . B3 B 0.4113(6) 0.2420(4) 0.7313(3) 0.035(2) Uani 1 1 d . . . H3 H 0.4347 0.2671 0.7763 0.042 Uiso 1 1 calc R . . B4 B 0.2681(6) 0.2336(4) 0.7081(4) 0.039(2) Uani 1 1 d . . . H4 H 0.1967 0.2528 0.7374 0.046 Uiso 1 1 calc R . . B5 B 0.2582(6) 0.1563(4) 0.6636(3) 0.0298(18) Uani 1 1 d . . . H5 H 0.1806 0.1232 0.6627 0.036 Uiso 1 1 calc R . . B6 B 0.4811(6) 0.1744(3) 0.6193(3) 0.0272(18) Uani 1 1 d . . . H6 H 0.5496 0.1531 0.589 0.033 Uiso 1 1 calc R . . B7 B 0.4961(6) 0.2515(4) 0.6639(3) 0.0298(18) Uani 1 1 d . . . H7 H 0.5758 0.2826 0.6643 0.036 Uiso 1 1 calc R . . B8 B 0.3595(6) 0.2904(4) 0.6673(3) 0.0346(19) Uani 1 1 d . . . H8 H 0.3482 0.3479 0.6697 0.041 Uiso 1 1 calc R . . B9 B 0.2651(6) 0.2387(4) 0.6261(3) 0.0310(19) Uani 1 1 d . . . H9 H 0.191 0.2613 0.601 0.037 Uiso 1 1 calc R . . B10 B 0.4054(5) 0.2497(3) 0.5991(3) 0.0277(18) Uani 1 1 d . . . H10A H 0.4256 0.2797 0.5561 0.033 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 0.0362(10) 0.0251(9) 0.0317(10) 0.0020(8) -0.0008(8) -0.0008(8) P2 0.0331(10) 0.0218(9) 0.0306(10) 0.0026(8) -0.0045(8) -0.0010(8) N1 0.048(3) 0.022(3) 0.028(3) 0.000(3) -0.001(3) -0.004(3) C1 0.030(4) 0.026(4) 0.026(4) -0.001(3) -0.007(3) 0.004(3) C2 0.024(3) 0.022(4) 0.026(4) 0.003(3) -0.010(3) 0.001(3) C3 0.043(4) 0.026(4) 0.031(4) 0.006(3) 0.004(3) 0.000(3) C4 0.036(4) 0.021(3) 0.035(4) 0.002(3) -0.007(3) -0.003(3) C5 0.035(4) 0.030(4) 0.035(4) 0.008(3) 0.002(3) 0.003(3) C6 0.039(4) 0.046(5) 0.034(4) 0.007(4) -0.005(3) 0.005(3) C7 0.050(5) 0.033(4) 0.035(4) 0.008(3) 0.001(3) -0.004(3) C8 0.063(5) 0.031(4) 0.040(4) 0.015(3) 0.003(4) 0.004(4) C9 0.046(4) 0.018(3) 0.035(4) 0.005(3) -0.002(4) -0.005(3) C10 0.055(5) 0.028(4) 0.033(4) 0.004(3) -0.004(4) -0.005(3) C11 0.042(4) 0.036(4) 0.050(5) 0.010(4) -0.007(4) -0.003(4) C12 0.049(5) 0.033(4) 0.056(6) 0.001(4) -0.026(4) -0.009(4) C13 0.068(6) 0.031(4) 0.039(5) -0.001(4) -0.004(4) -0.001(4) C14 0.044(4) 0.020(4) 0.041(5) -0.003(3) -0.001(4) -0.004(3) C15 0.042(4) 0.027(4) 0.025(4) 0.001(3) -0.006(3) -0.005(3) C16 0.042(4) 0.034(4) 0.032(4) 0.000(3) -0.003(3) -0.007(3) C17 0.053(4) 0.031(4) 0.033(4) 0.013(3) -0.005(3) -0.001(3) C18 0.045(4) 0.028(4) 0.038(4) 0.006(3) -0.010(3) 0.003(3) B1 0.043(5) 0.031(5) 0.025(5) 0.006(4) -0.001(4) -0.002(4) B2 0.037(5) 0.022(4) 0.029(5) -0.005(3) -0.005(4) 0.000(4) B3 0.047(5) 0.029(4) 0.030(5) -0.006(4) -0.001(4) -0.016(4) B4 0.047(5) 0.032(5) 0.037(5) 0.001(4) 0.013(4) 0.005(4) B5 0.025(4) 0.033(4) 0.031(5) 0.002(4) 0.011(3) -0.003(3) B6 0.027(4) 0.021(4) 0.034(5) 0.001(4) -0.004(3) -0.004(3) B7 0.040(5) 0.026(4) 0.024(4) -0.006(4) 0.000(4) -0.008(4) B8 0.052(5) 0.025(4) 0.027(5) -0.003(4) 0.004(4) 0.003(4) B9 0.024(4) 0.027(4) 0.041(5) 0.005(4) 0.003(3) 0.004(3) B10 0.035(4) 0.020(4) 0.029(4) -0.001(3) 0.003(3) -0.001(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C3 1.860(6) . ? P1 C5 1.886(6) . ? P1 C1 1.915(6) . ? P2 C4 1.869(6) . ? P2 C15 1.880(6) . ? P2 C2 1.895(6) . ? N1 C9 1.436(7) . ? N1 C4 1.447(7) . ? N1 C3 1.472(7) . ? C1 B1 1.682(9) . ? C1 B2 1.683(8) . ? C1 B6 1.717(9) . ? C1 B5 1.722(8) . ? C1 C2 1.750(7) . ? C2 B9 1.712(9) . ? C2 B10 1.713(8) . ? C2 B6 1.715(8) . ? C2 B5 1.735(8) . ? C5 C7 1.523(7) . ? C5 C6 1.526(8) . ? C5 C8 1.537(8) . ? C9 C10 1.383(8) . ? C9 C14 1.391(8) . ? C10 C11 1.380(8) . ? C11 C12 1.370(9) . ? C12 C13 1.379(9) . ? C13 C14 1.377(9) . ? C15 C16 1.527(7) . ? C15 C18 1.539(8) . ? C15 C17 1.555(8) . ? B1 B5 1.751(10) . ? B1 B3 1.755(9) . ? B1 B2 1.761(10) . ? B1 B4 1.767(10) . ? B2 B7 1.753(9) . ? B2 B6 1.754(10) . ? B2 B3 1.776(10) . ? B3 B8 1.776(10) . ? B3 B7 1.777(10) . ? B3 B4 1.777(10) . ? B4 B9 1.770(10) . ? B4 B8 1.773(10) . ? B4 B5 1.778(10) . ? B5 B9 1.786(10) . ? B6 B10 1.762(9) . ? B6 B7 1.781(9) . ? B7 B10 1.763(9) . ? B7 B8 1.787(10) . ? B8 B9 1.741(10) . ? B8 B10 1.754(9) . ? B9 B10 1.774(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 P1 C5 99.1(3) . . ? C3 P1 C1 101.1(3) . . ? C5 P1 C1 109.0(3) . . ? C4 P2 C15 100.2(3) . . ? C4 P2 C2 101.1(3) . . ? C15 P2 C2 108.4(3) . . ? C9 N1 C4 115.5(5) . . ? C9 N1 C3 113.7(5) . . ? C4 N1 C3 111.3(5) . . ? B1 C1 B2 63.1(4) . . ? B1 C1 B6 112.9(5) . . ? B2 C1 B6 62.1(4) . . ? B1 C1 B5 61.9(4) . . ? B2 C1 B5 113.2(5) . . ? B6 C1 B5 110.8(4) . . ? B1 C1 C2 109.0(4) . . ? B2 C1 C2 109.0(4) . . ? B6 C1 C2 59.3(3) . . ? B5 C1 C2 60.0(3) . . ? B1 C1 P1 125.1(4) . . ? B2 C1 P1 114.5(4) . . ? B6 C1 P1 111.0(4) . . ? B5 C1 P1 127.0(4) . . ? C2 C1 P1 121.1(4) . . ? B9 C2 B10 62.4(4) . . ? B9 C2 B6 112.5(4) . . ? B10 C2 B6 61.9(4) . . ? B9 C2 B5 62.4(4) . . ? B10 C2 B5 112.5(4) . . ? B6 C2 B5 110.3(4) . . ? B9 C2 C1 108.7(4) . . ? B10 C2 C1 108.4(4) . . ? B6 C2 C1 59.4(3) . . ? B5 C2 C1 59.2(3) . . ? B9 C2 P2 115.5(4) . . ? B10 C2 P2 125.1(4) . . ? B6 C2 P2 126.5(4) . . ? B5 C2 P2 111.8(4) . . ? C1 C2 P2 121.5(4) . . ? N1 C3 P1 110.8(4) . . ? N1 C4 P2 113.1(4) . . ? C7 C5 C6 110.3(5) . . ? C7 C5 C8 108.5(5) . . ? C6 C5 C8 107.2(5) . . ? C7 C5 P1 116.9(4) . . ? C6 C5 P1 111.1(4) . . ? C8 C5 P1 102.1(4) . . ? C10 C9 C14 119.2(6) . . ? C10 C9 N1 123.9(6) . . ? C14 C9 N1 116.9(6) . . ? C11 C10 C9 120.1(6) . . ? C12 C11 C10 120.9(7) . . ? C11 C12 C13 119.0(6) . . ? C14 C13 C12 121.1(7) . . ? C13 C14 C9 119.7(6) . . ? C16 C15 C18 111.7(5) . . ? C16 C15 C17 108.5(5) . . ? C18 C15 C17 105.7(5) . . ? C16 C15 P2 118.1(4) . . ? C18 C15 P2 109.5(4) . . ? C17 C15 P2 102.3(4) . . ? C1 B1 B5 60.2(4) . . ? C1 B1 B3 107.1(5) . . ? B5 B1 B3 109.1(5) . . ? C1 B1 B2 58.5(4) . . ? B5 B1 B2 108.1(5) . . ? B3 B1 B2 60.7(4) . . ? C1 B1 B4 108.0(5) . . ? B5 B1 B4 60.7(4) . . ? B3 B1 B4 60.6(4) . . ? B2 B1 B4 109.1(5) . . ? C1 B2 B7 108.0(5) . . ? C1 B2 B6 59.9(4) . . ? B7 B2 B6 61.0(4) . . ? C1 B2 B1 58.4(4) . . ? B7 B2 B1 108.2(5) . . ? B6 B2 B1 107.5(5) . . ? C1 B2 B3 106.1(5) . . ? B7 B2 B3 60.4(4) . . ? B6 B2 B3 108.6(5) . . ? B1 B2 B3 59.5(4) . . ? B1 B3 B8 107.2(5) . . ? B1 B3 B2 59.8(4) . . ? B8 B3 B2 107.0(5) . . ? B1 B3 B7 107.3(5) . . ? B8 B3 B7 60.4(4) . . ? B2 B3 B7 59.1(4) . . ? B1 B3 B4 60.0(4) . . ? B8 B3 B4 59.9(4) . . ? B2 B3 B4 108.0(5) . . ? B7 B3 B4 108.6(5) . . ? B1 B4 B9 107.2(5) . . ? B1 B4 B8 106.8(5) . . ? B9 B4 B8 58.9(4) . . ? B1 B4 B3 59.4(4) . . ? B9 B4 B3 107.2(5) . . ? B8 B4 B3 60.0(4) . . ? B1 B4 B5 59.2(4) . . ? B9 B4 B5 60.4(4) . . ? B8 B4 B5 106.9(5) . . ? B3 B4 B5 106.9(5) . . ? C1 B5 C2 60.8(3) . . ? C1 B5 B1 57.9(4) . . ? C2 B5 B1 106.6(4) . . ? C1 B5 B4 105.8(5) . . ? C2 B5 B4 105.7(5) . . ? B1 B5 B4 60.1(4) . . ? C1 B5 B9 106.6(4) . . ? C2 B5 B9 58.2(4) . . ? B1 B5 B9 107.2(5) . . ? B4 B5 B9 59.5(4) . . ? C2 B6 C1 61.3(3) . . ? C2 B6 B2 107.3(5) . . ? C1 B6 B2 58.0(4) . . ? C2 B6 B10 59.0(3) . . ? C1 B6 B10 107.6(5) . . ? B2 B6 B10 107.6(5) . . ? C2 B6 B7 106.1(5) . . ? C1 B6 B7 105.2(5) . . ? B2 B6 B7 59.5(4) . . ? B10 B6 B7 59.7(4) . . ? B2 B7 B10 107.6(5) . . ? B2 B7 B3 60.4(4) . . ? B10 B7 B3 107.5(5) . . ? B2 B7 B6 59.5(4) . . ? B10 B7 B6 59.6(4) . . ? B3 B7 B6 107.4(5) . . ? B2 B7 B8 107.6(5) . . ? B10 B7 B8 59.2(4) . . ? B3 B7 B8 59.8(4) . . ? B6 B7 B8 106.5(5) . . ? B9 B8 B10 61.0(4) . . ? B9 B8 B4 60.5(4) . . ? B10 B8 B4 109.2(5) . . ? B9 B8 B3 108.5(5) . . ? B10 B8 B3 108.0(5) . . ? B4 B8 B3 60.1(4) . . ? B9 B8 B7 108.7(5) . . ? B10 B8 B7 59.7(4) . . ? B4 B8 B7 108.3(5) . . ? B3 B8 B7 59.8(4) . . ? C2 B9 B8 106.3(5) . . ? C2 B9 B4 107.0(5) . . ? B8 B9 B4 60.7(4) . . ? C2 B9 B10 58.8(3) . . ? B8 B9 B10 59.9(4) . . ? B4 B9 B10 108.4(5) . . ? C2 B9 B5 59.4(4) . . ? B8 B9 B5 108.0(5) . . ? B4 B9 B5 60.0(4) . . ? B10 B9 B5 107.3(5) . . ? C2 B10 B8 105.7(5) . . ? C2 B10 B6 59.1(4) . . ? B8 B10 B6 108.7(5) . . ? C2 B10 B7 107.0(5) . . ? B8 B10 B7 61.1(4) . . ? B6 B10 B7 60.7(4) . . ? C2 B10 B9 58.8(4) . . ? B8 B10 B9 59.1(4) . . ? B6 B10 B9 107.4(5) . . ? B7 B10 B9 108.3(5) . . ? # END of CIF