#------------------------------------------------------------------------------ #$Date: 2012-02-24 17:13:23 +0000 (Fri, 24 Feb 2012) $ #$Revision: 34330 $ #$URL: svn://www.crystallography.net/cod/cif/4/06/02/4060263.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4060263 _journal_name_full 'Organometallics' _journal_year 2004 _chemical_formula_sum 'C29 H68 B12 Li N O6 P Y' _chemical_formula_weight 783.38 _symmetry_cell_setting monoclinic _space_group_IT_number 15 _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _[local]_cod_cif_authors_sg_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.6463(15) _cell_length_b 21.4575(12) _cell_length_c 20.0659(10) _cell_angle_alpha 90.00 _cell_angle_beta 130.7080(10) _cell_angle_gamma 90.00 _cell_volume 9349.7(9) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.113 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3312 _exptl_absorpt_coefficient_mu 1.316 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.7553 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25121 _diffrn_reflns_av_R_equivalents 0.0691 _diffrn_reflns_av_sigmaI/netI 0.1175 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8243 _reflns_number_gt 3592 _reflns_threshold_expression >2sigma(I) _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^)+(0.0727P)^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_number_reflns 8243 _refine_ls_number_parameters 493 _refine_ls_number_restraints 81 _refine_ls_R_factor_all 0.1336 _refine_ls_R_factor_gt 0.0556 _refine_ls_wR_factor_ref 0.1489 _refine_ls_wR_factor_gt 0.1316 _refine_ls_goodness_of_fit_ref 0.849 _refine_ls_restrained_S_all 0.859 _refine_ls_shift/su_max 0.066 _refine_ls_shift/su_mean 0.005 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 Y1 Y 0.174454(7) 0.124834(9) 0.075741(10) 0.06480(6) Uani 1 1 d . . . P1 P 0.210121(16) 0.27335(2) 0.20672(2) 0.05512(16) Uani 1 1 d . . . N1 N 0.25193(5) 0.33761(6) 0.23449(7) 0.0635(5) Uani 1 1 d . . . C1 C 0.26552(6) 0.20933(8) 0.28268(8) 0.0523(6) Uani 1 1 d . . . C2 C 0.25426(6) 0.13834(7) 0.23719(9) 0.0561(6) Uani 1 1 d . . . C3 C 0.29559(7) 0.34934(9) 0.22063(10) 0.0783(7) Uani 1 1 d . . . H3A H 0.3066 0.3087 0.2121 0.094 Uiso 1 1 calc R . . C4 C 0.26647(8) 0.38757(10) 0.13685(11) 0.1055(9) Uani 1 1 d . . . H4A H 0.2295 0.3674 0.0875 0.158 Uiso 1 1 calc R . . H4B H 0.2950 0.3906 0.1270 0.158 Uiso 1 1 calc R . . H4C H 0.2568 0.4286 0.1437 0.158 Uiso 1 1 calc R . . C5 C 0.35585(7) 0.37987(10) 0.30088(13) 0.1089(10) Uani 1 1 d . . . H5A H 0.3737 0.3549 0.3522 0.163 Uiso 1 1 calc R . . H5B H 0.3472 0.4208 0.3098 0.163 Uiso 1 1 calc R . . H5C H 0.3842 0.3830 0.2907 0.163 Uiso 1 1 calc R . . C6 C 0.23145(7) 0.39259(9) 0.25500(11) 0.0866(8) Uani 1 1 d . . . H6A H 0.2571 0.4277 0.2646 0.104 Uiso 1 1 calc R . . C7 C 0.16531(8) 0.41099(11) 0.17934(14) 0.1283(12) Uani 1 1 d . . . H7A H 0.1600 0.4174 0.1274 0.193 Uiso 1 1 calc R . . H7B H 0.1558 0.4488 0.1938 0.193 Uiso 1 1 calc R . . H7C H 0.1382 0.3784 0.1689 0.193 Uiso 1 1 calc R . . C8 C 0.24390(9) 0.38334(10) 0.34004(12) 0.1272(11) Uani 1 1 d . . . H8A H 0.2864 0.3726 0.3860 0.191 Uiso 1 1 calc R . . H8B H 0.2183 0.3503 0.3329 0.191 Uiso 1 1 calc R . . H8C H 0.2349 0.4212 0.3552 0.191 Uiso 1 1 calc R . . C11 C 0.18426(6) 0.24629(8) 0.10177(8) 0.0522(6) Uani 1 1 d . . . C12 C 0.21434(6) 0.23235(8) 0.06861(9) 0.0631(6) Uani 1 1 d . . . H12A H 0.2577 0.2416 0.0998 0.076 Uiso 1 1 calc R . . C13 C 0.17235(6) 0.21378(9) -0.01849(9) 0.0703(7) Uani 1 1 d . . . H13A H 0.1813 0.2080 -0.0577 0.084 Uiso 1 1 calc R . . C14 C 0.05310(8) 0.20281(11) -0.12607(11) 0.0991(10) Uani 1 1 d . . . H14A H 0.0480 0.1874 -0.1738 0.119 Uiso 1 1 calc R . . C15 C 0.00414(9) 0.21293(12) -0.13211(12) 0.1122(11) Uani 1 1 d . . . H15A H -0.0351 0.2047 -0.1850 0.135 Uiso 1 1 calc R . . C16 C 0.01057(7) 0.23558(11) -0.06089(11) 0.1009(10) Uani 1 1 d . . . H16A H -0.0245 0.2423 -0.0680 0.121 Uiso 1 1 calc R . . C17 C 0.06658(6) 0.24788(9) 0.01793(10) 0.0784(8) Uani 1 1 d . . . H17A H 0.0699 0.2625 0.0645 0.094 Uiso 1 1 calc R . . C18 C 0.11980(6) 0.23832(8) 0.02850(9) 0.0601(7) Uani 1 1 d . . . C19 C 0.11312(7) 0.21622(9) -0.04489(9) 0.0703(7) Uani 1 1 d . . . C21 C 0.47613(8) 0.00082(13) 0.37878(12) 0.1578(13) Uani 1 1 d D . . H21A H 0.4857 0.0139 0.4323 0.237 Uiso 1 1 calc R . . H21B H 0.4902 -0.0412 0.3853 0.237 Uiso 1 1 calc R . . H21C H 0.4324 0.0027 0.3313 0.237 Uiso 1 1 calc R . . C22 C 0.54560(10) 0.08062(14) 0.42349(13) 0.1536(15) Uani 1 1 d D . . H22A H 0.5749 0.0585 0.4786 0.184 Uiso 1 1 calc R . . H22B H 0.5239 0.1103 0.4312 0.184 Uiso 1 1 calc R . . C23 C 0.58102(12) 0.11649(17) 0.40118(16) 0.214(2) Uani 1 1 d D . . H23A H 0.5718 0.1605 0.3977 0.257 Uiso 1 1 calc R . . H23B H 0.6247 0.1114 0.4503 0.257 Uiso 1 1 calc R . . C24 C 0.59575(9) 0.14104(13) 0.30573(14) 0.1544(14) Uani 1 1 d D . . H24A H 0.6263 0.1659 0.3563 0.232 Uiso 1 1 calc R . . H24B H 0.5643 0.1677 0.2586 0.232 Uiso 1 1 calc R . . H24C H 0.6147 0.1181 0.2878 0.232 Uiso 1 1 calc R . . C25 C 0.62473(9) -0.0384(2) 0.36844(15) 0.248(2) Uani 1 1 d D . . H25A H 0.6437 -0.0775 0.3751 0.371 Uiso 1 1 calc R . . H25B H 0.6288 -0.0309 0.4192 0.371 Uiso 1 1 calc R . . H25C H 0.6445 -0.0055 0.3626 0.371 Uiso 1 1 calc R . . C27 C 0.4179(2) 0.4099(3) 0.5585(3) 0.480(5) Uani 1 1 d D . . H27A H 0.4029 0.3946 0.5026 0.720 Uiso 1 1 calc R . . H27B H 0.4363 0.4501 0.5693 0.720 Uiso 1 1 calc R . . H27C H 0.3843 0.4133 0.5581 0.720 Uiso 1 1 calc R . . C28 C 0.49009(16) 0.3396(3) 0.6013(2) 0.524(3) Uani 1 1 d D . . H28A H 0.5129 0.3685 0.5947 0.629 Uiso 1 1 calc R . . H28B H 0.4613 0.3165 0.5471 0.629 Uiso 1 1 calc R . . C29 C 0.54148(13) 0.2877(2) 0.69388(18) 0.315(2) Uani 1 1 d D . . H29A H 0.5191 0.2504 0.6856 0.378 Uiso 1 1 calc R . . H29B H 0.5749 0.2754 0.6957 0.378 Uiso 1 1 calc R . . C30 C 0.61255(14) 0.2902(2) 0.8532(2) 0.308(3) Uani 1 1 d D . . H30A H 0.6358 0.2606 0.8493 0.463 Uiso 1 1 calc R . . H30B H 0.5957 0.2701 0.8762 0.463 Uiso 1 1 calc R . . H30C H 0.6390 0.3237 0.8916 0.463 Uiso 1 1 calc R . . C31 C 0.60955(8) 0.45884(17) 0.78486(17) 0.2434(17) Uani 1 1 d D . . H31A H 0.6242 0.5008 0.7940 0.365 Uiso 1 1 calc R . . H31B H 0.6015 0.4418 0.7340 0.365 Uiso 1 1 calc R . . H31C H 0.6402 0.4341 0.8355 0.365 Uiso 1 1 calc R . . C32 C 0.52828(10) 0.51639(15) 0.7505(2) 0.248(2) Uani 1 1 d D . . H32A H 0.5134 0.5285 0.6930 0.297 Uiso 1 1 calc R . . H32B H 0.5585 0.5470 0.7927 0.297 Uiso 1 1 calc R . . B3 B 0.22674(8) 0.15328(10) 0.28995(11) 0.0666(8) Uani 1 1 d . . . H3 H 0.1772 0.1556 0.2551 0.080 Uiso 1 1 calc R . . B4 B 0.28019(9) 0.20218(11) 0.37887(12) 0.0761(9) Uani 1 1 d . . . H4 H 0.2656 0.2364 0.4030 0.091 Uiso 1 1 calc R . . B5 B 0.33876(9) 0.21919(12) 0.37658(12) 0.0785(10) Uani 1 1 d . . . H5 H 0.3628 0.2643 0.3996 0.094 Uiso 1 1 calc R . . B6 B 0.32100(8) 0.17916(10) 0.28462(12) 0.0666(8) Uani 1 1 d . . . H6 H 0.3329 0.1982 0.2465 0.080 Uiso 1 1 calc R . . B7 B 0.26438(9) 0.08241(11) 0.30609(12) 0.0790(10) Uani 1 1 d . . . H7 H 0.2397 0.0376 0.2827 0.095 Uiso 1 1 calc R . . B8 B 0.28109(9) 0.12219(12) 0.39714(12) 0.0840(9) Uani 1 1 d . . . H8 H 0.2675 0.1038 0.4335 0.101 Uiso 1 1 calc R . . B9 B 0.35109(10) 0.16225(12) 0.45035(14) 0.0937(12) Uani 1 1 d . . . H9 H 0.3837 0.1698 0.5219 0.112 Uiso 1 1 calc R . . B10 B 0.37642(10) 0.14780(12) 0.39103(15) 0.0915(12) Uani 1 1 d . . . H10 H 0.4255 0.1462 0.4234 0.110 Uiso 1 1 calc R . . B11 B 0.32256(9) 0.09853(11) 0.30340(13) 0.0795(10) Uani 1 1 d . . . H11 H 0.3363 0.0643 0.2782 0.095 Uiso 1 1 calc R . . B12 B 0.34109(10) 0.08817(13) 0.40459(14) 0.0918(11) Uani 1 1 d . . . H12 H 0.3671 0.0474 0.4464 0.110 Uiso 1 1 calc R . . B13 B 0.22174(11) 0.05161(14) 0.03858(15) 0.1126(12) Uani 1 1 d . . . B14 B 0.08731(10) 0.07042(15) 0.05142(17) 0.1226(13) Uani 1 1 d . . . O1 O 0.50520(6) 0.03993(8) 0.36068(7) 0.1271(7) Uani 1 1 d D . . O2 O 0.57035(5) 0.10087(8) 0.32613(8) 0.1189(7) Uani 1 1 d D . . O3 O 0.56403(6) -0.04040(8) 0.29540(9) 0.1268(8) Uani 1 1 d D . . O4 O 0.46123(10) 0.36936(13) 0.62369(12) 0.2309(14) Uani 1 1 d D . . O5 O 0.56479(8) 0.31392(13) 0.76984(11) 0.2459(12) Uani 1 1 d D . . O6 O 0.55626(7) 0.45859(9) 0.77212(12) 0.1863(10) Uani 1 1 d D . . Li1 Li 0.5000 0.0336(2) 0.2500 0.0724(17) Uani 1 2 d S . . Li2 Li 0.5000 0.3829(3) 0.7500 0.098(2) Uani 1 2 d S . . C26 C 0.54138(17) -0.09751(16) 0.2934(3) 0.310(4) Uani 1 1 d D . . H26A H 0.5521 -0.1056 0.3494 0.372 Uiso 1 1 calc R . . H26B H 0.5594 -0.1300 0.2828 0.372 Uiso 1 1 calc R . . H13B H 0.2171(7) 0.0304(11) 0.0824(11) 0.162(9) Uiso 1 1 d . . . H13C H 0.1729(6) 0.0714(10) -0.0136(9) 0.127(7) Uiso 1 1 d . . . H14B H 0.1206(7) 0.1071(10) 0.0845(11) 0.144(8) Uiso 1 1 d . . . H14C H 0.0842(7) 0.0773(10) -0.0086(10) 0.140(8) Uiso 1 1 d . . . H13D H 0.2517(7) 0.0928(11) 0.0763(10) 0.142(8) Uiso 1 1 d . . . H14D H 0.1252(6) 0.0417(9) 0.0826(9) 0.113(7) Uiso 1 1 d . . . H13E H 0.2412(6) 0.0191(9) 0.0182(9) 0.124(7) Uiso 1 1 d . . . H14E H 0.0525(6) 0.0441(9) 0.0365(9) 0.113(7) 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 Y1 0.08107(7) 0.04694(10) 0.06454(6) -0.00350(8) 0.04667(5) -0.00495(9) P1 0.06533(17) 0.0399(3) 0.06431(17) 0.00231(18) 0.04413(12) 0.00353(19) N1 0.0800(5) 0.0376(8) 0.0798(6) -0.0005(6) 0.0551(4) 0.0020(6) C1 0.0586(6) 0.0424(10) 0.0562(6) 0.0033(7) 0.0374(4) 0.0005(7) C2 0.0717(7) 0.0335(10) 0.0596(6) 0.0055(6) 0.0413(5) 0.0038(7) C3 0.1023(8) 0.0435(11) 0.1167(8) -0.0065(8) 0.0836(5) -0.0072(8) C4 0.1514(10) 0.0807(16) 0.1092(9) 0.0019(10) 0.0959(6) -0.0254(11) C5 0.0960(9) 0.0853(16) 0.1416(12) -0.0068(12) 0.0757(7) -0.0214(11) C6 0.1139(9) 0.0386(11) 0.1194(9) -0.0117(8) 0.0815(6) -0.0005(9) C7 0.1125(11) 0.0743(15) 0.1537(15) 0.0052(13) 0.0672(10) 0.0423(12) C8 0.1921(12) 0.0847(17) 0.1400(10) -0.0350(11) 0.1238(8) -0.0076(13) C11 0.0633(6) 0.0412(10) 0.0572(6) 0.0057(6) 0.0415(4) 0.0035(7) C12 0.0744(7) 0.0448(10) 0.0790(7) 0.0066(7) 0.0540(5) -0.0069(7) C13 0.0909(7) 0.0680(13) 0.0668(6) 0.0043(8) 0.0580(5) -0.0035(9) C14 0.1001(10) 0.1132(18) 0.0615(8) 0.0047(10) 0.0428(7) -0.0102(12) C15 0.0846(11) 0.130(2) 0.0750(11) 0.0110(12) 0.0312(8) -0.0083(14) C16 0.0625(8) 0.122(2) 0.0989(10) 0.0159(12) 0.0441(7) 0.0044(11) C17 0.0639(7) 0.0825(14) 0.0829(8) 0.0104(9) 0.0454(5) 0.0077(9) C18 0.0660(7) 0.0480(11) 0.0594(7) 0.0063(7) 0.0378(5) -0.0026(8) C19 0.0839(8) 0.0621(12) 0.0509(7) 0.0079(8) 0.0378(5) -0.0021(9) C21 0.1612(10) 0.211(3) 0.1670(10) 0.0699(14) 0.1359(7) 0.0236(15) C22 0.1736(17) 0.150(3) 0.0997(12) -0.0289(15) 0.0727(10) 0.0022(19) C23 0.218(2) 0.216(4) 0.171(2) -0.081(2) 0.1103(16) -0.091(2) C24 0.1389(12) 0.157(2) 0.1741(16) -0.0255(16) 0.1052(9) -0.0680(14) C25 0.0982(13) 0.497(6) 0.0941(15) 0.056(3) 0.0392(11) 0.120(2) C27 0.393(6) 0.506(8) 0.131(4) -0.001(5) -0.010(4) 0.232(6) C28 0.664(3) 0.797(9) 0.3692(17) -0.405(3) 0.4514(15) -0.483(4) C29 0.4683(19) 0.280(5) 0.4645(19) -0.145(2) 0.4220(12) -0.095(3) C30 0.196(2) 0.406(5) 0.282(3) 0.218(3) 0.1382(19) 0.137(3) C31 0.1959(11) 0.207(4) 0.448(2) -0.103(2) 0.2629(10) -0.0746(18) C32 0.273(2) 0.157(3) 0.378(3) -0.056(2) 0.2408(18) -0.067(2) B3 0.0796(9) 0.0596(14) 0.0686(8) 0.0107(9) 0.0519(6) 0.0034(10) B4 0.0938(10) 0.0702(16) 0.0558(8) 0.0027(10) 0.0451(7) 0.0088(11) B5 0.0704(11) 0.0646(16) 0.0578(10) 0.0026(11) 0.0230(8) -0.0028(11) B6 0.0588(8) 0.0551(14) 0.0804(9) 0.0093(10) 0.0430(6) 0.0120(9) B7 0.1013(11) 0.0482(13) 0.0778(10) 0.0157(10) 0.0542(7) 0.0047(11) B8 0.1100(11) 0.0735(16) 0.0726(9) 0.0220(10) 0.0614(7) 0.0140(12) B9 0.0975(14) 0.0713(17) 0.0615(11) 0.0094(12) 0.0295(9) 0.0091(14) B10 0.0676(11) 0.0763(17) 0.0867(13) 0.0147(13) 0.0310(9) 0.0196(12) B11 0.0878(10) 0.0553(14) 0.0890(11) 0.0167(10) 0.0548(7) 0.0264(11) B12 0.1007(12) 0.0668(17) 0.0811(11) 0.0228(12) 0.0474(8) 0.0198(13) B13 0.1561(13) 0.090(2) 0.1201(11) 0.0008(13) 0.1025(8) 0.0276(14) B14 0.1084(11) 0.111(2) 0.1510(15) -0.0164(16) 0.0858(9) -0.0524(14) O1 0.1529(7) 0.1579(15) 0.0816(5) -0.0341(8) 0.0813(4) -0.0499(9) O2 0.1216(7) 0.1378(13) 0.0909(6) -0.0335(8) 0.0665(5) -0.0548(8) O3 0.1307(8) 0.0931(12) 0.1416(8) 0.0076(8) 0.0822(6) 0.0184(9) O4 0.2774(17) 0.257(3) 0.1221(10) -0.0452(13) 0.1145(9) 0.0231(18) O5 0.3235(11) 0.263(3) 0.2993(11) 0.0833(14) 0.2682(7) 0.1183(15) O6 0.2164(9) 0.1098(15) 0.3154(12) -0.0394(11) 0.2099(7) -0.0347(10) Li1 0.0642(16) 0.080(3) 0.0659(17) 0.000 0.0393(12) 0.000 Li2 0.099(2) 0.099(4) 0.090(2) 0.000 0.0590(15) 0.000 C26 0.409(6) 0.113(3) 0.230(4) 0.037(3) 0.130(3) 0.047(4) _cod_database_code 4060263