# ic000858p.cif data_global _publ_requested_journal 'Inorganic Chemistry' _publ_contact_letter ; Please consider this new CIF submission as crystallographic information file for compounds [NBu~4~][7-P(O)Ph~2~-8-Ph-7,8-C~2~B~9~H~10~] and [7-PH(^i^Pr)~2~-8-Me-7,8-C~2~B~9~H~10~] included in manuscript IC000858P. ; _publ_contact_author ; Dr. Clara Vi\~nas Institut de Ci\`encia de Materials de Barcelona C.S.C.I. Campus U.A.B. 08193 Bellaterra Spain ; _publ_contact_author_phone '+ 34 3 5801853' _publ_contact_author_fax '+ 34 3 5805729' _publ_contact_author_email 'clara@icmab.es' loop_ _publ_author_name _publ_author_address 'Teixidor, Francesc' ; Institut de Ci\`encia de Materials de Barcelona C.S.C.I. Campus U.A.B. 08193 Bellaterra Spain ; 'Nu\~nez, Rosario' ; Institut de Ci\`encia de Materials de Barcelona C.S.C.I. Campus U.A.B. 08193 Bellaterra Spain ; 'Vi\~nas, Clara' ; Institut de Ci\`encia de Materials de Barcelona C.S.C.I. Campus U.A.B. 08193 Bellaterra Spain ; 'Sillanp\"a\"a, Reijo' ; Department of Chemistry University of Turku FIN-20014 Turku Finland ; 'Kivek\"as, Raikko' ; Department of Chemistry P.O.Box 55 FIN-00014 University of Helsinki Finland ; _publ_section_title ; Contribution of the nido-[7,8-C~2~B~9~H~10~]^-^ anion to the chemical stability, basicity and ^31^P-NMR chemical shift in nido-o-carboranylmonophosphines. ; _publ_section_exptl_prep synthesis _publ_section_exptl_refinement ? data_[NBu~4~][7-P(O)Ph~2~-8-Ph-7,8-C~2~B~9~H~10~] _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'N C16 H36, C20 H25 B9 O P' _chemical_formula_sum 'C36 H61 B9 N O P' _chemical_formula_weight 652.12 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' 'B' 'B' 0.0013 0.0007 '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' '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 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 13.884(7) _cell_length_b 21.485(4) _cell_length_c 13.404(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3998(3) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 7.75 _cell_measurement_theta_max 13.26 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.083 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 0.097 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC5S' _diffrn_measurement_method 'w\--2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 3929 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.2148 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3929 _reflns_number_gt 1526 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1995) ; _computing_cell_refinement ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1995) ; _computing_data_reduction ; Texsan Process (Molecular Structure Corporation, 1989) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0725P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.3(3) _refine_ls_number_reflns 3929 _refine_ls_number_parameters 404 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.2505 _refine_ls_R_factor_gt 0.0752 _refine_ls_wR_factor_ref 0.1987 _refine_ls_wR_factor_gt 0.1478 _refine_ls_goodness_of_fit_ref 0.967 _refine_ls_restrained_S_all 0.970 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P P 0.48344(16) 0.95936(10) 0.03816(16) 0.0454(6) Uani 1 d . . . O O 0.5232(4) 0.9309(2) -0.0539(4) 0.0603(17) Uani 1 d . . . N N 0.6217(6) 0.8563(4) 0.7064(6) 0.067(2) Uani 1 d . . . B1 B 0.6571(10) 0.8629(6) 0.2604(9) 0.077(4) Uiso 1 d . . . H1 H 0.7335 0.8515 0.2726 0.093 Uiso 1 calc R . . B2 B 0.6217(8) 0.9354(5) 0.2089(8) 0.067(3) Uiso 1 d D . . H2 H 0.6742 0.9710 0.1859 0.081 Uiso 1 calc R . . B3 B 0.6045(8) 0.8671(5) 0.1416(9) 0.067(3) Uiso 1 d . . . H3 H 0.6447 0.8586 0.0722 0.080 Uiso 1 calc R . . B4 B 0.5761(8) 0.8059(5) 0.2241(8) 0.061(3) Uiso 1 d D . . H4 H 0.5989 0.7576 0.2105 0.073 Uiso 1 calc R . . B5 B 0.5688(8) 0.8380(5) 0.3418(9) 0.073(4) Uiso 1 d D . . H5 H 0.5870 0.8095 0.4073 0.088 Uiso 1 calc R . . B6 B 0.5953(9) 0.9178(5) 0.3333(9) 0.076(4) Uiso 1 d D . . H6 H 0.6315 0.9437 0.3932 0.091 Uiso 1 calc R . . C7 C 0.5121(6) 0.9191(3) 0.1531(5) 0.0359(19) Uani 1 d . . . C8 C 0.4870(6) 0.8470(4) 0.1619(5) 0.051(2) Uani 1 d . . . B9 B 0.4605(8) 0.8264(5) 0.2733(9) 0.066(3) Uiso 1 d D . . H9 H 0.4116(17) 0.7890(10) 0.297(2) 0.079 Uiso 1 d D . . B10 B 0.4775(9) 0.8942(5) 0.3508(8) 0.072(3) Uiso 1 d D . . H10A H 0.440(2) 0.9046(14) 0.4209(16) 0.086 Uiso 1 d D . . H10B H 0.421(4) 0.908(4) 0.298(4) 0.086 Uiso 1 d D . . B11 B 0.5058(8) 0.9523(5) 0.2604(7) 0.067(3) Uiso 1 d D . . H11 H 0.485(2) 1.0013(7) 0.271(2) 0.080 Uiso 1 d D . . C12 C 0.3546(6) 0.9651(4) 0.0323(7) 0.049(2) Uani 1 d . . . C13 C 0.2950(7) 0.9747(5) 0.1145(9) 0.072(3) Uani 1 d . . . H13 H 0.3229 0.9784 0.1773 0.087 Uiso 1 calc R . . C14 C 0.1957(9) 0.9787(5) 0.1061(11) 0.095(4) Uani 1 d . . . H14 H 0.1575 0.9852 0.1621 0.114 Uiso 1 calc R . . C15 C 0.1542(9) 0.9729(6) 0.0114(13) 0.118(6) Uani 1 d D . . H15 H 0.0878 0.9759 0.0038 0.142 Uiso 1 calc R . . C16 C 0.2123(10) 0.9629(7) -0.0706(10) 0.122(5) Uani 1 d D . . H16 H 0.1850 0.9594 -0.1337 0.147 Uiso 1 calc R . . C17 C 0.3114(8) 0.9580(5) -0.0593(8) 0.078(3) Uani 1 d . . . H17 H 0.3494 0.9497 -0.1149 0.094 Uiso 1 calc R . . C18 C 0.5245(6) 1.0392(4) 0.0477(6) 0.048(2) Uani 1 d . . . C19 C 0.4760(7) 1.0861(4) 0.0986(6) 0.061(3) Uani 1 d . . . H19 H 0.4220 1.0757 0.1362 0.073 Uiso 1 calc R . . C20 C 0.5049(8) 1.1471(5) 0.0954(7) 0.074(3) Uani 1 d . . . H20 H 0.4716 1.1772 0.1314 0.089 Uiso 1 calc R . . C21 C 0.5830(9) 1.1632(5) 0.0391(8) 0.079(3) Uani 1 d . . . H21 H 0.6018 1.2047 0.0358 0.095 Uiso 1 calc R . . C22 C 0.6335(8) 1.1196(5) -0.0122(7) 0.081(4) Uani 1 d . . . H22 H 0.6869 1.1312 -0.0497 0.097 Uiso 1 calc R . . C23 C 0.6052(7) 1.0566(5) -0.0087(7) 0.070(3) Uani 1 d . . . H23 H 0.6400 1.0267 -0.0436 0.084 Uiso 1 calc R . . C24 C 0.4284(8) 0.8160(4) 0.0787(7) 0.058(3) Uani 1 d . . . C25 C 0.4714(9) 0.7826(4) 0.0034(7) 0.082(4) Uani 1 d . . . H25 H 0.5382 0.7800 0.0013 0.098 Uiso 1 calc R . . C26 C 0.4177(14) 0.7526(6) -0.0694(10) 0.129(7) Uani 1 d D . . H26 H 0.4483 0.7311 -0.1206 0.155 Uiso 1 calc R . . C27 C 0.3188(15) 0.7549(8) -0.0649(12) 0.162(11) Uani 1 d D . . H27 H 0.2818 0.7342 -0.1123 0.195 Uiso 1 calc R . . C28 C 0.2743(12) 0.7888(6) 0.0117(13) 0.135(7) Uani 1 d . . . H28 H 0.2075 0.7911 0.0148 0.162 Uiso 1 calc R . . C29 C 0.3295(9) 0.8185(4) 0.0822(8) 0.079(4) Uani 1 d . . . H29 H 0.2995 0.8405 0.1331 0.095 Uiso 1 calc R . . C30 C 0.6801(8) 0.8601(5) 0.8052(6) 0.073(3) Uani 1 d . . . H30A H 0.6566 0.8952 0.8436 0.088 Uiso 1 calc R . . H30B H 0.6678 0.8228 0.8438 0.088 Uiso 1 calc R . . C31 C 0.7852(8) 0.8669(5) 0.7924(7) 0.079(3) Uani 1 d . . . H31A H 0.7984 0.9022 0.7494 0.095 Uiso 1 calc R . . H31B H 0.8108 0.8299 0.7604 0.095 Uiso 1 calc R . . C32 C 0.8338(9) 0.8762(5) 0.8900(7) 0.090(4) Uani 1 d . . . H32A H 0.8132 0.8434 0.9349 0.109 Uiso 1 calc R . . H32B H 0.8122 0.9154 0.9179 0.109 Uiso 1 calc R . . C33 C 0.9430(8) 0.8765(5) 0.8868(8) 0.104(4) Uani 1 d . . . H33A H 0.9647 0.9093 0.8437 0.155 Uiso 1 calc R . . H33B H 0.9657 0.8373 0.8620 0.155 Uiso 1 calc R . . H33C H 0.9678 0.8832 0.9528 0.155 Uiso 1 calc R . . C34 C 0.6325(7) 0.9179(5) 0.6483(6) 0.069(3) Uani 1 d . . . H34A H 0.6996 0.9227 0.6295 0.083 Uiso 1 calc R . . H34B H 0.5953 0.9148 0.5873 0.083 Uiso 1 calc R . . C35 C 0.6012(9) 0.9762(5) 0.7032(9) 0.102(4) Uani 1 d . . . H35A H 0.5363 0.9706 0.7283 0.123 Uiso 1 calc R . . H35B H 0.6434 0.9830 0.7599 0.123 Uiso 1 calc R . . C36 C 0.6041(8) 1.0309(6) 0.6373(9) 0.104(4) Uani 1 d . . . H36A H 0.5673 1.0220 0.5775 0.124 Uiso 1 calc R . . H36B H 0.6703 1.0384 0.6174 0.124 Uiso 1 calc R . . C37 C 0.5650(11) 1.0884(6) 0.6849(11) 0.149(6) Uani 1 d . . . H37A H 0.6070 1.1012 0.7380 0.224 Uiso 1 calc R . . H37B H 0.5021 1.0800 0.7113 0.224 Uiso 1 calc R . . H37C H 0.5608 1.1209 0.6360 0.224 Uiso 1 calc R . . C38 C 0.6588(7) 0.8042(5) 0.6406(7) 0.073(3) Uani 1 d . . . H38A H 0.7268 0.8113 0.6287 0.088 Uiso 1 calc R . . H38B H 0.6263 0.8070 0.5767 0.088 Uiso 1 calc R . . C39 C 0.6468(9) 0.7383(5) 0.6798(8) 0.094(4) Uani 1 d . . . H39A H 0.6799 0.7340 0.7431 0.113 Uiso 1 calc R . . H39B H 0.5790 0.7295 0.6904 0.113 Uiso 1 calc R . . C40 C 0.6879(9) 0.6935(5) 0.6053(9) 0.107(4) Uani 1 d . . . H40A H 0.7562 0.7017 0.5977 0.128 Uiso 1 calc R . . H40B H 0.6574 0.7004 0.5412 0.128 Uiso 1 calc R . . C41 C 0.6742(11) 0.6260(5) 0.6351(10) 0.153(6) Uani 1 d . . . H41A H 0.6075 0.6186 0.6496 0.229 Uiso 1 calc R . . H41B H 0.7122 0.6172 0.6932 0.229 Uiso 1 calc R . . H41C H 0.6942 0.5995 0.5813 0.229 Uiso 1 calc R . . C42 C 0.5158(8) 0.8464(5) 0.7333(7) 0.074(3) Uani 1 d . . . H42A H 0.5102 0.8073 0.7692 0.089 Uiso 1 calc R . . H42B H 0.4962 0.8793 0.7784 0.089 Uiso 1 calc R . . C43 C 0.4462(8) 0.8450(7) 0.6468(9) 0.117(5) Uani 1 d D . . H43A H 0.4805 0.8300 0.5885 0.141 Uiso 0.64(2) d P A 1 H43B H 0.4263 0.8874 0.6328 0.141 Uiso 0.64(2) d P A 1 C44A C 0.3529(13) 0.8041(9) 0.661(2) 0.159(12) Uiso 0.64(2) d PD A 1 H44A H 0.3293 0.7883 0.5980 0.190 Uiso 0.64(2) calc PR A 1 H44B H 0.3646 0.7695 0.7061 0.190 Uiso 0.64(2) calc PR A 1 C45A C 0.2826(15) 0.8513(13) 0.707(2) 0.227(16) Uiso 0.64(2) d PD A 1 H45A H 0.2861 0.8897 0.6705 0.341 Uiso 0.64(2) calc PR A 1 H45B H 0.2995 0.8585 0.7753 0.341 Uiso 0.64(2) calc PR A 1 H45C H 0.2183 0.8351 0.7033 0.341 Uiso 0.64(2) calc PR A 1 H43D H 0.4557 0.8082 0.6060 0.273 Uiso 0.36(2) d P A 2 H43D H 0.4530 0.8818 0.6054 0.273 Uiso 0.36(2) d P A 2 C44B C 0.3477(12) 0.8437(13) 0.6992(15) 0.064(11) Uiso 0.36(2) d PD A 2 H44C H 0.3480 0.8137 0.7532 0.076 Uiso 0.36(2) calc PR A 2 H44D H 0.3325 0.8844 0.7264 0.076 Uiso 0.36(2) calc PR A 2 C45B C 0.2736(16) 0.8253(17) 0.620(2) 0.124(16) Uiso 0.36(2) d PD A 2 H45D H 0.2962 0.8378 0.5556 0.186 Uiso 0.36(2) calc PR A 2 H45E H 0.2135 0.8455 0.6343 0.186 Uiso 0.36(2) calc PR A 2 H45F H 0.2647 0.7810 0.6214 0.186 Uiso 0.36(2) calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P 0.0514(16) 0.0464(13) 0.0385(12) -0.0008(13) -0.0021(13) -0.0003(14) O 0.077(4) 0.064(4) 0.040(3) -0.006(3) 0.011(4) 0.006(3) N 0.073(7) 0.076(6) 0.052(5) 0.008(5) 0.006(5) 0.007(5) C7 0.038(5) 0.037(5) 0.032(4) -0.002(4) 0.002(4) -0.004(4) C8 0.056(6) 0.057(6) 0.039(5) -0.014(4) -0.006(5) -0.005(5) C12 0.037(5) 0.055(6) 0.054(6) 0.017(6) -0.016(6) -0.005(5) C13 0.048(8) 0.065(7) 0.104(9) -0.012(7) -0.006(7) -0.004(6) C14 0.045(9) 0.094(10) 0.146(13) -0.007(9) -0.013(8) -0.004(7) C15 0.053(9) 0.089(10) 0.212(19) 0.042(11) -0.009(11) -0.012(8) C16 0.079(11) 0.144(12) 0.144(14) 0.042(12) -0.049(10) -0.003(11) C17 0.068(8) 0.086(8) 0.081(9) 0.029(7) -0.025(6) -0.012(7) C18 0.044(5) 0.059(5) 0.042(5) -0.009(5) -0.004(5) 0.000(5) C19 0.063(7) 0.051(6) 0.069(6) 0.001(5) -0.004(6) -0.016(6) C20 0.086(9) 0.059(7) 0.078(7) 0.002(6) -0.009(7) 0.004(7) C21 0.096(10) 0.059(7) 0.082(8) 0.002(7) -0.033(8) -0.020(7) C22 0.104(10) 0.067(7) 0.072(8) 0.010(6) -0.009(7) -0.044(7) C23 0.060(7) 0.084(8) 0.067(7) -0.003(6) 0.000(6) -0.012(6) C24 0.079(8) 0.038(6) 0.055(6) 0.015(5) -0.010(6) -0.009(6) C25 0.144(11) 0.055(6) 0.047(6) -0.003(5) 0.011(7) -0.026(8) C26 0.24(2) 0.081(9) 0.065(9) -0.012(7) 0.005(12) -0.097(12) C27 0.30(3) 0.097(14) 0.093(14) 0.052(10) -0.084(18) -0.113(18) C28 0.140(14) 0.082(11) 0.183(17) 0.053(11) -0.102(15) -0.074(10) C29 0.065(8) 0.058(7) 0.114(10) 0.028(7) -0.028(7) -0.026(6) C30 0.108(9) 0.071(7) 0.041(6) 0.011(5) 0.000(6) 0.020(7) C31 0.100(10) 0.085(8) 0.053(7) -0.002(6) 0.000(7) -0.007(7) C32 0.132(12) 0.083(8) 0.056(7) 0.007(6) -0.028(8) -0.028(8) C33 0.093(11) 0.109(10) 0.108(10) 0.030(8) -0.030(8) -0.039(8) C34 0.068(7) 0.091(8) 0.049(6) 0.030(6) -0.001(6) -0.002(6) C35 0.129(11) 0.072(8) 0.106(9) 0.026(7) 0.030(9) -0.001(8) C36 0.082(8) 0.092(9) 0.137(11) 0.040(9) -0.026(8) -0.009(8) C37 0.184(16) 0.069(9) 0.194(15) 0.007(10) -0.048(13) -0.005(10) C38 0.069(7) 0.107(9) 0.043(6) -0.001(6) 0.003(6) -0.007(7) C39 0.124(11) 0.072(8) 0.086(8) -0.012(7) -0.005(8) 0.006(8) C40 0.122(11) 0.093(9) 0.106(9) -0.022(9) -0.037(9) 0.013(9) C41 0.225(18) 0.080(10) 0.153(13) -0.008(10) -0.067(13) 0.012(11) C42 0.079(8) 0.090(8) 0.054(6) 0.009(5) 0.013(7) -0.005(7) C43 0.064(8) 0.197(15) 0.090(8) 0.038(10) -0.021(7) -0.029(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P O 1.484(5) . y P C12 1.795(8) . y P C7 1.811(7) . y P C18 1.812(9) . y N C38 1.514(11) . ? N C42 1.529(12) . ? N C34 1.544(11) . ? N C30 1.555(11) . ? B1 B5 1.725(16) . ? B1 B4 1.732(16) . ? B1 B3 1.754(16) . ? B1 B6 1.755(16) . ? B1 B2 1.774(17) . ? B1 H1 1.1000 . ? B2 C7 1.732(13) . ? B2 B3 1.739(15) . ? B2 B6 1.750(16) . ? B2 B11 1.789(15) . ? B2 H2 1.1000 . ? B3 C7 1.709(14) . ? B3 C8 1.710(14) . ? B3 B4 1.762(15) . ? B3 H3 1.1000 . ? B4 B5 1.725(15) . ? B4 C8 1.733(14) . ? B4 B9 1.790(15) . ? B4 H4 1.1000 . ? B5 B10 1.754(15) . ? B5 B6 1.755(16) . ? B5 B9 1.779(16) . ? B5 H5 1.1000 . ? B6 B10 1.727(17) . ? B6 B11 1.746(16) . ? B6 H6 1.1000 . ? C7 C8 1.592(11) . y C7 B11 1.608(12) . y C8 C24 1.533(11) . y C8 B9 1.600(13) . y B9 B10 1.804(15) . y B9 H9 1.1000(11) . ? B10 B11 1.784(14) . y B10 H10A 1.0999(11) . ? B10 H10B 1.1000(11) . ? B11 H10B 1.60(7) . ? B11 H11 1.0999(11) . ? C12 C17 1.375(12) . ? C12 C13 1.393(12) . ? C13 C14 1.386(13) . ? C13 H13 0.9300 . ? C14 C15 1.399(15) . ? C14 H14 0.9300 . ? C15 C16 1.381(9) . ? C15 H15 0.9300 . ? C16 C17 1.388(14) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.391(11) . ? C18 C23 1.403(11) . ? C19 C20 1.371(12) . ? C19 H19 0.9300 . ? C20 C21 1.366(13) . ? C20 H20 0.9300 . ? C21 C22 1.359(13) . ? C21 H21 0.9300 . ? C22 C23 1.409(12) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C29 1.375(13) . ? C24 C25 1.375(12) . ? C25 C26 1.387(15) . ? C25 H25 0.9300 . ? C26 C27 1.376(10) . ? C26 H26 0.9300 . ? C27 C28 1.402(19) . ? C27 H27 0.9300 . ? C28 C29 1.373(14) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C31 1.477(13) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.485(12) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.517(14) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 C35 1.515(13) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.472(13) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.492(15) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 C39 1.519(12) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.501(13) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 C41 1.516(14) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 C43 1.509(13) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44B 1.538(10) . ? C43 C44A 1.577(10) . ? C43 H43A 0.970(13) . ? C43 H43B 0.970(14) . ? C43 H43D 0.970(15) . ? C43 H43D 0.970(13) . ? C44A C45A 1.533(10) . ? C44A H44A 0.9700 . ? C44A H44B 0.9700 . ? C45A H45A 0.9600 . ? C45A H45B 0.9600 . ? C45A H45C 0.9600 . ? C44B C45B 1.527(10) . ? C44B H44C 0.9700 . ? C44B H44D 0.9700 . ? C45B H45D 0.9600 . ? C45B H45E 0.9600 . ? C45B H45F 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 O P C12 111.3(4) . . y O P C7 115.4(3) . . y C12 P C7 106.8(4) . . y O P C18 109.4(4) . . y C12 P C18 104.6(4) . . y C7 P C18 108.8(4) . . y C38 N C42 111.2(8) . . ? C38 N C34 107.9(7) . . ? C42 N C34 109.4(7) . . ? C38 N C30 111.0(7) . . ? C42 N C30 108.0(7) . . ? C34 N C30 109.5(7) . . ? B5 B1 B4 59.8(7) . . ? B5 B1 B3 107.1(9) . . ? B4 B1 B3 60.7(7) . . ? B5 B1 B6 60.6(7) . . ? B4 B1 B6 108.3(9) . . ? B3 B1 B6 105.5(9) . . ? B5 B1 B2 108.8(9) . . ? B4 B1 B2 109.4(9) . . ? B3 B1 B2 59.1(6) . . ? B6 B1 B2 59.4(7) . . ? B5 B1 H1 121.5 . . ? B4 B1 H1 120.7 . . ? B3 B1 H1 123.1 . . ? B6 B1 H1 122.5 . . ? B2 B1 H1 121.3 . . ? C7 B2 B3 59.0(6) . . ? C7 B2 B6 100.6(8) . . ? B3 B2 B6 106.4(9) . . ? C7 B2 B1 103.5(8) . . ? B3 B2 B1 59.9(6) . . ? B6 B2 B1 59.7(6) . . ? C7 B2 B11 54.3(5) . . ? B3 B2 B11 104.4(8) . . ? B6 B2 B11 59.1(6) . . ? B1 B2 B11 106.1(8) . . ? C7 B2 H2 127.1 . . ? B3 B2 H2 122.2 . . ? B6 B2 H2 123.8 . . ? B1 B2 H2 122.4 . . ? B11 B2 H2 124.3 . . ? C7 B3 C8 55.5(5) . . ? C7 B3 B2 60.3(6) . . ? C8 B3 B2 105.2(8) . . ? C7 B3 B1 105.3(8) . . ? C8 B3 B1 103.9(8) . . ? B2 B3 B1 61.0(7) . . ? C7 B3 B4 105.2(8) . . ? C8 B3 B4 59.9(6) . . ? B2 B3 B4 109.6(8) . . ? B1 B3 B4 59.0(6) . . ? C7 B3 H3 124.3 . . ? C8 B3 H3 125.2 . . ? B2 B3 H3 120.5 . . ? B1 B3 H3 123.3 . . ? B4 B3 H3 121.4 . . ? B5 B4 B1 59.9(6) . . ? B5 B4 C8 101.2(7) . . ? B1 B4 C8 103.8(8) . . ? B5 B4 B3 106.8(8) . . ? B1 B4 B3 60.2(6) . . ? C8 B4 B3 58.6(6) . . ? B5 B4 B9 60.8(6) . . ? B1 B4 B9 107.7(8) . . ? C8 B4 B9 54.0(6) . . ? B3 B4 B9 104.4(8) . . ? B5 B4 H4 123.0 . . ? B1 B4 H4 121.8 . . ? C8 B4 H4 127.3 . . ? B3 B4 H4 122.4 . . ? B9 B4 H4 123.4 . . ? B4 B5 B1 60.3(6) . . ? B4 B5 B10 112.4(9) . . ? B1 B5 B10 110.1(9) . . ? B4 B5 B6 108.6(9) . . ? B1 B5 B6 60.6(7) . . ? B10 B5 B6 59.0(7) . . ? B4 B5 B9 61.4(6) . . ? B1 B5 B9 108.5(8) . . ? B10 B5 B9 61.4(7) . . ? B6 B5 B9 106.3(8) . . ? B4 B5 H5 119.6 . . ? B1 B5 H5 121.0 . . ? B10 B5 H5 119.5 . . ? B6 B5 H5 123.1 . . ? B9 B5 H5 121.8 . . ? B10 B6 B11 61.8(7) . . ? B10 B6 B2 113.1(9) . . ? B11 B6 B2 61.5(6) . . ? B10 B6 B1 110.0(9) . . ? B11 B6 B1 108.8(9) . . ? B2 B6 B1 60.8(7) . . ? B10 B6 B5 60.5(6) . . ? B11 B6 B5 107.6(9) . . ? B2 B6 B5 108.5(9) . . ? B1 B6 B5 58.9(7) . . ? B10 B6 H6 118.8 . . ? B11 B6 H6 121.2 . . ? B2 B6 H6 119.4 . . ? B1 B6 H6 121.6 . . ? B5 B6 H6 122.9 . . ? C8 C7 B11 110.7(6) . . ? C8 C7 B3 62.3(6) . . ? B11 C7 B3 114.3(7) . . ? C8 C7 B2 110.9(7) . . ? B11 C7 B2 64.6(6) . . ? B3 C7 B2 60.7(6) . . ? C8 C7 P 118.7(5) . . y B11 C7 P 122.5(6) . . y B3 C7 P 113.7(6) . . y B2 C7 P 117.6(6) . . y C24 C8 C7 118.9(6) . . y C24 C8 B9 116.0(8) . . y C7 C8 B9 112.8(7) . . ? C24 C8 B3 120.0(8) . . y C7 C8 B3 62.2(6) . . ? B9 C8 B3 115.9(8) . . ? C24 C8 B4 120.5(7) . . y C7 C8 B4 112.0(7) . . ? B9 C8 B4 64.8(6) . . ? B3 C8 B4 61.6(6) . . ? C8 B9 B5 104.4(8) . . ? C8 B9 B4 61.2(6) . . ? B5 B9 B4 57.8(6) . . ? C8 B9 B10 106.5(7) . . ? B5 B9 B10 58.6(6) . . ? B4 B9 B10 107.1(8) . . ? C8 B9 H9 128(2) . . ? B5 B9 H9 118.3(19) . . ? B4 B9 H9 118.7(17) . . ? B10 B9 H9 120.2(17) . . ? B6 B10 B5 60.5(7) . . ? B6 B10 B11 59.6(6) . . ? B5 B10 B11 106.0(8) . . ? B6 B10 B9 106.4(8) . . ? B5 B10 B9 60.0(6) . . ? B11 B10 B9 101.7(7) . . ? B6 B10 H10A 121(2) . . ? B5 B10 H10A 123.1(17) . . ? B11 B10 H10A 122.9(17) . . ? B9 B10 H10A 126(2) . . ? B6 B10 H10B 121(4) . . ? B5 B10 H10B 131(4) . . ? B11 B10 H10B 62(4) . . ? B9 B10 H10B 76(4) . . ? H10A B10 H10B 99(5) . . ? C7 B11 B6 105.9(8) . . ? C7 B11 B10 108.0(7) . . ? B6 B11 B10 58.6(7) . . ? C7 B11 B2 61.0(6) . . ? B6 B11 B2 59.3(6) . . ? B10 B11 B2 108.6(8) . . ? C7 B11 H10B 93(3) . . ? B6 B11 H10B 95.5(10) . . ? B10 B11 H10B 37.5(5) . . ? B2 B11 H10B 132(3) . . ? C7 B11 H11 124(2) . . ? B6 B11 H11 121(2) . . ? B10 B11 H11 121.6(16) . . ? B2 B11 H11 118.6(17) . . ? H10B B11 H11 110(3) . . ? C17 C12 C13 117.7(8) . . ? C17 C12 P 117.8(8) . . ? C13 C12 P 124.6(7) . . ? C14 C13 C12 122.4(11) . . ? C14 C13 H13 118.8 . . ? C12 C13 H13 118.8 . . ? C13 C14 C15 118.5(13) . . ? C13 C14 H14 120.7 . . ? C15 C14 H14 120.7 . . ? C16 C15 C14 119.7(12) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 120.3(12) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C12 C17 C16 121.4(11) . . ? C12 C17 H17 119.3 . . ? C16 C17 H17 119.3 . . ? C19 C18 C23 117.2(9) . . ? C19 C18 P 124.6(7) . . ? C23 C18 P 117.8(7) . . ? C20 C19 C18 122.3(10) . . ? C20 C19 H19 118.8 . . ? C18 C19 H19 118.8 . . ? C21 C20 C19 119.5(10) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C22 C21 C20 120.9(10) . . ? C22 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? C21 C22 C23 120.1(10) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C18 C23 C22 119.8(10) . . ? C18 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C29 C24 C25 118.6(11) . . ? C29 C24 C8 119.3(10) . . ? C25 C24 C8 122.0(10) . . ? C24 C25 C26 121.7(12) . . ? C24 C25 H25 119.1 . . ? C26 C25 H25 119.1 . . ? C27 C26 C25 119.3(16) . . ? C27 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? C26 C27 C28 119.4(18) . . ? C26 C27 H27 120.3 . . ? C28 C27 H27 120.3 . . ? C29 C28 C27 119.9(17) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C28 C29 C24 121.1(13) . . ? C28 C29 H29 119.4 . . ? C24 C29 H29 119.4 . . ? C31 C30 N 114.9(8) . . ? C31 C30 H30A 108.5 . . ? N C30 H30A 108.5 . . ? C31 C30 H30B 108.5 . . ? N C30 H30B 108.5 . . ? H30A C30 H30B 107.5 . . ? C30 C31 C32 111.1(9) . . ? C30 C31 H31A 109.4 . . ? C32 C31 H31A 109.4 . . ? C30 C31 H31B 109.4 . . ? C32 C31 H31B 109.4 . . ? H31A C31 H31B 108.0 . . ? C31 C32 C33 115.5(10) . . ? C31 C32 H32A 108.4 . . ? C33 C32 H32A 108.4 . . ? C31 C32 H32B 108.4 . . ? C33 C32 H32B 108.4 . . ? H32A C32 H32B 107.5 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 N 115.8(7) . . ? C35 C34 H34A 108.3 . . ? N C34 H34A 108.3 . . ? C35 C34 H34B 108.3 . . ? N C34 H34B 108.3 . . ? H34A C34 H34B 107.4 . . ? C36 C35 C34 111.1(10) . . ? C36 C35 H35A 109.4 . . ? C34 C35 H35A 109.4 . . ? C36 C35 H35B 109.4 . . ? C34 C35 H35B 109.4 . . ? H35A C35 H35B 108.0 . . ? C35 C36 C37 113.3(11) . . ? C35 C36 H36A 108.9 . . ? C37 C36 H36A 108.9 . . ? C35 C36 H36B 108.9 . . ? C37 C36 H36B 108.9 . . ? H36A C36 H36B 107.7 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N C38 C39 116.7(8) . . ? N C38 H38A 108.1 . . ? C39 C38 H38A 108.1 . . ? N C38 H38B 108.1 . . ? C39 C38 H38B 108.1 . . ? H38A C38 H38B 107.3 . . ? C40 C39 C38 109.1(9) . . ? C40 C39 H39A 109.9 . . ? C38 C39 H39A 109.9 . . ? C40 C39 H39B 109.9 . . ? C38 C39 H39B 109.9 . . ? H39A C39 H39B 108.3 . . ? C39 C40 C41 113.1(11) . . ? C39 C40 H40A 109.0 . . ? C41 C40 H40A 109.0 . . ? C39 C40 H40B 109.0 . . ? C41 C40 H40B 109.0 . . ? H40A C40 H40B 107.8 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C43 C42 N 115.9(8) . . ? C43 C42 H42A 108.3 . . ? N C42 H42A 108.3 . . ? C43 C42 H42B 108.3 . . ? N C42 H42B 108.3 . . ? H42A C42 H42B 107.4 . . ? C42 C43 C44B 102.6(11) . . ? C42 C43 C44A 116.2(14) . . ? C44B C43 C44A 37.2(12) . . ? C42 C43 H43A 108.1(9) . . ? C44B C43 H43A 142.9(13) . . ? C44A C43 H43A 108.4(14) . . ? C42 C43 H43B 108.2(12) . . ? C44B C43 H43B 81.4(13) . . ? C44A C43 H43B 108.2(11) . . ? H43A C43 H43B 107.3(11) . . ? C42 C43 H43D 111.2(11) . . ? C44B C43 H43D 111.3(13) . . ? C44A C43 H43D 74.2(11) . . ? H43A C43 H43D 37.6(5) . . ? H43B C43 H43D 134.0(12) . . ? C42 C43 H43D 111.2(11) . . ? C44B C43 H43D 111.2(15) . . ? C44A C43 H43D 127.1(13) . . ? H43A C43 H43D 76.3(8) . . ? H43B C43 H43D 32.1(4) . . ? H43D C43 H43D 109.1(11) . . ? C45A C44A C43 101.8(12) . . ? C45A C44A H44A 111.4 . . ? C43 C44A H44A 111.4 . . ? C45A C44A H44B 111.4 . . ? C43 C44A H44B 111.4 . . ? H44A C44A H44B 109.3 . . ? C45B C44B C43 106.7(13) . . ? C45B C44B H44C 110.4 . . ? C43 C44B H44C 110.4 . . ? C45B C44B H44D 110.4 . . ? C43 C44B H44D 110.4 . . ? H44C C44B H44D 108.6 . . ? C44B C45B H45D 109.5 . . ? C44B C45B H45E 109.5 . . ? H45D C45B H45E 109.5 . . ? C44B C45B H45F 109.5 . . ? H45D C45B H45F 109.5 . . ? H45E C45B H45F 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 P C7 C8 C24 -7.6(11) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.273 _refine_diff_density_min -0.216 _refine_diff_density_rms 0.046 #===END data_[7-PH(^i^Pr)~2~-8-Me-C~2~B~9~H~10~] _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C9 H28 B9 P' _chemical_formula_sum 'C9 H28 B9 P' _chemical_formula_weight 264.57 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' 'B' 'B' 0.0013 0.0007 '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' 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 11.1860(9) _cell_length_b 9.3633(10) _cell_length_c 16.1673(11) _cell_angle_alpha 90.00 _cell_angle_beta 93.090(7) _cell_angle_gamma 90.00 _cell_volume 1690.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 17.2 _cell_measurement_theta_max 20.6 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.039 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 568 _exptl_absorpt_coefficient_mu 0.140 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC5S' _diffrn_measurement_method \w/2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1 _diffrn_reflns_number 3121 _diffrn_reflns_av_R_equivalents 0.0170 _diffrn_reflns_av_sigmaI/netI 0.0314 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2964 _reflns_number_gt 2323 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; MSC/AFC5S Diffractometer Control Software (Molecular Structure Corporation, 1995) ; _computing_cell_refinement ; MSC/AFC5S Diffractometer Control Software (Molecular Structure Corporation, 1995) ; _computing_data_reduction 'teXsan for Windows (MSC, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0557P)^2^+0.3806P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2964 _refine_ls_number_parameters 221 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0596 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.1085 _refine_ls_wR_factor_gt 0.0990 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P P 0.21718(4) 0.31397(5) 0.79836(3) 0.03197(16) Uani 1 d . . . B1 B 0.1694(2) 0.7326(2) 0.68031(15) 0.0424(5) Uani 1 d . . . B2 B 0.24605(19) 0.6323(2) 0.75788(14) 0.0378(5) Uani 1 d . . . B3 B 0.10332(18) 0.5750(2) 0.71636(13) 0.0358(5) Uani 1 d . . . B4 B 0.0949(2) 0.6155(2) 0.61067(14) 0.0415(5) Uani 1 d . . . B5 B 0.2314(2) 0.6885(3) 0.58251(16) 0.0473(6) Uani 1 d . . . B6 B 0.3268(2) 0.6987(2) 0.67652(16) 0.0452(6) Uani 1 d . . . C7 C 0.22229(15) 0.45663(18) 0.72513(10) 0.0308(4) Uani 1 d . . . C8 C 0.13525(16) 0.44753(19) 0.64358(10) 0.0335(4) Uani 1 d . . . B9 B 0.2034(2) 0.5047(3) 0.56430(14) 0.0433(5) Uani 1 d . . . B10 B 0.3534(2) 0.5689(3) 0.60022(16) 0.0484(6) Uani 1 d . . . B11 B 0.35421(19) 0.5227(2) 0.70992(14) 0.0394(5) Uani 1 d . . . C12 C 0.32301(16) 0.17434(19) 0.77490(11) 0.0381(4) Uani 1 d . . . H12 H 0.4037 0.2109 0.7886 0.046 Uiso 1 calc R . . C13 C 0.3156(2) 0.1358(2) 0.68308(13) 0.0575(6) Uani 1 d . . . H13A H 0.3253 0.2206 0.6507 0.086 Uiso 1 calc R . . H13B H 0.2390 0.0937 0.6687 0.086 Uiso 1 calc R . . H13C H 0.3778 0.0690 0.6720 0.086 Uiso 1 calc R . . C14 C 0.3044(2) 0.0429(2) 0.82899(14) 0.0529(6) Uani 1 d . . . H14A H 0.3203 0.0675 0.8862 0.079 Uiso 1 calc R . . H14B H 0.3580 -0.0316 0.8139 0.079 Uiso 1 calc R . . H14C H 0.2232 0.0104 0.8208 0.079 Uiso 1 calc R . . C15 C 0.23452(19) 0.3584(2) 0.90797(11) 0.0454(5) Uani 1 d . . . H15 H 0.2270 0.2673 0.9371 0.054 Uiso 1 calc R . . C16 C 0.1312(2) 0.4504(2) 0.93608(13) 0.0574(6) Uani 1 d . . . H16A H 0.0564 0.4077 0.9177 0.086 Uiso 1 calc R . . H16B H 0.1368 0.5443 0.9127 0.086 Uiso 1 calc R . . H16C H 0.1357 0.4570 0.9954 0.086 Uiso 1 calc R . . C17 C 0.3587(2) 0.4146(3) 0.93531(13) 0.0649(7) Uani 1 d . . . H17A H 0.4181 0.3453 0.9224 0.097 Uiso 1 calc R . . H17B H 0.3624 0.4315 0.9940 0.097 Uiso 1 calc R . . H17C H 0.3735 0.5022 0.9068 0.097 Uiso 1 calc R . . C18 C 0.04174(17) 0.3295(2) 0.63219(12) 0.0441(5) Uani 1 d . . . H18A H -0.0070 0.3467 0.5825 0.066 Uiso 1 calc R . . H18B H -0.0078 0.3285 0.6788 0.066 Uiso 1 calc R . . H18C H 0.0812 0.2389 0.6281 0.066 Uiso 1 calc R . . H H 0.1112(16) 0.258(2) 0.7888(11) 0.040(5) Uiso 1 d . . . H1 H 0.1311(17) 0.840(2) 0.6926(12) 0.050(6) Uiso 1 d . . . H2 H 0.2520(17) 0.660(2) 0.8238(12) 0.048(5) Uiso 1 d . . . H3 H 0.0254(16) 0.5600(19) 0.7554(11) 0.040(5) Uiso 1 d . . . H4 H 0.0051(17) 0.634(2) 0.5785(11) 0.043(5) Uiso 1 d . . . H5 H 0.237(2) 0.768(3) 0.5340(14) 0.069(7) Uiso 1 d . . . H6 H 0.3907(19) 0.784(2) 0.6864(13) 0.059(6) Uiso 1 d . . . H9 H 0.1826(18) 0.459(2) 0.5026(13) 0.053(6) Uiso 1 d . . . H10B H 0.325(2) 0.455(3) 0.6023(15) 0.076(7) Uiso 1 d . . . H10A H 0.4321(18) 0.580(2) 0.5635(12) 0.054(6) Uiso 1 d . . . H11 H 0.4343(16) 0.486(2) 0.7502(11) 0.041(5) Uiso 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 P 0.0323(3) 0.0311(3) 0.0327(3) -0.0007(2) 0.00363(18) -0.0007(2) B1 0.0402(12) 0.0294(11) 0.0576(14) 0.0023(10) 0.0025(10) 0.0040(9) B2 0.0370(11) 0.0302(11) 0.0458(13) -0.0037(9) -0.0008(9) -0.0028(9) B3 0.0317(11) 0.0338(11) 0.0420(11) -0.0041(9) 0.0037(9) 0.0028(9) B4 0.0422(12) 0.0375(12) 0.0442(12) 0.0056(10) -0.0024(10) 0.0065(10) B5 0.0474(13) 0.0425(13) 0.0525(14) 0.0132(11) 0.0066(11) 0.0028(11) B6 0.0380(12) 0.0351(12) 0.0628(15) 0.0039(11) 0.0054(11) -0.0051(10) C7 0.0302(9) 0.0284(9) 0.0335(9) -0.0014(7) 0.0004(7) -0.0001(7) C8 0.0335(9) 0.0330(10) 0.0337(9) -0.0019(7) -0.0010(7) 0.0020(7) B9 0.0471(13) 0.0461(13) 0.0371(12) 0.0013(10) 0.0056(10) 0.0040(11) B10 0.0420(13) 0.0471(14) 0.0578(14) 0.0080(12) 0.0176(11) 0.0014(11) B11 0.0303(11) 0.0359(12) 0.0522(13) 0.0034(10) 0.0043(10) -0.0012(9) C12 0.0369(10) 0.0336(10) 0.0441(10) 0.0018(8) 0.0053(8) 0.0048(8) C13 0.0775(16) 0.0476(13) 0.0480(12) -0.0023(10) 0.0101(11) 0.0209(11) C14 0.0617(14) 0.0381(11) 0.0599(13) 0.0095(10) 0.0123(11) 0.0088(10) C15 0.0592(13) 0.0455(11) 0.0317(10) -0.0002(8) 0.0042(9) 0.0015(10) C16 0.0696(15) 0.0569(14) 0.0475(12) -0.0143(10) 0.0198(11) -0.0018(11) C17 0.0650(15) 0.0825(18) 0.0456(12) -0.0097(12) -0.0113(11) 0.0022(13) C18 0.0434(11) 0.0424(11) 0.0457(11) -0.0043(9) -0.0059(9) -0.0055(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P C7 1.7880(17) . y P C12 1.8174(18) . y P C15 1.8203(19) . y P H 1.299(18) . y B1 B4 1.750(3) . ? B1 B2 1.753(3) . ? B1 B3 1.763(3) . ? B1 B6 1.794(3) . ? B1 B5 1.808(3) . ? B1 H1 1.11(2) . ? B2 C7 1.744(3) . ? B2 B6 1.750(3) . ? B2 B3 1.781(3) . ? B2 B11 1.794(3) . ? B2 H2 1.09(2) . ? B3 C8 1.727(3) . ? B3 C7 1.732(3) . ? B3 B4 1.748(3) . ? B3 H3 1.112(18) . ? B4 C8 1.713(3) . ? B4 B5 1.754(3) . ? B4 B9 1.792(3) . ? B4 H4 1.119(19) . ? B5 B9 1.771(3) . ? B5 B10 1.776(3) . ? B5 B6 1.812(4) . ? B5 H5 1.09(2) . ? B6 B11 1.756(3) . ? B6 B10 1.768(4) . ? B6 H6 1.08(2) . ? C7 C8 1.598(2) . y C7 B11 1.631(3) . y C8 C18 1.526(2) . y C8 B9 1.617(3) . y B9 B10 1.846(3) . y B9 H9 1.10(2) . ? B9 H10B 1.53(2) . ? B10 B11 1.825(3) . y B10 H10B 1.11(3) . ? B10 H10A 1.09(2) . ? B11 H11 1.131(19) . ? C12 C13 1.525(3) . ? C12 C14 1.530(3) . ? C12 H12 0.9800 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C17 1.528(3) . ? C15 C16 1.530(3) . ? C15 H15 0.9800 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 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 C7 P C12 110.78(8) . . y C7 P C15 117.94(9) . . y C12 P C15 109.33(9) . . y C7 P H 106.6(8) . . y C12 P H 106.5(8) . . y C15 P H 104.9(8) . . y B4 B1 B2 108.80(15) . . ? B4 B1 B3 59.67(12) . . ? B2 B1 B3 60.86(12) . . ? B4 B1 B6 107.54(16) . . ? B2 B1 B6 59.09(13) . . ? B3 B1 B6 107.03(15) . . ? B4 B1 B5 59.06(13) . . ? B2 B1 B5 107.89(16) . . ? B3 B1 B5 106.56(16) . . ? B6 B1 B5 60.41(14) . . ? B4 B1 H1 120.4(10) . . ? B2 B1 H1 122.2(10) . . ? B3 B1 H1 121.5(10) . . ? B6 B1 H1 123.6(10) . . ? B5 B1 H1 122.1(10) . . ? C7 B2 B6 100.56(15) . . ? C7 B2 B1 103.13(14) . . ? B6 B2 B1 61.60(13) . . ? C7 B2 B3 58.84(11) . . ? B6 B2 B3 108.20(16) . . ? B1 B2 B3 59.84(12) . . ? C7 B2 B11 54.87(11) . . ? B6 B2 B11 59.38(12) . . ? B1 B2 B11 108.20(16) . . ? B3 B2 B11 106.05(15) . . ? C7 B2 H2 121.0(10) . . ? B6 B2 H2 130.0(10) . . ? B1 B2 H2 125.0(10) . . ? B3 B2 H2 116.3(10) . . ? B11 B2 H2 123.2(10) . . ? C8 B3 C7 55.05(10) . . ? C8 B3 B4 59.08(11) . . ? C7 B3 B4 102.68(14) . . ? C8 B3 B1 104.33(15) . . ? C7 B3 B1 103.23(14) . . ? B4 B3 B1 59.78(13) . . ? C8 B3 B2 104.53(14) . . ? C7 B3 B2 59.52(11) . . ? B4 B3 B2 107.64(16) . . ? B1 B3 B2 59.30(12) . . ? C8 B3 H3 119.8(9) . . ? C7 B3 H3 119.7(9) . . ? B4 B3 H3 125.4(9) . . ? B1 B3 H3 130.4(9) . . ? B2 B3 H3 122.5(9) . . ? C8 B4 B3 59.85(11) . . ? C8 B4 B1 105.49(15) . . ? B3 B4 B1 60.55(13) . . ? C8 B4 B5 102.68(15) . . ? B3 B4 B5 109.66(17) . . ? B1 B4 B5 62.13(14) . . ? C8 B4 B9 54.90(11) . . ? B3 B4 B9 106.33(15) . . ? B1 B4 B9 108.81(16) . . ? B5 B4 B9 59.90(13) . . ? C8 B4 H4 120.0(10) . . ? B3 B4 H4 119.2(9) . . ? B1 B4 H4 125.9(10) . . ? B5 B4 H4 126.2(10) . . ? B9 B4 H4 120.4(10) . . ? B4 B5 B9 61.10(13) . . ? B4 B5 B10 112.62(17) . . ? B9 B5 B10 62.73(14) . . ? B4 B5 B1 58.81(13) . . ? B9 B5 B1 107.15(16) . . ? B10 B5 B1 109.30(17) . . ? B4 B5 B6 106.53(16) . . ? B9 B5 B6 106.36(16) . . ? B10 B5 B6 59.03(14) . . ? B1 B5 B6 59.40(13) . . ? B4 B5 H5 122.6(12) . . ? B9 B5 H5 124.4(12) . . ? B10 B5 H5 118.5(12) . . ? B1 B5 H5 120.8(12) . . ? B6 B5 H5 120.9(12) . . ? B2 B6 B11 61.57(12) . . ? B2 B6 B10 113.16(16) . . ? B11 B6 B10 62.38(14) . . ? B2 B6 B1 59.30(13) . . ? B11 B6 B1 108.11(15) . . ? B10 B6 B1 110.33(17) . . ? B2 B6 B5 107.88(16) . . ? B11 B6 B5 107.06(17) . . ? B10 B6 B5 59.46(14) . . ? B1 B6 B5 60.19(13) . . ? B2 B6 H6 121.1(11) . . ? B11 B6 H6 123.1(12) . . ? B10 B6 H6 118.6(11) . . ? B1 B6 H6 120.5(11) . . ? B5 B6 H6 121.3(11) . . ? C8 C7 B11 114.31(14) . . ? C8 C7 B3 62.32(11) . . ? B11 C7 B3 116.25(14) . . ? C8 C7 B2 112.14(13) . . ? B11 C7 B2 64.12(12) . . ? B3 C7 B2 61.64(11) . . ? C8 C7 P 117.81(12) . . y B11 C7 P 116.41(12) . . y B3 C7 P 118.72(12) . . y B2 C7 P 120.89(12) . . y C18 C8 C7 121.41(15) . . y C18 C8 B9 119.56(15) . . y C7 C8 B9 110.11(15) . . ? C18 C8 B4 117.40(15) . . y C7 C8 B4 110.23(14) . . ? B9 C8 B4 65.02(13) . . ? C18 C8 B3 114.67(15) . . y C7 C8 B3 62.64(11) . . ? B9 C8 B3 115.78(15) . . ? B4 C8 B3 61.07(12) . . ? C8 B9 B5 106.04(16) . . ? C8 B9 B4 60.08(12) . . ? B5 B9 B4 59.00(13) . . ? C8 B9 B10 108.52(16) . . ? B5 B9 B10 58.77(13) . . ? B4 B9 B10 107.70(16) . . ? C8 B9 H9 120.3(11) . . ? B5 B9 H9 123.8(11) . . ? B4 B9 H9 119.3(11) . . ? B10 B9 H9 123.9(11) . . ? C8 B9 H10B 91.6(9) . . ? B5 B9 H10B 94.7(10) . . ? B4 B9 H10B 127.9(9) . . ? B10 B9 H10B 37.0(9) . . ? H9 B9 H10B 112.7(14) . . ? B6 B10 B5 61.51(14) . . ? B6 B10 B11 58.48(13) . . ? B5 B10 B11 105.65(16) . . ? B6 B10 B9 105.05(16) . . ? B5 B10 B9 58.50(13) . . ? B11 B10 B9 100.69(15) . . ? B6 B10 H10B 125.3(12) . . ? B5 B10 H10B 112.9(13) . . ? B11 B10 H10B 74.4(12) . . ? B9 B10 H10B 56.0(13) . . ? B6 B10 H10A 119.1(11) . . ? B5 B10 H10A 119.3(10) . . ? B11 B10 H10A 126.0(10) . . ? B9 B10 H10A 127.2(10) . . ? H10B B10 H10A 110.1(16) . . ? C7 B11 B6 104.96(15) . . ? C7 B11 B2 61.00(11) . . ? B6 B11 B2 59.04(13) . . ? C7 B11 B10 106.20(16) . . ? B6 B11 B10 59.14(13) . . ? B2 B11 B10 108.43(15) . . ? C7 B11 H11 119.6(9) . . ? B6 B11 H11 125.4(10) . . ? B2 B11 H11 117.1(9) . . ? B10 B11 H11 126.4(9) . . ? C13 C12 C14 111.35(17) . . ? C13 C12 P 111.78(13) . . ? C14 C12 P 110.42(13) . . ? C13 C12 H12 107.7 . . ? C14 C12 H12 107.7 . . ? P C12 H12 107.7 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C17 C15 C16 114.15(18) . . ? C17 C15 P 114.06(14) . . ? C16 C15 P 112.04(14) . . ? C17 C15 H15 105.2 . . ? C16 C15 H15 105.2 . . ? P C15 H15 105.2 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C8 C18 H18A 109.5 . . ? C8 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C8 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 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 P C7 C8 C18 6.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.932 _refine_diff_density_max 0.264 _refine_diff_density_min -0.168 _refine_diff_density_rms 0.036 #===END