# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and The Centre National de la Recherche Scientifique, 2010 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Franois Nief' _publ_contact_author_email francois.nief@polytechnique.edu _publ_section_title ; Neutral ansa-bis(fluorenyl)silane neodymium borohydrides: synthesis, structural study and behaviour as catalysts in butadiene/ethylene copolymerisation ; loop_ _publ_author_name G.Cortial X.F.L.Goff M.Bousquie C.Boisson P.L.Floch 'Franois Nief' ; J.Thuilliez ; # Attachment '- 2010_cortial_njc.cif.txt' #compound 1a data_gc787 _database_code_depnum_ccdc_archive 'CCDC 772838' #TrackingRef '- 2010_cortial_njc.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H24 Si' _chemical_formula_sum 'C28 H24 Si' _chemical_formula_weight 388.56 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Aba2 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y, z+1/2' 'x+1/2, -y, z+1/2' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1' 'x+1/2, -y+1/2, z+1' _cell_length_a 18.538(1) _cell_length_b 35.874(1) _cell_length_c 12.751(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8479.8(8) _cell_formula_units_Z 16 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 5030 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.217 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3296 _exptl_absorpt_coefficient_mu 0.122 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9666 _exptl_absorpt_correction_T_max 0.9807 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _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 KappaCCD _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 24164 _diffrn_reflns_av_R_equivalents 0.0512 _diffrn_reflns_av_sigmaI/netI 0.0624 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7636 _reflns_number_gt 5763 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0611P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(12) _refine_ls_number_reflns 7636 _refine_ls_number_parameters 527 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0683 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.1191 _refine_ls_wR_factor_gt 0.0884 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si -0.75411(5) -0.635884(19) -0.32448(6) 0.03088(19) Uani 1 1 d . . . C1 C -0.85371(16) -0.62216(7) -0.3296(2) 0.0325(7) Uani 1 1 d . . . H1 H -0.8722 -0.6228 -0.4032 0.039 Uiso 1 1 calc R . . C2 C -0.89625(17) -0.64839(8) -0.2601(2) 0.0337(7) Uani 1 1 d . . . C3 C -0.90983(18) -0.68643(8) -0.2708(2) 0.0384(8) Uani 1 1 d . . . H3 H -0.8939 -0.6995 -0.3313 0.046 Uiso 1 1 calc R . . C4 C -0.9469(2) -0.70487(9) -0.1921(3) 0.0480(9) Uani 1 1 d . . . H4 H -0.9564 -0.7308 -0.1988 0.058 Uiso 1 1 calc R . . C5 C -0.97017(19) -0.68590(9) -0.1035(3) 0.0503(9) Uani 1 1 d . . . H5 H -0.9947 -0.6992 -0.0498 0.060 Uiso 1 1 calc R . . C6 C -0.95848(17) -0.64797(9) -0.0917(3) 0.0435(8) Uani 1 1 d . . . H6 H -0.9754 -0.6351 -0.0315 0.052 Uiso 1 1 calc R . . C7 C -0.92107(16) -0.62931(8) -0.1710(2) 0.0342(7) Uani 1 1 d . . . C8 C -0.90357(17) -0.58952(8) -0.1830(2) 0.0344(7) Uani 1 1 d . . . C9 C -0.91957(18) -0.55879(9) -0.1201(3) 0.0432(8) Uani 1 1 d . . . H9 H -0.9435 -0.5619 -0.0548 0.052 Uiso 1 1 calc R . . C10 C -0.9000(2) -0.52369(9) -0.1544(3) 0.0493(9) Uani 1 1 d . . . H10 H -0.9097 -0.5026 -0.1117 0.059 Uiso 1 1 calc R . . C11 C -0.86628(19) -0.51900(9) -0.2508(3) 0.0465(9) Uani 1 1 d . . . H11 H -0.8541 -0.4946 -0.2736 0.056 Uiso 1 1 calc R . . C12 C -0.84994(17) -0.54922(8) -0.3143(3) 0.0369(7) Uani 1 1 d . . . H12 H -0.8269 -0.5456 -0.3801 0.044 Uiso 1 1 calc R . . C13 C -0.86782(16) -0.58487(8) -0.2801(2) 0.0324(7) Uani 1 1 d . . . C14 C -0.72800(16) -0.63843(7) -0.1788(2) 0.0284(6) Uani 1 1 d . . . H14 H -0.7726 -0.6410 -0.1351 0.034 Uiso 1 1 calc R . . C15 C -0.67643(16) -0.66950(7) -0.1527(2) 0.0285(7) Uani 1 1 d . . . C16 C -0.68613(18) -0.70796(8) -0.1546(2) 0.0379(8) Uani 1 1 d . . . H16 H -0.7302 -0.7184 -0.1789 0.045 Uiso 1 1 calc R . . C17 C -0.6305(2) -0.73102(8) -0.1206(2) 0.0439(8) Uani 1 1 d . . . H17 H -0.6368 -0.7573 -0.1220 0.053 Uiso 1 1 calc R . . C18 C -0.56632(18) -0.71637(8) -0.0849(3) 0.0428(8) Uani 1 1 d . . . H18 H -0.5292 -0.7326 -0.0614 0.051 Uiso 1 1 calc R . . C19 C -0.55530(16) -0.67816(8) -0.0831(2) 0.0366(7) Uani 1 1 d . . . H19 H -0.5109 -0.6681 -0.0591 0.044 Uiso 1 1 calc R . . C20 C -0.61062(16) -0.65493(7) -0.1170(2) 0.0287(6) Uani 1 1 d . . . C21 C -0.61610(16) -0.61410(7) -0.11659(19) 0.0274(6) Uani 1 1 d . . . C22 C -0.56556(16) -0.58701(7) -0.0900(2) 0.0342(7) Uani 1 1 d . . . H22 H -0.5177 -0.5938 -0.0715 0.041 Uiso 1 1 calc R . . C23 C -0.58621(17) -0.54999(8) -0.0909(2) 0.0392(7) Uani 1 1 d . . . H23 H -0.5519 -0.5311 -0.0751 0.047 Uiso 1 1 calc R . . C24 C -0.65648(19) -0.54020(8) -0.1146(2) 0.0400(8) Uani 1 1 d . . . H24 H -0.6704 -0.5147 -0.1124 0.048 Uiso 1 1 calc R . . C25 C -0.70695(17) -0.56711(7) -0.1417(2) 0.0344(7) Uani 1 1 d . . . H25 H -0.7551 -0.5601 -0.1581 0.041 Uiso 1 1 calc R . . C26 C -0.68655(16) -0.60426(8) -0.1447(2) 0.0280(6) Uani 1 1 d . . . C27 C -0.69550(19) -0.60142(9) -0.3931(2) 0.0438(8) Uani 1 1 d . . . H27A H -0.6451 -0.6095 -0.3889 0.066 Uiso 1 1 calc R . . H27B H -0.7006 -0.5770 -0.3597 0.066 Uiso 1 1 calc R . . H27C H -0.7100 -0.5996 -0.4669 0.066 Uiso 1 1 calc R . . C28 C -0.7407(2) -0.68155(8) -0.3910(2) 0.0455(9) Uani 1 1 d . . . H28A H -0.7609 -0.6804 -0.4620 0.068 Uiso 1 1 calc R . . H28B H -0.7652 -0.7012 -0.3510 0.068 Uiso 1 1 calc R . . H28C H -0.6890 -0.6871 -0.3950 0.068 Uiso 1 1 calc R . . Si2 Si -0.77181(4) -0.88091(2) -0.58122(6) 0.03041(19) Uani 1 1 d . . . C29 C -0.79222(17) -0.88185(8) -0.4332(2) 0.0325(7) Uani 1 1 d . . . H29 H -0.7463 -0.8779 -0.3936 0.039 Uiso 1 1 calc R . . C30 C -0.82636(18) -0.91804(8) -0.3976(2) 0.0370(7) Uani 1 1 d . . . C31 C -0.7980(2) -0.95391(9) -0.3979(3) 0.0485(9) Uani 1 1 d . . . H31 H -0.7507 -0.9584 -0.4236 0.058 Uiso 1 1 calc R . . C32 C -0.8396(2) -0.98301(10) -0.3603(3) 0.0619(11) Uani 1 1 d . . . H32 H -0.8206 -1.0076 -0.3597 0.074 Uiso 1 1 calc R . . C33 C -0.9081(2) -0.97652(10) -0.3238(3) 0.0655(11) Uani 1 1 d . . . H33 H -0.9361 -0.9970 -0.2996 0.079 Uiso 1 1 calc R . . C34 C -0.9379(2) -0.94114(10) -0.3211(3) 0.0540(9) Uani 1 1 d . . . H34 H -0.9853 -0.9371 -0.2951 0.065 Uiso 1 1 calc R . . C35 C -0.89553(18) -0.91144(9) -0.3581(2) 0.0388(7) Uani 1 1 d . . . C36 C -0.90870(18) -0.87102(9) -0.3585(2) 0.0381(8) Uani 1 1 d . . . C37 C -0.9669(2) -0.85029(10) -0.3218(3) 0.0526(9) Uani 1 1 d . . . H37 H -1.0088 -0.8622 -0.2952 0.063 Uiso 1 1 calc R . . C38 C -0.9621(2) -0.81210(11) -0.3251(3) 0.0642(12) Uani 1 1 d . . . H38 H -1.0012 -0.7976 -0.2999 0.077 Uiso 1 1 calc R . . C39 C -0.9016(3) -0.79421(11) -0.3644(3) 0.0640(12) Uani 1 1 d . . . H39 H -0.9002 -0.7677 -0.3667 0.077 Uiso 1 1 calc R . . C40 C -0.8424(2) -0.81473(9) -0.4006(2) 0.0514(9) Uani 1 1 d . . . H40 H -0.8003 -0.8025 -0.4257 0.062 Uiso 1 1 calc R . . C41 C -0.84661(17) -0.85324(8) -0.3989(2) 0.0353(7) Uani 1 1 d . . . C42 C -0.67127(15) -0.87010(7) -0.5923(2) 0.0311(7) Uani 1 1 d . . . H42 H -0.6543 -0.8715 -0.6666 0.037 Uiso 1 1 calc R . . C43 C -0.62930(15) -0.89630(8) -0.5224(2) 0.0293(6) Uani 1 1 d . . . C44 C -0.61924(16) -0.93463(8) -0.5302(2) 0.0353(7) Uani 1 1 d . . . H44 H -0.6378 -0.9481 -0.5885 0.042 Uiso 1 1 calc R . . C45 C -0.58173(17) -0.95285(8) -0.4514(2) 0.0376(7) Uani 1 1 d . . . H45 H -0.5749 -0.9790 -0.4559 0.045 Uiso 1 1 calc R . . C46 C -0.55399(18) -0.93369(8) -0.3664(2) 0.0381(8) Uani 1 1 d . . . H46 H -0.5285 -0.9468 -0.3134 0.046 Uiso 1 1 calc R . . C47 C -0.56307(17) -0.89542(8) -0.3579(2) 0.0341(7) Uani 1 1 d . . . H47 H -0.5436 -0.8821 -0.3000 0.041 Uiso 1 1 calc R . . C48 C -0.60137(16) -0.87685(8) -0.4363(2) 0.0295(6) Uani 1 1 d . . . C49 C -0.61722(16) -0.83708(8) -0.4496(2) 0.0301(7) Uani 1 1 d . . . C50 C -0.59960(17) -0.80613(8) -0.3884(2) 0.0361(7) Uani 1 1 d . . . H50 H -0.5748 -0.8091 -0.3237 0.043 Uiso 1 1 calc R . . C51 C -0.61880(19) -0.77111(8) -0.4233(3) 0.0431(8) Uani 1 1 d . . . H51 H -0.6077 -0.7499 -0.3817 0.052 Uiso 1 1 calc R . . C52 C -0.65399(18) -0.76645(8) -0.5181(3) 0.0431(8) Uani 1 1 d . . . H52 H -0.6657 -0.7420 -0.5412 0.052 Uiso 1 1 calc R . . C53 C -0.67247(16) -0.79685(7) -0.5801(3) 0.0386(7) Uani 1 1 d . . . H53 H -0.6964 -0.7934 -0.6452 0.046 Uiso 1 1 calc R . . C54 C -0.65505(16) -0.83265(8) -0.5445(2) 0.0310(7) Uani 1 1 d . . . C55 C -0.79381(19) -0.92620(8) -0.6457(2) 0.0443(8) Uani 1 1 d . . . H55A H -0.8455 -0.9313 -0.6381 0.066 Uiso 1 1 calc R . . H55B H -0.7660 -0.9462 -0.6126 0.066 Uiso 1 1 calc R . . H55C H -0.7815 -0.9248 -0.7204 0.066 Uiso 1 1 calc R . . C56 C -0.82530(18) -0.84458(9) -0.6499(2) 0.0409(8) Uani 1 1 d . . . H56A H -0.8116 -0.8439 -0.7241 0.061 Uiso 1 1 calc R . . H56B H -0.8158 -0.8202 -0.6180 0.061 Uiso 1 1 calc R . . H56C H -0.8768 -0.8504 -0.6440 0.061 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 Si1 0.0347(5) 0.0330(4) 0.0250(4) -0.0026(4) -0.0030(3) -0.0004(4) C1 0.0356(19) 0.0332(15) 0.0285(15) 0.0026(13) -0.0090(13) -0.0004(13) C2 0.0297(18) 0.0389(17) 0.0323(16) 0.0011(13) -0.0100(13) 0.0006(14) C3 0.042(2) 0.0366(17) 0.0366(17) 0.0013(13) -0.0082(15) -0.0041(14) C4 0.049(2) 0.0405(18) 0.055(2) 0.0082(17) -0.0102(18) -0.0137(16) C5 0.046(2) 0.053(2) 0.053(2) 0.0143(17) 0.0010(17) -0.0126(16) C6 0.0354(19) 0.0525(18) 0.0425(19) 0.0071(16) 0.0013(16) -0.0016(15) C7 0.0292(19) 0.0410(17) 0.0325(16) 0.0046(14) -0.0075(14) 0.0013(14) C8 0.0290(19) 0.0378(17) 0.0364(16) 0.0018(14) -0.0070(13) 0.0039(13) C9 0.042(2) 0.0464(19) 0.0407(18) -0.0003(15) -0.0007(15) 0.0085(16) C10 0.053(2) 0.0413(19) 0.053(2) -0.0102(16) -0.0129(17) 0.0130(16) C11 0.056(2) 0.0317(17) 0.052(2) 0.0027(15) -0.0164(18) 0.0041(15) C12 0.0343(19) 0.0365(16) 0.0401(17) 0.0105(14) -0.0097(15) 0.0011(13) C13 0.0307(18) 0.0346(16) 0.0319(15) 0.0027(12) -0.0096(13) 0.0030(13) C14 0.0266(18) 0.0348(15) 0.0237(13) -0.0041(12) -0.0007(12) -0.0007(12) C15 0.0367(19) 0.0301(15) 0.0188(13) 0.0006(11) 0.0020(12) -0.0011(13) C16 0.048(2) 0.0333(16) 0.0326(16) -0.0007(13) -0.0005(15) -0.0041(14) C17 0.063(3) 0.0299(16) 0.0384(17) 0.0026(14) 0.0008(17) 0.0047(16) C18 0.052(2) 0.0384(16) 0.0379(16) 0.0015(16) -0.0020(18) 0.0163(15) C19 0.0367(18) 0.0399(16) 0.0333(15) -0.0010(15) -0.0029(16) 0.0061(13) C20 0.0329(18) 0.0310(15) 0.0223(13) -0.0007(11) 0.0022(12) 0.0002(13) C21 0.0295(18) 0.0326(15) 0.0200(13) -0.0006(11) 0.0012(12) -0.0016(12) C22 0.0279(17) 0.0390(16) 0.0356(16) -0.0030(14) -0.0041(14) -0.0045(12) C23 0.043(2) 0.0349(16) 0.0395(17) -0.0037(15) -0.0022(16) -0.0108(14) C24 0.057(2) 0.0281(15) 0.0352(17) -0.0022(13) -0.0052(15) 0.0002(15) C25 0.0375(19) 0.0329(16) 0.0327(15) -0.0008(13) -0.0084(14) 0.0044(13) C26 0.0312(18) 0.0318(15) 0.0210(13) -0.0020(11) -0.0008(12) 0.0007(13) C27 0.045(2) 0.054(2) 0.0319(16) 0.0032(15) 0.0040(15) -0.0055(16) C28 0.055(2) 0.0487(19) 0.0329(17) -0.0115(15) -0.0059(16) 0.0087(17) Si2 0.0320(5) 0.0328(4) 0.0264(4) -0.0024(4) -0.0013(4) -0.0020(3) C29 0.0296(18) 0.0403(17) 0.0277(14) -0.0005(12) 0.0003(13) -0.0034(13) C30 0.039(2) 0.0430(17) 0.0288(15) 0.0036(13) -0.0017(14) -0.0051(14) C31 0.056(2) 0.0433(19) 0.046(2) 0.0088(15) 0.0015(18) 0.0035(16) C32 0.074(3) 0.044(2) 0.068(3) 0.0145(19) 0.005(2) 0.002(2) C33 0.070(3) 0.051(2) 0.076(3) 0.016(2) 0.006(2) -0.018(2) C34 0.044(2) 0.070(2) 0.047(2) 0.0105(19) 0.0065(18) -0.0106(19) C35 0.035(2) 0.0497(19) 0.0314(15) 0.0031(14) -0.0018(14) -0.0063(16) C36 0.036(2) 0.055(2) 0.0239(15) 0.0003(14) -0.0013(14) 0.0038(16) C37 0.046(2) 0.076(3) 0.0360(18) 0.0011(19) 0.0064(16) 0.0147(19) C38 0.077(3) 0.077(3) 0.038(2) 0.001(2) 0.009(2) 0.039(2) C39 0.108(4) 0.047(2) 0.0365(19) -0.0036(16) 0.008(2) 0.019(2) C40 0.077(3) 0.043(2) 0.0338(18) -0.0069(15) 0.0090(18) 0.0004(18) C41 0.041(2) 0.0430(17) 0.0223(14) -0.0015(13) -0.0026(13) 0.0012(15) C42 0.0325(17) 0.0351(14) 0.0259(15) 0.0006(12) 0.0042(13) -0.0008(12) C43 0.0243(17) 0.0323(15) 0.0312(15) -0.0010(12) 0.0064(13) -0.0031(12) C44 0.0338(19) 0.0330(16) 0.0392(16) -0.0049(13) 0.0047(14) -0.0036(13) C45 0.0314(19) 0.0301(15) 0.0513(19) 0.0040(14) 0.0078(15) 0.0015(13) C46 0.0281(19) 0.0420(18) 0.0442(18) 0.0080(15) 0.0038(15) 0.0030(14) C47 0.0290(19) 0.0374(16) 0.0359(16) 0.0011(13) 0.0027(14) -0.0033(14) C48 0.0240(16) 0.0330(15) 0.0314(15) -0.0018(13) 0.0073(12) -0.0008(13) C49 0.0260(17) 0.0346(16) 0.0295(15) -0.0012(12) 0.0078(12) -0.0054(13) C50 0.0329(18) 0.0386(17) 0.0367(16) -0.0048(13) 0.0029(14) -0.0068(14) C51 0.048(2) 0.0307(17) 0.051(2) -0.0075(14) 0.0046(17) -0.0089(15) C52 0.049(2) 0.0293(16) 0.051(2) 0.0026(14) 0.0059(17) -0.0037(14) C53 0.0402(19) 0.0366(15) 0.0389(16) 0.0039(15) 0.0054(17) -0.0008(13) C54 0.0293(18) 0.0304(14) 0.0332(16) 0.0000(12) 0.0093(12) -0.0056(12) C55 0.049(2) 0.0444(19) 0.0396(17) -0.0082(15) -0.0051(16) -0.0045(16) C56 0.040(2) 0.0497(19) 0.0333(16) 0.0016(14) -0.0052(14) 0.0022(15) _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 Si1 C28 1.861(3) . ? Si1 C27 1.864(3) . ? Si1 C1 1.912(3) . ? Si1 C14 1.922(3) . ? C1 C13 1.502(4) . ? C1 C2 1.514(4) . ? C1 H1 1.0000 . ? C2 C3 1.395(4) . ? C2 C7 1.403(4) . ? C3 C4 1.384(5) . ? C3 H3 0.9500 . ? C4 C5 1.388(5) . ? C4 H4 0.9500 . ? C5 C6 1.386(4) . ? C5 H5 0.9500 . ? C6 C7 1.397(4) . ? C6 H6 0.9500 . ? C7 C8 1.471(4) . ? C8 C9 1.396(4) . ? C8 C13 1.414(4) . ? C9 C10 1.382(5) . ? C9 H9 0.9500 . ? C10 C11 1.389(5) . ? C10 H10 0.9500 . ? C11 C12 1.387(4) . ? C11 H11 0.9500 . ? C12 C13 1.391(4) . ? C12 H12 0.9500 . ? C14 C15 1.506(4) . ? C14 C26 1.510(4) . ? C14 H14 1.0000 . ? C15 C16 1.392(4) . ? C15 C20 1.403(4) . ? C16 C17 1.392(4) . ? C16 H16 0.9500 . ? C17 C18 1.377(5) . ? C17 H17 0.9500 . ? C18 C19 1.386(4) . ? C18 H18 0.9500 . ? C19 C20 1.390(4) . ? C19 H19 0.9500 . ? C20 C21 1.468(4) . ? C21 C22 1.392(4) . ? C21 C26 1.400(4) . ? C22 C23 1.382(4) . ? C22 H22 0.9500 . ? C23 C24 1.383(5) . ? C23 H23 0.9500 . ? C24 C25 1.388(4) . ? C24 H24 0.9500 . ? C25 C26 1.386(4) . ? C25 H25 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? Si2 C56 1.857(3) . ? Si2 C55 1.866(3) . ? Si2 C42 1.909(3) . ? Si2 C29 1.925(3) . ? C29 C41 1.504(4) . ? C29 C30 1.514(4) . ? C29 H29 1.0000 . ? C30 C31 1.390(4) . ? C30 C35 1.398(5) . ? C31 C32 1.383(5) . ? C31 H31 0.9500 . ? C32 C33 1.373(6) . ? C32 H32 0.9500 . ? C33 C34 1.385(5) . ? C33 H33 0.9500 . ? C34 C35 1.406(4) . ? C34 H34 0.9500 . ? C35 C36 1.470(4) . ? C36 C37 1.391(5) . ? C36 C41 1.413(4) . ? C37 C38 1.374(5) . ? C37 H37 0.9500 . ? C38 C39 1.386(6) . ? C38 H38 0.9500 . ? C39 C40 1.399(5) . ? C39 H39 0.9500 . ? C40 C41 1.384(4) . ? C40 H40 0.9500 . ? C42 C54 1.506(4) . ? C42 C43 1.511(4) . ? C42 H42 1.0000 . ? C43 C44 1.391(4) . ? C43 C48 1.399(4) . ? C44 C45 1.385(4) . ? C44 H44 0.9500 . ? C45 C46 1.383(4) . ? C45 H45 0.9500 . ? C46 C47 1.387(4) . ? C46 H46 0.9500 . ? C47 C48 1.396(4) . ? C47 H47 0.9500 . ? C48 C49 1.466(4) . ? C49 C50 1.396(4) . ? C49 C54 1.407(4) . ? C50 C51 1.380(4) . ? C50 H50 0.9500 . ? C51 C52 1.384(5) . ? C51 H51 0.9500 . ? C52 C53 1.390(4) . ? C52 H52 0.9500 . ? C53 C54 1.400(4) . ? C53 H53 0.9500 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C28 Si1 C27 106.98(16) . . ? C28 Si1 C1 109.89(15) . . ? C27 Si1 C1 112.09(14) . . ? C28 Si1 C14 111.41(13) . . ? C27 Si1 C14 109.79(14) . . ? C1 Si1 C14 106.75(13) . . ? C13 C1 C2 102.5(2) . . ? C13 C1 Si1 112.6(2) . . ? C2 C1 Si1 108.85(19) . . ? C13 C1 H1 110.9 . . ? C2 C1 H1 110.9 . . ? Si1 C1 H1 110.9 . . ? C3 C2 C7 119.9(3) . . ? C3 C2 C1 130.1(3) . . ? C7 C2 C1 109.9(2) . . ? C4 C3 C2 119.0(3) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 120.7(3) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C6 C5 C4 121.4(3) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C5 C6 C7 118.0(3) . . ? C5 C6 H6 121.0 . . ? C7 C6 H6 121.0 . . ? C6 C7 C2 121.0(3) . . ? C6 C7 C8 130.5(3) . . ? C2 C7 C8 108.5(3) . . ? C9 C8 C13 120.6(3) . . ? C9 C8 C7 131.3(3) . . ? C13 C8 C7 108.0(2) . . ? C10 C9 C8 118.8(3) . . ? C10 C9 H9 120.6 . . ? C8 C9 H9 120.6 . . ? C9 C10 C11 120.6(3) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C12 C11 C10 121.4(3) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C11 C12 C13 118.9(3) . . ? C11 C12 H12 120.6 . . ? C13 C12 H12 120.6 . . ? C12 C13 C8 119.7(3) . . ? C12 C13 C1 130.2(3) . . ? C8 C13 C1 110.1(2) . . ? C15 C14 C26 102.4(2) . . ? C15 C14 Si1 114.10(18) . . ? C26 C14 Si1 111.54(18) . . ? C15 C14 H14 109.5 . . ? C26 C14 H14 109.5 . . ? Si1 C14 H14 109.5 . . ? C16 C15 C20 119.2(3) . . ? C16 C15 C14 130.4(3) . . ? C20 C15 C14 110.4(2) . . ? C15 C16 C17 119.2(3) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? C18 C17 C16 121.1(3) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C17 C18 C19 120.7(3) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C18 C19 C20 118.6(3) . . ? C18 C19 H19 120.7 . . ? C20 C19 H19 120.7 . . ? C19 C20 C15 121.3(2) . . ? C19 C20 C21 130.4(3) . . ? C15 C20 C21 108.2(2) . . ? C22 C21 C26 121.0(2) . . ? C22 C21 C20 130.6(3) . . ? C26 C21 C20 108.4(2) . . ? C23 C22 C21 118.8(3) . . ? C23 C22 H22 120.6 . . ? C21 C22 H22 120.6 . . ? C22 C23 C24 120.5(3) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C23 C24 C25 120.8(3) . . ? C23 C24 H24 119.6 . . ? C25 C24 H24 119.6 . . ? C26 C25 C24 119.5(3) . . ? C26 C25 H25 120.3 . . ? C24 C25 H25 120.3 . . ? C25 C26 C21 119.3(3) . . ? C25 C26 C14 130.5(3) . . ? C21 C26 C14 110.1(2) . . ? Si1 C27 H27A 109.5 . . ? Si1 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si1 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si1 C28 H28A 109.5 . . ? Si1 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si1 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C56 Si2 C55 106.64(15) . . ? C56 Si2 C42 110.12(14) . . ? C55 Si2 C42 110.95(14) . . ? C56 Si2 C29 111.70(14) . . ? C55 Si2 C29 111.96(14) . . ? C42 Si2 C29 105.53(13) . . ? C41 C29 C30 102.6(2) . . ? C41 C29 Si2 113.9(2) . . ? C30 C29 Si2 113.04(19) . . ? C41 C29 H29 109.0 . . ? C30 C29 H29 109.0 . . ? Si2 C29 H29 109.0 . . ? C31 C30 C35 120.3(3) . . ? C31 C30 C29 129.4(3) . . ? C35 C30 C29 110.3(3) . . ? C32 C31 C30 119.2(4) . . ? C32 C31 H31 120.4 . . ? C30 C31 H31 120.4 . . ? C33 C32 C31 120.3(4) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C32 C33 C34 122.2(3) . . ? C32 C33 H33 118.9 . . ? C34 C33 H33 118.9 . . ? C33 C34 C35 117.6(3) . . ? C33 C34 H34 121.2 . . ? C35 C34 H34 121.2 . . ? C30 C35 C34 120.4(3) . . ? C30 C35 C36 108.5(3) . . ? C34 C35 C36 131.0(3) . . ? C37 C36 C41 120.8(3) . . ? C37 C36 C35 130.9(3) . . ? C41 C36 C35 108.1(3) . . ? C38 C37 C36 118.2(4) . . ? C38 C37 H37 120.9 . . ? C36 C37 H37 120.9 . . ? C37 C38 C39 121.7(3) . . ? C37 C38 H38 119.1 . . ? C39 C38 H38 119.1 . . ? C38 C39 C40 120.7(3) . . ? C38 C39 H39 119.7 . . ? C40 C39 H39 119.7 . . ? C41 C40 C39 118.4(4) . . ? C41 C40 H40 120.8 . . ? C39 C40 H40 120.8 . . ? C40 C41 C36 120.1(3) . . ? C40 C41 C29 129.7(3) . . ? C36 C41 C29 110.1(3) . . ? C54 C42 C43 102.3(2) . . ? C54 C42 Si2 110.27(19) . . ? C43 C42 Si2 109.45(18) . . ? C54 C42 H42 111.5 . . ? C43 C42 H42 111.5 . . ? Si2 C42 H42 111.5 . . ? C44 C43 C48 120.0(3) . . ? C44 C43 C42 129.9(3) . . ? C48 C43 C42 110.0(2) . . ? C45 C44 C43 118.8(3) . . ? C45 C44 H44 120.6 . . ? C43 C44 H44 120.6 . . ? C46 C45 C44 121.4(3) . . ? C46 C45 H45 119.3 . . ? C44 C45 H45 119.3 . . ? C45 C46 C47 120.5(3) . . ? C45 C46 H46 119.7 . . ? C47 C46 H46 119.7 . . ? C46 C47 C48 118.6(3) . . ? C46 C47 H47 120.7 . . ? C48 C47 H47 120.7 . . ? C47 C48 C43 120.8(3) . . ? C47 C48 C49 130.5(3) . . ? C43 C48 C49 108.7(2) . . ? C50 C49 C54 120.5(3) . . ? C50 C49 C48 131.5(3) . . ? C54 C49 C48 108.0(2) . . ? C51 C50 C49 118.9(3) . . ? C51 C50 H50 120.6 . . ? C49 C50 H50 120.6 . . ? C50 C51 C52 120.9(3) . . ? C50 C51 H51 119.5 . . ? C52 C51 H51 119.5 . . ? C51 C52 C53 121.2(3) . . ? C51 C52 H52 119.4 . . ? C53 C52 H52 119.4 . . ? C52 C53 C54 118.6(3) . . ? C52 C53 H53 120.7 . . ? C54 C53 H53 120.7 . . ? C53 C54 C49 119.8(3) . . ? C53 C54 C42 129.9(3) . . ? C49 C54 C42 110.3(2) . . ? Si2 C55 H55A 109.5 . . ? Si2 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? Si2 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? Si2 C56 H56A 109.5 . . ? Si2 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? Si2 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.307 _refine_diff_density_min -0.351 _refine_diff_density_rms 0.080 #===END #compound 1b data_gc671 _database_code_depnum_ccdc_archive 'CCDC 772839' #TrackingRef '- 2010_cortial_njc.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H28 Si' _chemical_formula_sum 'C30 H28 Si' _chemical_formula_weight 416.61 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' Si Si 0.0817 0.0704 '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 b c n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 17.026(1) _cell_length_b 9.952(1) _cell_length_c 13.230(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2241.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 24249 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.878 _exptl_crystal_description Plate _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.234 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 0.120 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9536 _exptl_absorpt_correction_T_max 0.9905 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _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 KappaCCD _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 14437 _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_av_sigmaI/netI 0.0316 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.30 _diffrn_reflns_theta_max 26.37 _reflns_number_total 2296 _reflns_number_gt 1797 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1670P)^2^+1.5409P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2296 _refine_ls_number_parameters 142 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1067 _refine_ls_R_factor_gt 0.0892 _refine_ls_wR_factor_ref 0.2523 _refine_ls_wR_factor_gt 0.2360 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.0000 -0.06086(11) 0.2500 0.0296(4) Uani 1 2 d S . . C1 C -0.00786(15) 0.0466(3) 0.3679(2) 0.0316(7) Uani 1 1 d . . . H1 H -0.0256 -0.0124 0.4247 0.038 Uiso 1 1 calc R . . C2 C -0.06560(16) 0.1613(3) 0.3587(2) 0.0352(7) Uani 1 1 d . . . C3 C -0.14539(18) 0.1587(4) 0.3343(2) 0.0405(8) Uani 1 1 d . . . H3 H -0.1717 0.0757 0.3237 0.049 Uiso 1 1 calc R . . C4 C -0.1858(2) 0.2799(4) 0.3258(3) 0.0486(9) Uani 1 1 d . . . H4 H -0.2401 0.2794 0.3095 0.058 Uiso 1 1 calc R . . C5 C -0.1475(2) 0.4016(4) 0.3406(3) 0.0512(9) Uani 1 1 d . . . H5 H -0.1758 0.4832 0.3331 0.061 Uiso 1 1 calc R . . C6 C -0.0686(2) 0.4057(4) 0.3663(3) 0.0450(8) Uani 1 1 d . . . H6 H -0.0428 0.4889 0.3778 0.054 Uiso 1 1 calc R . . C7 C -0.02803(18) 0.2840(3) 0.3748(2) 0.0360(7) Uani 1 1 d . . . C8 C 0.05351(17) 0.2571(3) 0.4021(2) 0.0314(7) Uani 1 1 d . . . C9 C 0.1141(2) 0.3459(4) 0.4312(2) 0.0450(8) Uani 1 1 d . . . H9 H 0.1057 0.4403 0.4313 0.054 Uiso 1 1 calc R . . C10 C 0.1860(2) 0.2932(4) 0.4595(2) 0.0455(9) Uani 1 1 d . . . H10 H 0.2274 0.3512 0.4798 0.055 Uiso 1 1 calc R . . C11 C 0.19733(18) 0.1554(4) 0.4582(2) 0.0426(8) Uani 1 1 d . . . H11 H 0.2471 0.1203 0.4773 0.051 Uiso 1 1 calc R . . C12 C 0.13820(18) 0.0666(3) 0.4296(2) 0.0388(8) Uani 1 1 d . . . H12 H 0.1471 -0.0277 0.4293 0.047 Uiso 1 1 calc R . . C13 C 0.06615(16) 0.1192(3) 0.4018(2) 0.0319(7) Uani 1 1 d . . . C14 C 0.08941(19) -0.1705(3) 0.2539(2) 0.0385(8) Uani 1 1 d . . . H14A H 0.0951 -0.2154 0.1875 0.046 Uiso 1 1 calc R . . H14B H 0.1361 -0.1126 0.2637 0.046 Uiso 1 1 calc R . . C15 C 0.0889(2) -0.2780(4) 0.3364(3) 0.0540(10) Uani 1 1 d . . . H15A H 0.0802 -0.2355 0.4022 0.081 Uiso 1 1 calc R . . H15B H 0.1395 -0.3250 0.3368 0.081 Uiso 1 1 calc R . . H15C H 0.0466 -0.3425 0.3229 0.081 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 Si1 0.0240(6) 0.0318(7) 0.0330(6) 0.000 0.0008(4) 0.000 C1 0.0260(14) 0.0387(16) 0.0301(14) 0.0011(12) 0.0028(10) -0.0022(12) C2 0.0277(15) 0.0517(19) 0.0263(13) -0.0033(12) 0.0065(11) 0.0046(13) C3 0.0296(15) 0.057(2) 0.0344(16) -0.0071(14) 0.0054(12) 0.0021(14) C4 0.0304(17) 0.071(2) 0.0446(18) -0.0055(17) 0.0061(14) 0.0128(16) C5 0.0391(19) 0.063(2) 0.0511(19) -0.0035(17) 0.0099(15) 0.0169(16) C6 0.0408(19) 0.051(2) 0.0431(17) -0.0025(15) 0.0079(14) 0.0022(15) C7 0.0325(16) 0.0468(18) 0.0285(14) -0.0043(13) 0.0082(12) 0.0004(13) C8 0.0293(15) 0.0407(17) 0.0240(13) -0.0006(11) 0.0035(11) -0.0024(12) C9 0.048(2) 0.0439(18) 0.0436(18) -0.0025(14) 0.0042(15) -0.0088(15) C10 0.0363(17) 0.057(2) 0.0433(17) -0.0017(15) -0.0059(14) -0.0116(15) C11 0.0320(16) 0.057(2) 0.0393(16) 0.0036(14) -0.0049(12) -0.0097(14) C12 0.0332(16) 0.0483(19) 0.0350(15) 0.0040(13) -0.0026(12) -0.0032(13) C13 0.0294(15) 0.0407(17) 0.0257(13) 0.0010(11) 0.0024(11) -0.0033(12) C14 0.0337(16) 0.0374(17) 0.0443(17) -0.0012(13) -0.0027(12) 0.0069(13) C15 0.045(2) 0.049(2) 0.068(2) 0.0132(17) -0.0101(17) 0.0047(16) _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 Si1 C14 1.873(3) 4 ? Si1 C14 1.873(3) . ? Si1 C1 1.896(3) . ? Si1 C1 1.896(3) 4 ? C1 C2 1.512(4) . ? C1 C13 1.520(4) . ? C1 H1 1.0000 . ? C2 C7 1.395(4) . ? C2 C3 1.396(4) . ? C3 C4 1.393(5) . ? C3 H3 0.9500 . ? C4 C5 1.389(5) . ? C4 H4 0.9500 . ? C5 C6 1.386(5) . ? C5 H5 0.9500 . ? C6 C7 1.399(5) . ? C6 H6 0.9500 . ? C7 C8 1.459(4) . ? C8 C13 1.390(4) . ? C8 C9 1.412(4) . ? C9 C10 1.383(5) . ? C9 H9 0.9500 . ? C10 C11 1.385(5) . ? C10 H10 0.9500 . ? C11 C12 1.392(4) . ? C11 H11 0.9500 . ? C12 C13 1.384(4) . ? C12 H12 0.9500 . ? C14 C15 1.529(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C14 Si1 C14 108.8(2) 4 . ? C14 Si1 C1 107.07(13) 4 . ? C14 Si1 C1 111.30(12) . . ? C14 Si1 C1 111.30(12) 4 4 ? C14 Si1 C1 107.07(13) . 4 ? C1 Si1 C1 111.34(19) . 4 ? C2 C1 C13 101.8(2) . . ? C2 C1 Si1 113.91(19) . . ? C13 C1 Si1 116.86(18) . . ? C2 C1 H1 107.9 . . ? C13 C1 H1 107.9 . . ? Si1 C1 H1 107.9 . . ? C7 C2 C3 119.8(3) . . ? C7 C2 C1 110.5(3) . . ? C3 C2 C1 129.6(3) . . ? C4 C3 C2 118.9(3) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C5 C4 C3 120.8(3) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C6 C5 C4 121.0(3) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 C7 118.2(3) . . ? C5 C6 H6 120.9 . . ? C7 C6 H6 120.9 . . ? C2 C7 C6 121.3(3) . . ? C2 C7 C8 108.3(3) . . ? C6 C7 C8 130.4(3) . . ? C13 C8 C9 120.4(3) . . ? C13 C8 C7 109.1(3) . . ? C9 C8 C7 130.4(3) . . ? C10 C9 C8 118.9(3) . . ? C10 C9 H9 120.6 . . ? C8 C9 H9 120.6 . . ? C9 C10 C11 119.7(3) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C10 C11 C12 122.1(3) . . ? C10 C11 H11 118.9 . . ? C12 C11 H11 118.9 . . ? C13 C12 C11 118.3(3) . . ? C13 C12 H12 120.9 . . ? C11 C12 H12 120.9 . . ? C12 C13 C8 120.7(3) . . ? C12 C13 C1 129.3(3) . . ? C8 C13 C1 110.0(3) . . ? C15 C14 Si1 115.0(2) . . ? C15 C14 H14A 108.5 . . ? Si1 C14 H14A 108.5 . . ? C15 C14 H14B 108.5 . . ? Si1 C14 H14B 108.5 . . ? H14A C14 H14B 107.5 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.507 _refine_diff_density_min -0.384 _refine_diff_density_rms 0.088 #===END #compound 1c data_gc235 _database_code_depnum_ccdc_archive 'CCDC 772840' #TrackingRef '- 2010_cortial_njc.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H24 Si' _chemical_formula_weight 400.57 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.740(1) _cell_length_b 9.839(1) _cell_length_c 13.604(1) _cell_angle_alpha 104.023(1) _cell_angle_beta 105.022(1) _cell_angle_gamma 102.433(1) _cell_volume 1046.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 3272 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.271 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 424 _exptl_absorpt_coefficient_mu 0.126 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9753 _exptl_absorpt_correction_T_max 0.9900 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _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 KappaCCD _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 7940 _diffrn_reflns_av_R_equivalents 0.0195 _diffrn_reflns_av_sigmaI/netI 0.0684 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 30.03 _reflns_number_total 6092 _reflns_number_gt 4019 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0590P)^2^+0.0151P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6092 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0848 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1304 _refine_ls_wR_factor_gt 0.1168 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.71734(5) 0.16734(4) 0.84119(3) 0.02584(12) Uani 1 1 d . . . C1 C 0.56453(17) 0.22840(16) 0.90552(12) 0.0276(3) Uani 1 1 d . . . H1 H 0.6089 0.2537 0.9853 0.033 Uiso 1 1 calc R . . C2 C 0.51835(17) 0.35471(17) 0.87390(12) 0.0286(3) Uani 1 1 d . . . C3 C 0.61485(19) 0.49788(17) 0.89849(13) 0.0349(4) Uani 1 1 d . . . H3 H 0.7266 0.5303 0.9449 0.042 Uiso 1 1 calc R . . C4 C 0.5464(2) 0.59335(19) 0.85454(14) 0.0415(4) Uani 1 1 d . . . H4 H 0.6119 0.6914 0.8703 0.050 Uiso 1 1 calc R . . C5 C 0.3822(2) 0.54578(19) 0.78736(14) 0.0417(4) Uani 1 1 d . . . H5 H 0.3375 0.6119 0.7570 0.050 Uiso 1 1 calc R . . C6 C 0.2835(2) 0.40517(19) 0.76403(13) 0.0361(4) Uani 1 1 d . . . H6 H 0.1710 0.3744 0.7190 0.043 Uiso 1 1 calc R . . C7 C 0.35162(17) 0.30853(17) 0.80785(12) 0.0285(3) Uani 1 1 d . . . C8 C 0.27868(17) 0.15632(17) 0.79901(11) 0.0274(3) Uani 1 1 d . . . C9 C 0.11852(18) 0.06200(18) 0.74453(12) 0.0316(4) Uani 1 1 d . . . H9 H 0.0362 0.0943 0.7038 0.038 Uiso 1 1 calc R . . C10 C 0.08056(18) -0.07877(18) 0.75025(13) 0.0335(4) Uani 1 1 d . . . H10 H -0.0288 -0.1432 0.7139 0.040 Uiso 1 1 calc R . . C11 C 0.20142(19) -0.12737(18) 0.80890(12) 0.0341(4) Uani 1 1 d . . . H11 H 0.1738 -0.2245 0.8124 0.041 Uiso 1 1 calc R . . C12 C 0.36238(18) -0.03404(17) 0.86239(12) 0.0304(3) Uani 1 1 d . . . H12 H 0.4452 -0.0680 0.9008 0.037 Uiso 1 1 calc R . . C13 C 0.40077(17) 0.10801(16) 0.85921(11) 0.0267(3) Uani 1 1 d . . . C14 C 0.61784(17) 0.10763(16) 0.68955(11) 0.0255(3) Uani 1 1 d . . . H14 H 0.4996 0.1082 0.6716 0.031 Uiso 1 1 calc R . . C15 C 0.70702(16) 0.20405(16) 0.63811(11) 0.0261(3) Uani 1 1 d . . . C16 C 0.74342(19) 0.35455(17) 0.65749(13) 0.0332(4) Uani 1 1 d . . . H16 H 0.7086 0.4127 0.7090 0.040 Uiso 1 1 calc R . . C17 C 0.8313(2) 0.41886(19) 0.60074(14) 0.0389(4) Uani 1 1 d . . . H17 H 0.8571 0.5218 0.6138 0.047 Uiso 1 1 calc R . . C18 C 0.8821(2) 0.33394(19) 0.52456(14) 0.0383(4) Uani 1 1 d . . . H18 H 0.9411 0.3795 0.4857 0.046 Uiso 1 1 calc R . . C19 C 0.84747(18) 0.18496(18) 0.50528(13) 0.0327(4) Uani 1 1 d . . . H19 H 0.8827 0.1274 0.4537 0.039 Uiso 1 1 calc R . . C20 C 0.76045(16) 0.11971(16) 0.56219(11) 0.0254(3) Uani 1 1 d . . . C21 C 0.70882(16) -0.03320(16) 0.55917(11) 0.0246(3) Uani 1 1 d . . . C22 C 0.73322(17) -0.15802(17) 0.49845(12) 0.0302(4) Uani 1 1 d . . . H22 H 0.7898 -0.1516 0.4480 0.036 Uiso 1 1 calc R . . C23 C 0.67376(19) -0.29074(17) 0.51293(13) 0.0340(4) Uani 1 1 d . . . H23 H 0.6890 -0.3766 0.4718 0.041 Uiso 1 1 calc R . . C24 C 0.59131(19) -0.30020(17) 0.58739(13) 0.0358(4) Uani 1 1 d . . . H24 H 0.5525 -0.3921 0.5973 0.043 Uiso 1 1 calc R . . C25 C 0.56551(18) -0.17655(17) 0.64696(12) 0.0313(3) Uani 1 1 d . . . H25 H 0.5079 -0.1836 0.6968 0.038 Uiso 1 1 calc R . . C26 C 0.62478(16) -0.04247(16) 0.63303(11) 0.0249(3) Uani 1 1 d . . . C27 C 0.82094(18) 0.04984(18) 0.90776(12) 0.0332(4) Uani 1 1 d . . . H27A H 0.7656 0.0112 0.9545 0.040 Uiso 1 1 calc R . . H27B H 0.8436 -0.0290 0.8580 0.040 Uiso 1 1 calc R . . C28 C 0.9729(2) 0.1892(2) 0.96910(14) 0.0424(4) Uani 1 1 d . . . H28A H 0.9781 0.2315 1.0442 0.051 Uiso 1 1 calc R . . H28B H 1.0784 0.1677 0.9686 0.051 Uiso 1 1 calc R . . C29 C 0.93449(18) 0.29265(17) 0.90205(13) 0.0349(4) Uani 1 1 d . . . H29A H 0.9957 0.2962 0.8504 0.042 Uiso 1 1 calc R . . H29B H 0.9441 0.3925 0.9455 0.042 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 Si1 0.0240(2) 0.0272(2) 0.0257(2) 0.00732(17) 0.00792(17) 0.00800(16) C1 0.0264(7) 0.0310(8) 0.0236(7) 0.0063(6) 0.0068(6) 0.0093(6) C2 0.0300(7) 0.0305(8) 0.0271(7) 0.0056(6) 0.0131(6) 0.0120(6) C3 0.0328(8) 0.0315(9) 0.0379(9) 0.0046(7) 0.0133(7) 0.0101(7) C4 0.0433(9) 0.0315(9) 0.0527(11) 0.0096(8) 0.0222(9) 0.0136(7) C5 0.0510(10) 0.0372(10) 0.0487(11) 0.0170(8) 0.0235(9) 0.0243(8) C6 0.0344(8) 0.0423(10) 0.0372(9) 0.0137(8) 0.0138(7) 0.0189(7) C7 0.0294(7) 0.0330(8) 0.0275(8) 0.0084(6) 0.0135(6) 0.0141(6) C8 0.0260(7) 0.0342(9) 0.0243(7) 0.0075(6) 0.0109(6) 0.0120(6) C9 0.0255(7) 0.0388(9) 0.0287(8) 0.0065(7) 0.0084(6) 0.0113(6) C10 0.0266(7) 0.0376(9) 0.0316(8) 0.0040(7) 0.0125(7) 0.0044(6) C11 0.0376(8) 0.0346(9) 0.0341(8) 0.0105(7) 0.0193(7) 0.0098(7) C12 0.0314(7) 0.0379(9) 0.0267(8) 0.0122(7) 0.0127(6) 0.0135(6) C13 0.0269(7) 0.0321(8) 0.0226(7) 0.0076(6) 0.0107(6) 0.0099(6) C14 0.0252(7) 0.0276(8) 0.0251(7) 0.0092(6) 0.0088(6) 0.0093(6) C15 0.0239(7) 0.0303(8) 0.0263(7) 0.0123(6) 0.0077(6) 0.0092(6) C16 0.0376(8) 0.0318(9) 0.0347(8) 0.0129(7) 0.0138(7) 0.0145(7) C17 0.0415(9) 0.0336(9) 0.0484(10) 0.0222(8) 0.0177(8) 0.0108(7) C18 0.0389(9) 0.0402(10) 0.0440(10) 0.0232(8) 0.0193(8) 0.0094(7) C19 0.0318(8) 0.0382(9) 0.0335(8) 0.0142(7) 0.0154(7) 0.0125(7) C20 0.0220(6) 0.0305(8) 0.0249(7) 0.0114(6) 0.0071(6) 0.0078(6) C21 0.0208(6) 0.0284(8) 0.0219(7) 0.0076(6) 0.0037(6) 0.0061(5) C22 0.0287(7) 0.0331(9) 0.0274(8) 0.0067(7) 0.0091(6) 0.0098(6) C23 0.0349(8) 0.0273(8) 0.0327(8) 0.0027(7) 0.0064(7) 0.0084(6) C24 0.0384(8) 0.0250(8) 0.0360(9) 0.0079(7) 0.0066(7) 0.0021(6) C25 0.0299(7) 0.0301(8) 0.0298(8) 0.0089(7) 0.0094(7) 0.0020(6) C26 0.0223(6) 0.0263(8) 0.0227(7) 0.0066(6) 0.0044(6) 0.0051(5) C27 0.0334(8) 0.0416(10) 0.0309(8) 0.0138(7) 0.0141(7) 0.0164(7) C28 0.0313(8) 0.0590(12) 0.0343(9) 0.0157(8) 0.0057(7) 0.0136(8) C29 0.0277(7) 0.0327(9) 0.0392(9) 0.0062(7) 0.0085(7) 0.0081(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 C29 1.8683(16) . ? Si1 C27 1.8733(15) . ? Si1 C1 1.8992(15) . ? Si1 C14 1.9026(14) . ? Si1 C28 2.3791(15) . ? C1 C2 1.509(2) . ? C1 C13 1.513(2) . ? C1 H1 1.0000 . ? C2 C3 1.386(2) . ? C2 C7 1.4056(19) . ? C3 C4 1.388(2) . ? C3 H3 0.9500 . ? C4 C5 1.392(2) . ? C4 H4 0.9500 . ? C5 C6 1.375(2) . ? C5 H5 0.9500 . ? C6 C7 1.396(2) . ? C6 H6 0.9500 . ? C7 C8 1.458(2) . ? C8 C9 1.393(2) . ? C8 C13 1.4105(19) . ? C9 C10 1.379(2) . ? C9 H9 0.9500 . ? C10 C11 1.395(2) . ? C10 H10 0.9500 . ? C11 C12 1.393(2) . ? C11 H11 0.9500 . ? C12 C13 1.379(2) . ? C12 H12 0.9500 . ? C14 C15 1.511(2) . ? C14 C26 1.5127(19) . ? C14 H14 1.0000 . ? C15 C16 1.388(2) . ? C15 C20 1.405(2) . ? C16 C17 1.386(2) . ? C16 H16 0.9500 . ? C17 C18 1.396(2) . ? C17 H17 0.9500 . ? C18 C19 1.375(2) . ? C18 H18 0.9500 . ? C19 C20 1.388(2) . ? C19 H19 0.9500 . ? C20 C21 1.462(2) . ? C21 C22 1.3958(19) . ? C21 C26 1.398(2) . ? C22 C23 1.378(2) . ? C22 H22 0.9500 . ? C23 C24 1.396(2) . ? C23 H23 0.9500 . ? C24 C25 1.387(2) . ? C24 H24 0.9500 . ? C25 C26 1.387(2) . ? C25 H25 0.9500 . ? C27 C28 1.558(2) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.555(2) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? 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 C29 Si1 C27 80.19(7) . . ? C29 Si1 C1 114.76(7) . . ? C27 Si1 C1 112.12(7) . . ? C29 Si1 C14 118.14(7) . . ? C27 Si1 C14 121.06(7) . . ? C1 Si1 C14 108.48(6) . . ? C29 Si1 C28 40.77(7) . . ? C27 Si1 C28 40.86(7) . . ? C1 Si1 C28 112.95(6) . . ? C14 Si1 C28 138.57(6) . . ? C2 C1 C13 102.72(11) . . ? C2 C1 Si1 111.72(11) . . ? C13 C1 Si1 109.15(10) . . ? C2 C1 H1 111.0 . . ? C13 C1 H1 111.0 . . ? Si1 C1 H1 111.0 . . ? C3 C2 C7 120.16(14) . . ? C3 C2 C1 129.77(13) . . ? C7 C2 C1 110.05(13) . . ? C2 C3 C4 119.26(14) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C3 C4 C5 120.18(16) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C6 C5 C4 121.39(16) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C5 C6 C7 118.70(14) . . ? C5 C6 H6 120.6 . . ? C7 C6 H6 120.6 . . ? C6 C7 C2 120.28(15) . . ? C6 C7 C8 131.17(13) . . ? C2 C7 C8 108.55(13) . . ? C9 C8 C13 120.22(15) . . ? C9 C8 C7 130.94(13) . . ? C13 C8 C7 108.84(12) . . ? C10 C9 C8 119.35(13) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C9 C10 C11 120.58(14) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C12 C11 C10 120.28(16) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C13 C12 C11 119.63(13) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C12 C13 C8 119.91(13) . . ? C12 C13 C1 130.40(12) . . ? C8 C13 C1 109.54(13) . . ? C15 C14 C26 102.32(12) . . ? C15 C14 Si1 112.89(9) . . ? C26 C14 Si1 113.41(9) . . ? C15 C14 H14 109.3 . . ? C26 C14 H14 109.3 . . ? Si1 C14 H14 109.3 . . ? C16 C15 C20 119.73(15) . . ? C16 C15 C14 130.04(14) . . ? C20 C15 C14 110.20(13) . . ? C17 C16 C15 119.15(15) . . ? C17 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? C16 C17 C18 120.71(16) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C19 C18 C17 120.55(17) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C18 C19 C20 119.16(15) . . ? C18 C19 H19 120.4 . . ? C20 C19 H19 120.4 . . ? C19 C20 C15 120.70(14) . . ? C19 C20 C21 130.85(13) . . ? C15 C20 C21 108.45(13) . . ? C22 C21 C26 120.70(14) . . ? C22 C21 C20 130.59(14) . . ? C26 C21 C20 108.71(12) . . ? C23 C22 C21 118.84(15) . . ? C23 C22 H22 120.6 . . ? C21 C22 H22 120.6 . . ? C22 C23 C24 120.64(15) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C25 C24 C23 120.57(15) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C26 C25 C24 119.27(15) . . ? C26 C25 H25 120.4 . . ? C24 C25 H25 120.4 . . ? C25 C26 C21 119.97(14) . . ? C25 C26 C14 129.69(14) . . ? C21 C26 C14 110.32(13) . . ? C28 C27 Si1 87.28(10) . . ? C28 C27 H27A 114.1 . . ? Si1 C27 H27A 114.1 . . ? C28 C27 H27B 114.1 . . ? Si1 C27 H27B 114.1 . . ? H27A C27 H27B 111.3 . . ? C29 C28 C27 101.43(12) . . ? C29 C28 Si1 51.68(7) . . ? C27 C28 Si1 51.86(7) . . ? C29 C28 H28A 111.5 . . ? C27 C28 H28A 111.5 . . ? Si1 C28 H28A 113.1 . . ? C29 C28 H28B 111.5 . . ? C27 C28 H28B 111.5 . . ? Si1 C28 H28B 137.6 . . ? H28A C28 H28B 109.3 . . ? C28 C29 Si1 87.55(10) . . ? C28 C29 H29A 114.1 . . ? Si1 C29 H29A 114.1 . . ? C28 C29 H29B 114.1 . . ? Si1 C29 H29B 114.1 . . ? H29A C29 H29B 111.2 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.374 _refine_diff_density_min -0.323 _refine_diff_density_rms 0.050 #===END #compound 1d data_gc247 _database_code_depnum_ccdc_archive 'CCDC 772841' #TrackingRef '- 2010_cortial_njc.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H26 Si' _chemical_formula_weight 450.63 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.389(1) _cell_length_b 10.038(1) _cell_length_c 12.922(1) _cell_angle_alpha 92.983(1) _cell_angle_beta 90.812(1) _cell_angle_gamma 99.215(1) _cell_volume 1200.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 3548 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.247 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 476 _exptl_absorpt_coefficient_mu 0.118 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9545 _exptl_absorpt_correction_T_max 0.9883 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _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 KappaCCD _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 13437 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 30.02 _reflns_number_total 6979 _reflns_number_gt 5451 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+0.1610P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6979 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0572 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.1176 _refine_ls_wR_factor_gt 0.1101 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.15945(3) 0.22198(3) 0.25887(2) 0.02447(9) Uani 1 1 d . . . C1 C 0.08992(13) 0.08938(11) 0.35416(9) 0.0277(2) Uani 1 1 d . . . H1 H -0.0157 0.0563 0.3428 0.033 Uiso 1 1 calc R . . C2 C 0.12269(13) 0.14839(11) 0.46381(9) 0.0298(2) Uani 1 1 d . . . C3 C 0.06644(15) 0.25062(13) 0.51835(10) 0.0373(3) Uani 1 1 d . . . H3 H -0.0061 0.2929 0.4878 0.045 Uiso 1 1 calc R . . C4 C 0.11889(16) 0.28972(13) 0.61880(11) 0.0422(3) Uani 1 1 d . . . H4 H 0.0817 0.3597 0.6567 0.051 Uiso 1 1 calc R . . C5 C 0.22370(17) 0.22860(13) 0.66400(10) 0.0432(3) Uani 1 1 d . . . H5 H 0.2592 0.2581 0.7319 0.052 Uiso 1 1 calc R . . C6 C 0.27785(16) 0.12444(13) 0.61125(10) 0.0389(3) Uani 1 1 d . . . H6 H 0.3486 0.0811 0.6430 0.047 Uiso 1 1 calc R . . C7 C 0.22663(14) 0.08455(11) 0.51087(9) 0.0316(3) Uani 1 1 d . . . C8 C 0.25836(14) -0.02469(11) 0.44021(9) 0.0311(3) Uani 1 1 d . . . C9 C 0.34695(16) -0.12120(12) 0.45319(11) 0.0408(3) Uani 1 1 d . . . H9 H 0.4042 -0.1192 0.5146 0.049 Uiso 1 1 calc R . . C10 C 0.35032(17) -0.22030(13) 0.37512(12) 0.0438(3) Uani 1 1 d . . . H10 H 0.4098 -0.2874 0.3834 0.053 Uiso 1 1 calc R . . C11 C 0.26782(16) -0.22279(12) 0.28484(11) 0.0386(3) Uani 1 1 d . . . H11 H 0.2713 -0.2918 0.2322 0.046 Uiso 1 1 calc R . . C12 C 0.18019(14) -0.12570(11) 0.27041(10) 0.0319(3) Uani 1 1 d . . . H12 H 0.1248 -0.1273 0.2081 0.038 Uiso 1 1 calc R . . C13 C 0.17495(13) -0.02622(11) 0.34864(9) 0.0284(2) Uani 1 1 d . . . C14 C 0.12779(12) 0.14780(11) 0.11962(9) 0.0258(2) Uani 1 1 d . . . H14 H 0.1764 0.0671 0.1067 0.031 Uiso 1 1 calc R . . C15 C -0.03310(13) 0.11503(11) 0.09742(9) 0.0266(2) Uani 1 1 d . . . C16 C -0.13652(13) 0.01520(11) 0.13497(9) 0.0302(2) Uani 1 1 d . . . H16 H -0.1090 -0.0489 0.1798 0.036 Uiso 1 1 calc R . . C17 C -0.28064(14) 0.01028(12) 0.10616(10) 0.0355(3) Uani 1 1 d . . . H17 H -0.3516 -0.0584 0.1309 0.043 Uiso 1 1 calc R . . C18 C -0.32221(14) 0.10457(13) 0.04168(11) 0.0374(3) Uani 1 1 d . . . H18 H -0.4214 0.1011 0.0242 0.045 Uiso 1 1 calc R . . C19 C -0.22024(14) 0.20335(12) 0.00278(10) 0.0341(3) Uani 1 1 d . . . H19 H -0.2488 0.2678 -0.0412 0.041 Uiso 1 1 calc R . . C20 C -0.07528(13) 0.20700(11) 0.02893(9) 0.0285(2) Uani 1 1 d . . . C21 C 0.05408(14) 0.29222(11) -0.00540(9) 0.0283(2) Uani 1 1 d . . . C22 C 0.07010(16) 0.39044(12) -0.07863(9) 0.0355(3) Uani 1 1 d . . . H22 H -0.0121 0.4152 -0.1116 0.043 Uiso 1 1 calc R . . C23 C 0.20695(17) 0.45102(12) -0.10241(10) 0.0400(3) Uani 1 1 d . . . H23 H 0.2192 0.5181 -0.1522 0.048 Uiso 1 1 calc R . . C24 C 0.32740(16) 0.41488(13) -0.05412(10) 0.0391(3) Uani 1 1 d . . . H24 H 0.4211 0.4565 -0.0723 0.047 Uiso 1 1 calc R . . C25 C 0.31288(14) 0.31845(12) 0.02066(10) 0.0331(3) Uani 1 1 d . . . H25 H 0.3955 0.2957 0.0545 0.040 Uiso 1 1 calc R . . C26 C 0.17527(13) 0.25654(11) 0.04452(9) 0.0272(2) Uani 1 1 d . . . C27 C 0.35552(12) 0.27944(11) 0.28897(9) 0.0256(2) Uani 1 1 d . . . C28 C 0.46188(13) 0.20149(12) 0.26311(10) 0.0314(3) Uani 1 1 d . . . H28 H 0.4348 0.1165 0.2263 0.038 Uiso 1 1 calc R . . C29 C 0.60610(14) 0.24522(13) 0.28991(10) 0.0357(3) Uani 1 1 d . . . H29 H 0.6764 0.1907 0.2710 0.043 Uiso 1 1 calc R . . C30 C 0.64754(14) 0.36799(13) 0.34411(10) 0.0356(3) Uani 1 1 d . . . H30 H 0.7461 0.3976 0.3629 0.043 Uiso 1 1 calc R . . C31 C 0.54524(15) 0.44729(13) 0.37079(12) 0.0401(3) Uani 1 1 d . . . H31 H 0.5733 0.5319 0.4079 0.048 Uiso 1 1 calc R . . C32 C 0.40149(14) 0.40354(12) 0.34344(11) 0.0359(3) Uani 1 1 d . . . H32 H 0.3322 0.4593 0.3622 0.043 Uiso 1 1 calc R . . C33 C 0.05969(14) 0.36809(12) 0.27173(10) 0.0350(3) Uani 1 1 d . . . H33A H 0.0764 0.4115 0.3415 0.053 Uiso 1 1 calc R . . H33B H -0.0438 0.3361 0.2601 0.053 Uiso 1 1 calc R . . H33C H 0.0940 0.4335 0.2203 0.053 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 Si1 0.02571(17) 0.02394(15) 0.02395(16) 0.00150(11) -0.00050(12) 0.00458(11) C1 0.0271(6) 0.0293(5) 0.0254(6) 0.0009(4) 0.0005(4) 0.0005(4) C2 0.0314(6) 0.0302(5) 0.0245(6) 0.0017(4) 0.0040(5) -0.0054(4) C3 0.0370(7) 0.0377(6) 0.0342(7) -0.0013(5) 0.0089(5) -0.0027(5) C4 0.0485(8) 0.0385(6) 0.0339(7) -0.0067(5) 0.0122(6) -0.0083(6) C5 0.0554(9) 0.0403(7) 0.0259(6) -0.0027(5) 0.0019(6) -0.0150(6) C6 0.0457(8) 0.0371(6) 0.0288(6) 0.0037(5) -0.0059(6) -0.0088(5) C7 0.0372(7) 0.0291(5) 0.0251(6) 0.0044(4) 0.0001(5) -0.0064(5) C8 0.0374(7) 0.0259(5) 0.0274(6) 0.0060(4) -0.0035(5) -0.0040(4) C9 0.0497(8) 0.0302(6) 0.0407(7) 0.0073(5) -0.0159(6) 0.0004(5) C10 0.0515(9) 0.0280(6) 0.0528(9) 0.0048(6) -0.0118(7) 0.0091(5) C11 0.0479(8) 0.0265(5) 0.0403(7) -0.0008(5) -0.0031(6) 0.0035(5) C12 0.0391(7) 0.0265(5) 0.0288(6) 0.0030(4) -0.0023(5) 0.0007(5) C13 0.0323(6) 0.0255(5) 0.0257(6) 0.0053(4) 0.0000(5) -0.0021(4) C14 0.0280(6) 0.0241(5) 0.0256(5) 0.0034(4) -0.0005(4) 0.0045(4) C15 0.0306(6) 0.0254(5) 0.0236(5) -0.0024(4) -0.0021(4) 0.0048(4) C16 0.0338(6) 0.0276(5) 0.0282(6) -0.0023(4) -0.0002(5) 0.0025(4) C17 0.0317(7) 0.0362(6) 0.0353(7) -0.0071(5) 0.0009(5) -0.0015(5) C18 0.0302(7) 0.0443(7) 0.0370(7) -0.0104(5) -0.0057(5) 0.0081(5) C19 0.0371(7) 0.0371(6) 0.0293(6) -0.0036(5) -0.0066(5) 0.0119(5) C20 0.0351(6) 0.0278(5) 0.0229(5) -0.0030(4) -0.0032(5) 0.0081(4) C21 0.0380(7) 0.0251(5) 0.0218(5) -0.0015(4) -0.0017(5) 0.0068(4) C22 0.0534(8) 0.0294(6) 0.0247(6) 0.0018(4) -0.0042(5) 0.0103(5) C23 0.0630(9) 0.0300(6) 0.0255(6) 0.0059(5) 0.0019(6) 0.0017(6) C24 0.0479(8) 0.0359(6) 0.0293(6) 0.0018(5) 0.0048(6) -0.0061(5) C25 0.0359(7) 0.0339(6) 0.0277(6) 0.0016(5) -0.0006(5) 0.0001(5) C26 0.0355(6) 0.0242(5) 0.0213(5) -0.0005(4) 0.0003(5) 0.0036(4) C27 0.0285(6) 0.0250(5) 0.0233(5) 0.0041(4) 0.0011(4) 0.0032(4) C28 0.0315(6) 0.0310(6) 0.0317(6) -0.0025(5) -0.0007(5) 0.0068(5) C29 0.0311(7) 0.0406(6) 0.0368(7) -0.0002(5) 0.0010(5) 0.0102(5) C30 0.0272(6) 0.0433(7) 0.0342(7) 0.0021(5) 0.0000(5) -0.0007(5) C31 0.0349(7) 0.0324(6) 0.0492(8) -0.0083(5) 0.0008(6) -0.0022(5) C32 0.0312(7) 0.0280(5) 0.0478(8) -0.0048(5) 0.0024(6) 0.0042(5) C33 0.0366(7) 0.0349(6) 0.0355(7) -0.0017(5) -0.0023(5) 0.0131(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 C33 1.8642(12) . ? Si1 C27 1.8679(12) . ? Si1 C1 1.9050(12) . ? Si1 C14 1.9119(12) . ? C1 C13 1.5095(16) . ? C1 C2 1.5149(16) . ? C1 H1 1.0000 . ? C2 C3 1.3919(17) . ? C2 C7 1.3990(18) . ? C3 C4 1.3959(19) . ? C3 H3 0.9500 . ? C4 C5 1.378(2) . ? C4 H4 0.9500 . ? C5 C6 1.386(2) . ? C5 H5 0.9500 . ? C6 C7 1.3930(17) . ? C6 H6 0.9500 . ? C7 C8 1.4605(17) . ? C8 C9 1.3891(18) . ? C8 C13 1.4077(16) . ? C9 C10 1.384(2) . ? C9 H9 0.9500 . ? C10 C11 1.388(2) . ? C10 H10 0.9500 . ? C11 C12 1.3903(18) . ? C11 H11 0.9500 . ? C12 C13 1.3906(16) . ? C12 H12 0.9500 . ? C14 C15 1.5136(16) . ? C14 C26 1.5161(15) . ? C14 H14 1.0000 . ? C15 C16 1.3910(16) . ? C15 C20 1.4088(15) . ? C16 C17 1.3908(18) . ? C16 H16 0.9500 . ? C17 C18 1.3906(19) . ? C17 H17 0.9500 . ? C18 C19 1.3835(19) . ? C18 H18 0.9500 . ? C19 C20 1.3920(17) . ? C19 H19 0.9500 . ? C20 C21 1.4579(17) . ? C21 C22 1.3942(16) . ? C21 C26 1.4046(17) . ? C22 C23 1.377(2) . ? C22 H22 0.9500 . ? C23 C24 1.391(2) . ? C23 H23 0.9500 . ? C24 C25 1.3957(17) . ? C24 H24 0.9500 . ? C25 C26 1.3874(17) . ? C25 H25 0.9500 . ? C27 C28 1.3978(16) . ? C27 C32 1.4005(16) . ? C28 C29 1.3880(18) . ? C28 H28 0.9500 . ? C29 C30 1.3819(18) . ? C29 H29 0.9500 . ? C30 C31 1.3787(18) . ? C30 H30 0.9500 . ? C31 C32 1.3856(18) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C33 Si1 C27 110.05(6) . . ? C33 Si1 C1 110.56(6) . . ? C27 Si1 C1 107.61(5) . . ? C33 Si1 C14 106.86(5) . . ? C27 Si1 C14 111.55(5) . . ? C1 Si1 C14 110.24(5) . . ? C13 C1 C2 102.36(9) . . ? C13 C1 Si1 111.18(8) . . ? C2 C1 Si1 109.24(7) . . ? C13 C1 H1 111.2 . . ? C2 C1 H1 111.2 . . ? Si1 C1 H1 111.2 . . ? C3 C2 C7 119.99(12) . . ? C3 C2 C1 129.93(12) . . ? C7 C2 C1 110.08(10) . . ? C2 C3 C4 118.62(13) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C5 C4 C3 121.17(13) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 119.4 . . ? C4 C5 C6 120.63(13) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C5 C6 C7 118.80(13) . . ? C5 C6 H6 120.6 . . ? C7 C6 H6 120.6 . . ? C6 C7 C2 120.76(12) . . ? C6 C7 C8 130.49(12) . . ? C2 C7 C8 108.68(10) . . ? C9 C8 C13 120.69(11) . . ? C9 C8 C7 130.70(12) . . ? C13 C8 C7 108.54(11) . . ? C10 C9 C8 118.86(12) . . ? C10 C9 H9 120.6 . . ? C8 C9 H9 120.6 . . ? C9 C10 C11 120.74(12) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C10 C11 C12 120.91(12) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C11 C12 C13 118.91(12) . . ? C11 C12 H12 120.5 . . ? C13 C12 H12 120.5 . . ? C12 C13 C8 119.88(11) . . ? C12 C13 C1 130.16(11) . . ? C8 C13 C1 109.96(10) . . ? C15 C14 C26 102.22(9) . . ? C15 C14 Si1 108.81(8) . . ? C26 C14 Si1 109.72(7) . . ? C15 C14 H14 111.9 . . ? C26 C14 H14 111.9 . . ? Si1 C14 H14 111.9 . . ? C16 C15 C20 119.64(11) . . ? C16 C15 C14 130.36(10) . . ? C20 C15 C14 109.99(10) . . ? C17 C16 C15 119.20(11) . . ? C17 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? C18 C17 C16 120.85(12) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C19 C18 C17 120.51(12) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C18 C19 C20 119.10(12) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? C19 C20 C15 120.61(11) . . ? C19 C20 C21 130.93(11) . . ? C15 C20 C21 108.44(10) . . ? C22 C21 C26 120.71(12) . . ? C22 C21 C20 130.34(12) . . ? C26 C21 C20 108.87(10) . . ? C23 C22 C21 118.98(12) . . ? C23 C22 H22 120.5 . . ? C21 C22 H22 120.5 . . ? C22 C23 C24 120.54(11) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C23 C24 C25 121.10(13) . . ? C23 C24 H24 119.5 . . ? C25 C24 H24 119.5 . . ? C26 C25 C24 118.60(12) . . ? C26 C25 H25 120.7 . . ? C24 C25 H25 120.7 . . ? C25 C26 C21 120.06(11) . . ? C25 C26 C14 130.00(11) . . ? C21 C26 C14 109.94(10) . . ? C28 C27 C32 116.77(11) . . ? C28 C27 Si1 123.07(9) . . ? C32 C27 Si1 120.12(9) . . ? C29 C28 C27 121.57(11) . . ? C29 C28 H28 119.2 . . ? C27 C28 H28 119.2 . . ? C30 C29 C28 120.11(11) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C31 C30 C29 119.74(12) . . ? C31 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C30 C31 C32 119.95(12) . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C31 C32 C27 121.86(11) . . ? C31 C32 H32 119.1 . . ? C27 C32 H32 119.1 . . ? Si1 C33 H33A 109.5 . . ? Si1 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si1 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.258 _refine_diff_density_min -0.308 _refine_diff_density_rms 0.041 #===END #compound 3a data_gc436 _database_code_depnum_ccdc_archive 'CCDC 772842' #TrackingRef '- 2010_cortial_njc.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H34 B Nd O Si' _chemical_formula_weight 617.73 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' Nd Nd -0.1943 3.0179 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P212121 ' 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 9.400(1) _cell_length_b 11.887(1) _cell_length_c 24.070(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2689.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 33750 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.526 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1252 _exptl_absorpt_coefficient_mu 1.999 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7149 _exptl_absorpt_correction_T_max 0.8895 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _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 KappaCCD _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 23520 _diffrn_reflns_av_R_equivalents 0.0616 _diffrn_reflns_av_sigmaI/netI 0.0717 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 30.01 _reflns_number_total 7719 _reflns_number_gt 6287 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0777P)^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 -0.013(18) _refine_ls_number_reflns 7719 _refine_ls_number_parameters 339 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0548 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.1367 _refine_ls_wR_factor_gt 0.0913 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.17906(3) 0.47383(2) 0.359218(12) 0.02292(9) Uani 1 1 d . . . Si1 Si 0.50296(18) 0.41669(14) 0.41831(7) 0.0248(3) Uani 1 1 d . . . O1 O -0.0212(5) 0.6017(4) 0.37280(18) 0.0348(11) Uani 1 1 d . . . C1 C 0.4551(6) 0.5297(6) 0.3678(2) 0.0276(11) Uani 1 1 d . . . C2 C 0.3856(7) 0.6337(5) 0.3819(3) 0.0274(13) Uani 1 1 d . . . C3 C 0.3693(7) 0.6916(5) 0.4327(3) 0.0320(14) Uani 1 1 d . . . H3 H 0.4082 0.6618 0.4660 0.038 Uiso 1 1 calc R . . C4 C 0.2966(8) 0.7915(5) 0.4332(3) 0.0397(17) Uani 1 1 d . . . H4 H 0.2864 0.8302 0.4676 0.048 Uiso 1 1 calc R . . C5 C 0.2368(8) 0.8391(6) 0.3854(3) 0.0405(17) Uani 1 1 d . . . H5 H 0.1880 0.9089 0.3880 0.049 Uiso 1 1 calc R . . C6 C 0.2476(7) 0.7872(5) 0.3362(3) 0.0324(14) Uani 1 1 d . . . H6 H 0.2070 0.8191 0.3037 0.039 Uiso 1 1 calc R . . C7 C 0.3216(8) 0.6834(5) 0.3340(2) 0.0276(12) Uani 1 1 d . . . C8 C 0.3524(7) 0.6105(5) 0.2879(2) 0.0290(14) Uani 1 1 d . . . C9 C 0.3163(8) 0.6206(6) 0.2316(2) 0.0351(14) Uani 1 1 d . . . H9 H 0.2591 0.6812 0.2188 0.042 Uiso 1 1 calc R . . C10 C 0.3663(8) 0.5404(7) 0.1957(3) 0.0456(18) Uani 1 1 d . . . H10 H 0.3439 0.5455 0.1573 0.055 Uiso 1 1 calc R . . C11 C 0.4507(8) 0.4500(6) 0.2150(3) 0.0414(18) Uani 1 1 d . . . H11 H 0.4847 0.3964 0.1889 0.050 Uiso 1 1 calc R . . C12 C 0.4855(8) 0.4368(6) 0.2701(3) 0.0348(15) Uani 1 1 d . . . H12 H 0.5407 0.3744 0.2820 0.042 Uiso 1 1 calc R . . C13 C 0.4375(6) 0.5180(6) 0.3083(2) 0.0267(12) Uani 1 1 d . . . C14 C 0.6376(7) 0.3163(6) 0.3895(3) 0.0350(15) Uani 1 1 d . . . H14A H 0.6513 0.2539 0.4156 0.052 Uiso 1 1 calc R . . H14B H 0.7281 0.3556 0.3840 0.052 Uiso 1 1 calc R . . H14C H 0.6038 0.2868 0.3538 0.052 Uiso 1 1 calc R . . C15 C 0.5847(7) 0.4729(6) 0.4831(2) 0.0327(13) Uani 1 1 d . . . H15A H 0.5131 0.5150 0.5042 0.049 Uiso 1 1 calc R . . H15B H 0.6638 0.5229 0.4735 0.049 Uiso 1 1 calc R . . H15C H 0.6202 0.4103 0.5057 0.049 Uiso 1 1 calc R . . C16 C 0.3279(7) 0.3504(5) 0.4313(2) 0.0241(11) Uani 1 1 d . . . C17 C 0.2571(7) 0.2653(5) 0.3961(2) 0.0271(13) Uani 1 1 d . . . C18 C 0.3084(7) 0.1934(5) 0.3527(2) 0.0296(12) Uani 1 1 d . . . H18 H 0.4055 0.1963 0.3419 0.036 Uiso 1 1 calc R . . C19 C 0.2158(8) 0.1194(5) 0.3266(3) 0.0348(15) Uani 1 1 d . . . H19 H 0.2514 0.0712 0.2984 0.042 Uiso 1 1 calc R . . C20 C 0.0727(8) 0.1138(5) 0.3406(3) 0.0354(16) Uani 1 1 d . . . H20 H 0.0127 0.0618 0.3218 0.042 Uiso 1 1 calc R . . C21 C 0.0163(8) 0.1821(5) 0.3810(3) 0.0311(14) Uani 1 1 d . . . H21 H -0.0818 0.1776 0.3903 0.037 Uiso 1 1 calc R . . C22 C 0.1077(7) 0.2603(5) 0.4088(2) 0.0254(13) Uani 1 1 d . . . C23 C 0.0809(7) 0.3400(5) 0.4541(3) 0.0261(12) Uani 1 1 d . . . C24 C -0.0401(7) 0.3620(5) 0.4850(3) 0.0304(13) Uani 1 1 d . . . H24 H -0.1269 0.3243 0.4770 0.036 Uiso 1 1 calc R . . C25 C -0.0329(8) 0.4396(5) 0.5275(3) 0.0332(14) Uani 1 1 d . . . H25 H -0.1151 0.4545 0.5493 0.040 Uiso 1 1 calc R . . C26 C 0.0951(7) 0.4969(5) 0.5391(2) 0.0287(13) Uani 1 1 d . . . H26 H 0.0967 0.5525 0.5675 0.034 Uiso 1 1 calc R . . C27 C 0.2161(7) 0.4741(6) 0.5103(2) 0.0288(12) Uani 1 1 d . . . H27 H 0.3012 0.5134 0.5192 0.035 Uiso 1 1 calc R . . C28 C 0.2174(7) 0.3926(5) 0.4673(2) 0.0249(12) Uani 1 1 d . . . C29 C -0.1207(10) 0.6362(8) 0.3268(3) 0.054(2) Uani 1 1 d . . . H29A H -0.0671 0.6717 0.2960 0.064 Uiso 1 1 calc R . . H29B H -0.1723 0.5700 0.3121 0.064 Uiso 1 1 calc R . . C30 C -0.2222(9) 0.7183(8) 0.3519(3) 0.055(2) Uani 1 1 d . . . H30A H -0.2441 0.7800 0.3256 0.066 Uiso 1 1 calc R . . H30B H -0.3120 0.6808 0.3628 0.066 Uiso 1 1 calc R . . C31 C -0.1452(12) 0.7612(9) 0.4013(5) 0.088(4) Uani 1 1 d . . . H31A H -0.2133 0.7865 0.4301 0.106 Uiso 1 1 calc R . . H31B H -0.0835 0.8254 0.3910 0.106 Uiso 1 1 calc R . . C32 C -0.0547(9) 0.6620(7) 0.4231(3) 0.0458(18) Uani 1 1 d . . . H32A H 0.0325 0.6890 0.4419 0.055 Uiso 1 1 calc R . . H32B H -0.1097 0.6145 0.4492 0.055 Uiso 1 1 calc R . . B1 B 0.0458(3) 0.4018(3) 0.26978(13) 0.0401(19) Uani 1 1 d D . . H1A H 0.0030(18) 0.389(4) 0.2346(5) 0.048 Uiso 1 1 d D . . H1B H 0.125(3) 0.353(3) 0.2741(16) 0.048 Uiso 1 1 d D . . H1C H -0.023(2) 0.387(4) 0.2978(8) 0.048 Uiso 1 1 d D . . H1D H 0.075(5) 0.4782(12) 0.272(2) 0.048 Uiso 1 1 d 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 Nd1 0.02255(14) 0.02309(13) 0.02312(14) 0.00235(13) -0.00238(13) 0.00015(13) Si1 0.0226(8) 0.0253(7) 0.0266(8) -0.0010(7) -0.0037(7) 0.0015(6) O1 0.035(3) 0.038(2) 0.032(2) 0.0044(19) 0.003(2) 0.008(2) C1 0.021(3) 0.036(3) 0.026(3) 0.001(3) 0.000(2) -0.002(3) C2 0.026(3) 0.026(3) 0.031(3) 0.000(2) -0.002(3) -0.007(3) C3 0.037(4) 0.029(3) 0.030(3) 0.000(3) -0.004(3) 0.000(3) C4 0.044(5) 0.031(3) 0.044(4) -0.008(3) 0.005(3) 0.004(3) C5 0.035(4) 0.027(3) 0.059(5) -0.001(3) -0.003(4) 0.002(3) C6 0.027(3) 0.026(3) 0.044(4) 0.010(3) -0.001(3) 0.000(3) C7 0.029(3) 0.027(3) 0.027(3) 0.002(2) -0.003(3) -0.006(3) C8 0.027(3) 0.034(3) 0.026(3) 0.006(2) 0.004(2) -0.008(2) C9 0.036(4) 0.044(3) 0.026(3) 0.011(3) 0.003(3) -0.007(3) C10 0.046(4) 0.065(5) 0.026(3) 0.006(3) -0.001(3) -0.013(4) C11 0.044(4) 0.051(4) 0.029(3) -0.006(3) 0.009(3) -0.007(3) C12 0.034(4) 0.036(3) 0.035(3) -0.001(3) 0.002(3) -0.002(3) C13 0.025(3) 0.032(3) 0.023(2) 0.005(3) 0.001(2) -0.005(3) C14 0.032(4) 0.034(3) 0.039(4) -0.004(3) -0.004(3) 0.002(3) C15 0.031(3) 0.034(3) 0.033(3) 0.001(3) -0.006(3) -0.007(3) C16 0.021(3) 0.025(2) 0.026(3) 0.004(2) -0.004(3) 0.001(2) C17 0.033(4) 0.024(3) 0.025(3) 0.005(2) -0.003(3) 0.005(3) C18 0.036(3) 0.028(3) 0.025(3) -0.001(2) 0.004(3) 0.004(3) C19 0.043(4) 0.025(3) 0.036(3) -0.003(3) -0.009(3) 0.004(3) C20 0.046(4) 0.020(3) 0.040(3) 0.000(2) -0.019(3) -0.004(3) C21 0.033(4) 0.025(3) 0.035(3) 0.006(3) -0.011(3) -0.006(3) C22 0.029(3) 0.020(3) 0.027(3) 0.006(2) -0.006(3) -0.001(2) C23 0.022(3) 0.025(3) 0.030(3) 0.008(2) 0.001(3) -0.001(2) C24 0.024(3) 0.031(3) 0.036(3) 0.008(3) 0.002(3) 0.001(3) C25 0.033(4) 0.035(3) 0.032(3) 0.006(3) 0.008(3) 0.004(3) C26 0.032(3) 0.029(3) 0.025(3) -0.003(2) 0.000(3) 0.002(2) C27 0.028(3) 0.031(3) 0.027(3) -0.004(3) -0.003(2) 0.000(3) C28 0.027(3) 0.021(2) 0.026(3) 0.005(2) -0.004(2) 0.003(2) C29 0.057(5) 0.060(5) 0.043(4) 0.003(4) -0.011(4) 0.030(4) C30 0.044(4) 0.068(5) 0.053(5) 0.007(4) 0.002(4) 0.025(4) C31 0.072(8) 0.062(6) 0.132(10) 0.006(6) 0.024(7) 0.041(6) C32 0.044(4) 0.049(4) 0.044(4) -0.012(4) 0.007(4) 0.012(3) B1 0.045(5) 0.037(4) 0.038(4) -0.004(3) -0.014(4) -0.004(4) _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 Nd1 O1 2.441(5) . ? Nd1 B1 2.634(3) . ? Nd1 C16 2.668(6) . ? Nd1 C1 2.687(6) . ? Nd1 C17 2.733(6) . ? Nd1 C2 2.770(6) . ? Nd1 C13 2.771(6) . ? Nd1 C28 2.799(5) . ? Nd1 C8 2.871(6) . ? Nd1 C22 2.884(6) . ? Nd1 C7 2.892(6) . ? Nd1 C23 2.933(6) . ? Nd1 H1B 2.55(4) . ? Nd1 H1C 2.62(3) . ? Nd1 H1D 2.32(5) . ? Si1 C16 1.851(7) . ? Si1 C15 1.862(6) . ? Si1 C1 1.866(6) . ? Si1 C14 1.873(7) . ? O1 C32 1.442(8) . ? O1 C29 1.507(8) . ? C1 C2 1.438(9) . ? C1 C13 1.450(8) . ? C2 C3 1.413(9) . ? C2 C7 1.427(8) . ? C3 C4 1.369(9) . ? C3 H3 0.9500 . ? C4 C5 1.400(10) . ? C4 H4 0.9500 . ? C5 C6 1.340(10) . ? C5 H5 0.9500 . ? C6 C7 1.418(9) . ? C6 H6 0.9500 . ? C7 C8 1.437(9) . ? C8 C9 1.402(8) . ? C8 C13 1.445(9) . ? C9 C10 1.370(10) . ? C9 H9 0.9500 . ? C10 C11 1.414(11) . ? C10 H10 0.9500 . ? C11 C12 1.374(9) . ? C11 H11 0.9500 . ? C12 C13 1.407(9) . ? C12 H12 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C28 1.443(9) . ? C16 C17 1.477(8) . ? C17 C18 1.433(8) . ? C17 C22 1.439(9) . ? C18 C19 1.387(9) . ? C18 H18 0.9500 . ? C19 C20 1.388(10) . ? C19 H19 0.9500 . ? C20 C21 1.373(10) . ? C20 H20 0.9500 . ? C21 C22 1.432(8) . ? C21 H21 0.9500 . ? C22 C23 1.467(9) . ? C23 C24 1.384(9) . ? C23 C28 1.462(9) . ? C24 C25 1.379(9) . ? C24 H24 0.9500 . ? C25 C26 1.411(9) . ? C25 H25 0.9500 . ? C26 C27 1.359(9) . ? C26 H26 0.9500 . ? C27 C28 1.418(8) . ? C27 H27 0.9500 . ? C29 C30 1.493(11) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.483(15) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.546(12) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? B1 H1A 0.95000(11) . ? B1 H1B 0.95000(18) . ? B1 H1C 0.95000(13) . ? B1 H1D 0.9500(3) . ? 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 O1 Nd1 B1 86.87(13) . . ? O1 Nd1 C16 131.27(17) . . ? B1 Nd1 C16 127.01(14) . . ? O1 Nd1 C1 125.47(19) . . ? B1 Nd1 C1 127.08(14) . . ? C16 Nd1 C1 65.12(18) . . ? O1 Nd1 C17 136.74(18) . . ? B1 Nd1 C17 95.65(15) . . ? C16 Nd1 C17 31.71(18) . . ? C1 Nd1 C17 86.5(2) . . ? O1 Nd1 C2 94.97(18) . . ? B1 Nd1 C2 135.81(15) . . ? C16 Nd1 C2 83.21(18) . . ? C1 Nd1 C2 30.51(19) . . ? C17 Nd1 C2 111.71(19) . . ? O1 Nd1 C13 128.11(17) . . ? B1 Nd1 C13 96.70(14) . . ? C16 Nd1 C13 86.10(19) . . ? C1 Nd1 C13 30.77(16) . . ? C17 Nd1 C13 94.6(2) . . ? C2 Nd1 C13 48.94(19) . . ? O1 Nd1 C28 100.93(16) . . ? B1 Nd1 C28 135.15(14) . . ? C16 Nd1 C28 30.49(18) . . ? C1 Nd1 C28 83.64(17) . . ? C17 Nd1 C28 49.49(17) . . ? C2 Nd1 C28 87.91(18) . . ? C13 Nd1 C28 111.34(17) . . ? O1 Nd1 C8 99.51(17) . . ? B1 Nd1 C8 88.01(14) . . ? C16 Nd1 C8 113.7(2) . . ? C1 Nd1 C8 50.05(18) . . ? C17 Nd1 C8 123.7(2) . . ? C2 Nd1 C8 48.07(17) . . ? C13 Nd1 C8 29.62(18) . . ? C28 Nd1 C8 132.69(18) . . ? O1 Nd1 C22 108.26(18) . . ? B1 Nd1 C22 86.65(14) . . ? C16 Nd1 C22 50.87(18) . . ? C1 Nd1 C22 114.22(19) . . ? C17 Nd1 C22 29.52(18) . . ? C2 Nd1 C22 133.24(17) . . ? C13 Nd1 C22 123.61(19) . . ? C28 Nd1 C22 48.81(17) . . ? C8 Nd1 C22 151.35(19) . . ? O1 Nd1 C7 81.31(18) . . ? B1 Nd1 C7 109.20(13) . . ? C16 Nd1 C7 111.52(18) . . ? C1 Nd1 C7 49.90(19) . . ? C17 Nd1 C7 136.4(2) . . ? C2 Nd1 C7 29.09(17) . . ? C13 Nd1 C7 48.56(19) . . ? C28 Nd1 C7 115.63(17) . . ? C8 Nd1 C7 28.88(17) . . ? C22 Nd1 C7 162.24(18) . . ? O1 Nd1 C23 89.49(16) . . ? B1 Nd1 C23 108.11(14) . . ? C16 Nd1 C23 50.22(19) . . ? C1 Nd1 C23 112.19(17) . . ? C17 Nd1 C23 48.66(18) . . ? C2 Nd1 C23 116.04(18) . . ? C13 Nd1 C23 136.30(17) . . ? C28 Nd1 C23 29.43(17) . . ? C8 Nd1 C23 162.03(17) . . ? C22 Nd1 C23 29.19(17) . . ? C7 Nd1 C23 140.91(17) . . ? O1 Nd1 H1B 107.7(2) . . ? B1 Nd1 H1B 21.04(9) . . ? C16 Nd1 H1B 108.5(5) . . ? C1 Nd1 H1B 113.1(8) . . ? C17 Nd1 H1B 78.7(6) . . ? C2 Nd1 H1B 133.1(10) . . ? C13 Nd1 H1B 85.7(9) . . ? C28 Nd1 H1B 125.3(9) . . ? C8 Nd1 H1B 87.2(11) . . ? C22 Nd1 H1B 77.9(10) . . ? C7 Nd1 H1B 114.1(10) . . ? C23 Nd1 H1B 104.9(10) . . ? O1 Nd1 H1C 76.3(10) . . ? B1 Nd1 H1C 20.84(11) . . ? C16 Nd1 H1C 122.0(10) . . ? C1 Nd1 H1C 147.3(4) . . ? C17 Nd1 H1C 91.1(11) . . ? C2 Nd1 H1C 152.8(8) . . ? C13 Nd1 H1C 117.4(2) . . ? C28 Nd1 H1C 118.8(6) . . ? C8 Nd1 H1C 107.3(4) . . ? C22 Nd1 H1C 73.6(9) . . ? C7 Nd1 H1C 123.9(8) . . ? C23 Nd1 H1C 89.9(5) . . ? H1B Nd1 H1C 35.0(4) . . ? O1 Nd1 H1D 77.4(11) . . ? B1 Nd1 H1D 20.89(19) . . ? C16 Nd1 H1D 145.4(7) . . ? C1 Nd1 H1D 118.2(10) . . ? C17 Nd1 H1D 115.3(5) . . ? C2 Nd1 H1D 117.3(5) . . ? C13 Nd1 H1D 88.0(11) . . ? C28 Nd1 H1D 154.8(6) . . ? C8 Nd1 H1D 71.6(8) . . ? C22 Nd1 H1D 107.3(3) . . ? C7 Nd1 H1D 89.2(4) . . ? C23 Nd1 H1D 125.8(7) . . ? H1B Nd1 H1D 37.0(3) . . ? H1C Nd1 H1D 36.0(3) . . ? C16 Si1 C15 112.2(3) . . ? C16 Si1 C1 101.6(3) . . ? C15 Si1 C1 112.7(3) . . ? C16 Si1 C14 113.1(3) . . ? C15 Si1 C14 105.1(3) . . ? C1 Si1 C14 112.4(3) . . ? C16 Si1 Nd1 50.56(17) . . ? C15 Si1 Nd1 130.0(2) . . ? C1 Si1 Nd1 51.19(18) . . ? C14 Si1 Nd1 124.9(2) . . ? C32 O1 C29 110.3(5) . . ? C32 O1 Nd1 126.2(4) . . ? C29 O1 Nd1 123.3(4) . . ? C2 C1 C13 105.2(5) . . ? C2 C1 Si1 125.1(4) . . ? C13 C1 Si1 127.0(5) . . ? C2 C1 Nd1 78.0(3) . . ? C13 C1 Nd1 77.8(3) . . ? Si1 C1 Nd1 96.0(2) . . ? C3 C2 C7 116.9(6) . . ? C3 C2 C1 132.2(6) . . ? C7 C2 C1 111.0(5) . . ? C3 C2 Nd1 115.4(4) . . ? C7 C2 Nd1 80.2(4) . . ? C1 C2 Nd1 71.5(3) . . ? C4 C3 C2 119.0(6) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 122.9(6) . . ? C3 C4 H4 118.6 . . ? C5 C4 H4 118.6 . . ? C6 C5 C4 120.7(6) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 118.0(6) . . ? C5 C6 H6 121.0 . . ? C7 C6 H6 121.0 . . ? C6 C7 C2 122.5(6) . . ? C6 C7 C8 130.7(6) . . ? C2 C7 C8 106.8(5) . . ? C6 C7 Nd1 121.0(5) . . ? C2 C7 Nd1 70.7(3) . . ? C8 C7 Nd1 74.7(3) . . ? C9 C8 C7 130.2(6) . . ? C9 C8 C13 121.8(6) . . ? C7 C8 C13 108.0(5) . . ? C9 C8 Nd1 119.3(4) . . ? C7 C8 Nd1 76.4(3) . . ? C13 C8 Nd1 71.4(3) . . ? C10 C9 C8 117.8(7) . . ? C10 C9 H9 121.1 . . ? C8 C9 H9 121.1 . . ? C9 C10 C11 121.0(6) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? C12 C11 C10 122.4(7) . . ? C12 C11 H11 118.8 . . ? C10 C11 H11 118.8 . . ? C11 C12 C13 118.4(7) . . ? C11 C12 H12 120.8 . . ? C13 C12 H12 120.8 . . ? C12 C13 C8 118.5(5) . . ? C12 C13 C1 132.5(6) . . ? C8 C13 C1 109.0(6) . . ? C12 C13 Nd1 116.2(4) . . ? C8 C13 Nd1 79.0(3) . . ? C1 C13 Nd1 71.4(3) . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C28 C16 C17 105.0(5) . . ? C28 C16 Si1 126.4(4) . . ? C17 C16 Si1 126.5(5) . . ? C28 C16 Nd1 79.8(3) . . ? C17 C16 Nd1 76.6(3) . . ? Si1 C16 Nd1 97.0(2) . . ? C18 C17 C22 117.3(6) . . ? C18 C17 C16 132.4(6) . . ? C22 C17 C16 110.3(6) . . ? C18 C17 Nd1 113.3(4) . . ? C22 C17 Nd1 81.1(4) . . ? C16 C17 Nd1 71.7(3) . . ? C19 C18 C17 119.8(6) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C20 122.0(6) . . ? C18 C19 H19 119.0 . . ? C20 C19 H19 119.0 . . ? C21 C20 C19 121.1(6) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C20 C21 C22 118.9(7) . . ? C20 C21 H21 120.6 . . ? C22 C21 H21 120.6 . . ? C21 C22 C17 120.9(6) . . ? C21 C22 C23 131.6(6) . . ? C17 C22 C23 107.4(5) . . ? C21 C22 Nd1 121.1(4) . . ? C17 C22 Nd1 69.4(3) . . ? C23 C22 Nd1 77.3(3) . . ? C24 C23 C28 121.6(6) . . ? C24 C23 C22 131.5(6) . . ? C28 C23 C22 106.7(5) . . ? C24 C23 Nd1 125.0(4) . . ? C28 C23 Nd1 70.2(3) . . ? C22 C23 Nd1 73.6(3) . . ? C25 C24 C23 119.0(6) . . ? C25 C24 H24 120.5 . . ? C23 C24 H24 120.5 . . ? C24 C25 C26 120.7(6) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C27 C26 C25 121.2(6) . . ? C27 C26 H26 119.4 . . ? C25 C26 H26 119.4 . . ? C26 C27 C28 121.0(6) . . ? C26 C27 H27 119.5 . . ? C28 C27 H27 119.5 . . ? C27 C28 C16 133.0(6) . . ? C27 C28 C23 116.3(6) . . ? C16 C28 C23 110.7(5) . . ? C27 C28 Nd1 116.2(4) . . ? C16 C28 Nd1 69.7(3) . . ? C23 C28 Nd1 80.4(3) . . ? C30 C29 O1 106.1(6) . . ? C30 C29 H29A 110.5 . . ? O1 C29 H29A 110.5 . . ? C30 C29 H29B 110.5 . . ? O1 C29 H29B 110.5 . . ? H29A C29 H29B 108.7 . . ? C31 C30 C29 103.7(7) . . ? C31 C30 H30A 111.0 . . ? C29 C30 H30A 111.0 . . ? C31 C30 H30B 111.0 . . ? C29 C30 H30B 111.0 . . ? H30A C30 H30B 109.0 . . ? C30 C31 C32 106.2(8) . . ? C30 C31 H31A 110.5 . . ? C32 C31 H31A 110.5 . . ? C30 C31 H31B 110.5 . . ? C32 C31 H31B 110.5 . . ? H31A C31 H31B 108.7 . . ? O1 C32 C31 102.4(7) . . ? O1 C32 H32A 111.3 . . ? C31 C32 H32A 111.3 . . ? O1 C32 H32B 111.3 . . ? C31 C32 H32B 111.3 . . ? H32A C32 H32B 109.2 . . ? Nd1 B1 H1A 169(3) . . ? Nd1 B1 H1B 75(2) . . ? H1A B1 H1B 109.4(10) . . ? Nd1 B1 H1C 78.7(18) . . ? H1A B1 H1C 108.3(9) . . ? H1B B1 H1C 109.9(10) . . ? Nd1 B1 H1D 60(3) . . ? H1A B1 H1D 108.9(10) . . ? H1B B1 H1D 110.5(10) . . ? H1C B1 H1D 109.7(10) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.090 _refine_diff_density_min -1.944 _refine_diff_density_rms 0.410 #===END #compound 3b data_gc289 _database_code_depnum_ccdc_archive 'CCDC 772843' #TrackingRef '- 2010_cortial_njc.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety C34H38BNdOSi,1/2(C7H8) _chemical_formula_sum 'C37.50 H42 B Nd O Si' _chemical_formula_weight 691.85 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' Nd Nd -0.1943 3.0179 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1980(10) _cell_length_b 11.5630(10) _cell_length_c 15.3250(10) _cell_angle_alpha 97.9190(10) _cell_angle_beta 93.6290(10) _cell_angle_gamma 93.8530(10) _cell_volume 1606.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 5953 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description needle _exptl_crystal_colour 'redish orange' _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 708 _exptl_absorpt_coefficient_mu 1.682 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6984 _exptl_absorpt_correction_T_max 0.8499 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _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 KappaCCD _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 20537 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0373 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 30.05 _reflns_number_total 9365 _reflns_number_gt 8485 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0460P)^2^+0.3955P] 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 SHELXL _refine_ls_extinction_coef 0.0021(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9365 _refine_ls_number_parameters 402 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0320 _refine_ls_R_factor_gt 0.0275 _refine_ls_wR_factor_ref 0.0792 _refine_ls_wR_factor_gt 0.0729 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.179643(10) 0.174761(9) 0.320469(6) 0.02174(5) Uani 1 1 d . . . Si1 Si -0.00989(6) 0.31640(5) 0.17349(3) 0.02074(11) Uani 1 1 d . . . O1 O 0.28334(18) -0.01379(16) 0.31198(13) 0.0398(4) Uani 1 1 d . A . C1 C 0.1908(2) 0.30513(17) 0.19161(12) 0.0203(3) Uani 1 1 d . . . C2 C 0.2700(2) 0.20634(17) 0.15774(12) 0.0211(4) Uani 1 1 d . . . C3 C 0.2319(2) 0.10921(18) 0.09059(13) 0.0250(4) Uani 1 1 d . . . H3 H 0.1386 0.1014 0.0590 0.030 Uiso 1 1 calc R . . C4 C 0.3304(2) 0.0267(2) 0.07157(15) 0.0309(5) Uani 1 1 d . . . H4 H 0.3041 -0.0373 0.0262 0.037 Uiso 1 1 calc R . . C5 C 0.4690(3) 0.0342(2) 0.11724(16) 0.0322(5) Uani 1 1 d . . . H5 H 0.5349 -0.0240 0.1023 0.039 Uiso 1 1 calc R . . C6 C 0.5093(2) 0.1255(2) 0.18344(15) 0.0292(4) Uani 1 1 d . . . H6 H 0.6029 0.1310 0.2143 0.035 Uiso 1 1 calc R . . C7 C 0.4103(2) 0.21095(18) 0.20503(13) 0.0232(4) Uani 1 1 d . . . C8 C 0.4239(2) 0.31539(18) 0.26832(13) 0.0234(4) Uani 1 1 d . . . C9 C 0.5416(2) 0.3646(2) 0.32871(15) 0.0311(5) Uani 1 1 d . . . H9 H 0.6290 0.3258 0.3333 0.037 Uiso 1 1 calc R . . C10 C 0.5280(3) 0.4692(2) 0.38056(16) 0.0346(5) Uani 1 1 d . . . H10 H 0.6070 0.5039 0.4207 0.042 Uiso 1 1 calc R . . C11 C 0.3973(3) 0.5256(2) 0.37458(15) 0.0324(5) Uani 1 1 d . . . H11 H 0.3893 0.5975 0.4117 0.039 Uiso 1 1 calc R . . C12 C 0.2809(2) 0.47949(19) 0.31656(14) 0.0273(4) Uani 1 1 d . . . H12 H 0.1936 0.5188 0.3146 0.033 Uiso 1 1 calc R . . C13 C 0.2914(2) 0.37282(17) 0.25939(13) 0.0219(4) Uani 1 1 d . . . C14 C -0.0825(2) 0.21994(18) 0.25172(12) 0.0206(4) Uani 1 1 d . . . C15 C -0.0932(2) 0.25189(18) 0.34597(13) 0.0235(4) Uani 1 1 d . . . C16 C -0.0938(2) 0.3628(2) 0.39925(14) 0.0286(4) Uani 1 1 d . . . H16 H -0.0830 0.4328 0.3735 0.034 Uiso 1 1 calc R . . C17 C -0.1100(3) 0.3680(2) 0.48816(15) 0.0357(5) Uani 1 1 d . . . H17 H -0.1132 0.4423 0.5230 0.043 Uiso 1 1 calc R . . C18 C -0.1220(3) 0.2667(2) 0.52916(16) 0.0392(6) Uani 1 1 d . . . H18 H -0.1321 0.2735 0.5909 0.047 Uiso 1 1 calc R . . C19 C -0.1193(3) 0.1580(2) 0.48080(15) 0.0340(5) Uani 1 1 d . . . H19 H -0.1265 0.0895 0.5087 0.041 Uiso 1 1 calc R . . C20 C -0.1057(2) 0.14938(19) 0.38881(13) 0.0248(4) Uani 1 1 d . . . C21 C -0.1081(2) 0.04943(19) 0.32155(13) 0.0239(4) Uani 1 1 d . . . C22 C -0.1313(2) -0.0712(2) 0.32622(15) 0.0303(4) Uani 1 1 d . . . H22 H -0.1377 -0.0985 0.3817 0.036 Uiso 1 1 calc R . . C23 C -0.1445(3) -0.1485(2) 0.24958(17) 0.0355(5) Uani 1 1 d . . . H23 H -0.1622 -0.2299 0.2518 0.043 Uiso 1 1 calc R . . C24 C -0.1320(3) -0.1084(2) 0.16755(16) 0.0334(5) Uani 1 1 d . . . H24 H -0.1410 -0.1637 0.1152 0.040 Uiso 1 1 calc R . . C25 C -0.1073(2) 0.00848(19) 0.16106(14) 0.0265(4) Uani 1 1 d . . . H25 H -0.0968 0.0330 0.1050 0.032 Uiso 1 1 calc R . . C26 C -0.0973(2) 0.09280(18) 0.23858(13) 0.0214(4) Uani 1 1 d . . . C27 C -0.0576(2) 0.47273(19) 0.19890(14) 0.0283(4) Uani 1 1 d . . . H27A H -0.1651 0.4754 0.1919 0.034 Uiso 1 1 calc R . . H27B H -0.0250 0.5033 0.2611 0.034 Uiso 1 1 calc R . . C28 C 0.0137(3) 0.5509(2) 0.13820(17) 0.0398(6) Uani 1 1 d . . . H28A H 0.1191 0.5424 0.1404 0.060 Uiso 1 1 calc R . . H28B H -0.0037 0.6328 0.1578 0.060 Uiso 1 1 calc R . . H28C H -0.0285 0.5276 0.0775 0.060 Uiso 1 1 calc R . . C29 C -0.0773(2) 0.26728(19) 0.05444(13) 0.0266(4) Uani 1 1 d . . . H29A H -0.0145 0.3079 0.0162 0.032 Uiso 1 1 calc R . . H29B H -0.0672 0.1822 0.0401 0.032 Uiso 1 1 calc R . . C30 C -0.2369(3) 0.2913(2) 0.03320(18) 0.0387(6) Uani 1 1 d . . . H30A H -0.2992 0.2562 0.0737 0.058 Uiso 1 1 calc R . . H30B H -0.2677 0.2569 -0.0278 0.058 Uiso 1 1 calc R . . H30C H -0.2456 0.3760 0.0401 0.058 Uiso 1 1 calc R . . C31 C 0.2328(3) -0.1213(2) 0.2532(2) 0.0480(7) Uani 1 1 d . A . H31A H 0.2057 -0.1038 0.1931 0.058 Uiso 1 1 calc R . . H31B H 0.1465 -0.1602 0.2756 0.058 Uiso 1 1 calc R . . C32 C 0.3571(5) -0.1974(3) 0.2516(3) 0.0827(14) Uani 1 1 d . . . H32A H 0.4188 -0.1859 0.2024 0.099 Uiso 0.593(8) 1 calc PR A 1 H32B H 0.3223 -0.2811 0.2465 0.099 Uiso 0.593(8) 1 calc PR A 1 H32C H 0.3277 -0.2696 0.2761 0.099 Uiso 0.407(8) 1 calc PR A 2 H32D H 0.3797 -0.2205 0.1896 0.099 Uiso 0.407(8) 1 calc PR A 2 C33A C 0.4449(7) -0.1520(6) 0.3468(6) 0.0667(17) Uani 0.593(8) 1 d P A 1 H33A H 0.4040 -0.1921 0.3939 0.080 Uiso 0.593(8) 1 calc PR A 1 H33B H 0.5502 -0.1645 0.3451 0.080 Uiso 0.593(8) 1 calc PR A 1 C33B C 0.4717(10) -0.1471(9) 0.2958(9) 0.0667(17) Uani 0.407(8) 1 d P A 2 H33C H 0.5441 -0.1228 0.2554 0.080 Uiso 0.407(8) 1 calc PR A 2 H33D H 0.5166 -0.2014 0.3324 0.080 Uiso 0.407(8) 1 calc PR A 2 C34 C 0.4218(3) -0.0310(3) 0.3597(3) 0.0619(9) Uani 1 1 d . . . H34A H 0.5032 0.0141 0.3372 0.074 Uiso 0.593(8) 1 calc PR A 1 H34B H 0.4182 -0.0028 0.4234 0.074 Uiso 0.593(8) 1 calc PR A 1 H34C H 0.4073 -0.0475 0.4203 0.074 Uiso 0.407(8) 1 calc PR A 2 H34D H 0.4934 0.0375 0.3621 0.074 Uiso 0.407(8) 1 calc PR A 2 B1 B 0.2801(4) 0.2309(3) 0.4847(2) 0.0468(8) Uani 1 1 d . . . H1B H 0.223(4) 0.144(3) 0.475(2) 0.056 Uiso 1 1 d . . . H2B H 0.384(4) 0.218(3) 0.446(2) 0.056 Uiso 1 1 d . . . H3B H 0.210(4) 0.292(3) 0.453(2) 0.056 Uiso 1 1 d . . . H4B H 0.318(3) 0.258(3) 0.556(2) 0.056 Uiso 1 1 d . . . C35 C 0.3984(19) -0.6305(14) -0.0997(10) 0.067(3) Uani 0.50 1 d P B 1 H35A H 0.4228 -0.7086 -0.0884 0.100 Uiso 0.50 1 calc PR B 1 H35B H 0.4330 -0.6158 -0.1566 0.100 Uiso 0.50 1 calc PR B 1 H35C H 0.2922 -0.6263 -0.1011 0.100 Uiso 0.50 1 calc PR B 1 C36 C 0.4689(5) -0.5422(4) -0.0293(4) 0.0374(8) Uani 0.50 1 d P B 1 C37 C 0.439(2) -0.5393(15) 0.0543(15) 0.0374(8) Uani 0.50 1 d P B 1 H37 H 0.3652 -0.5941 0.0676 0.045 Uiso 0.50 1 calc P C 1 C38 C 0.5077(7) -0.4628(5) 0.1229(4) 0.0481(9) Uani 0.50 1 d P B 1 H38 H 0.4918 -0.4728 0.1822 0.058 Uiso 0.50 1 calc P D 1 C39 C 0.6012(18) -0.3698(13) 0.1052(10) 0.0481(9) Uani 0.50 1 d P B 1 H39 H 0.6454 -0.3114 0.1507 0.058 Uiso 0.50 1 calc P E 1 C40 C 0.6258(7) -0.3684(6) 0.0142(4) 0.0481(9) Uani 0.50 1 d P B 1 H40 H 0.6929 -0.3101 -0.0018 0.058 Uiso 0.50 1 calc P F 1 C41 C 0.556(2) -0.4480(15) -0.0489(15) 0.0374(8) Uani 0.50 1 d P B 1 H41 H 0.5660 -0.4396 -0.1090 0.045 Uiso 0.50 1 calc P G 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.01894(7) 0.02714(7) 0.02046(7) 0.00906(4) 0.00049(4) 0.00077(4) Si1 0.0215(2) 0.0222(3) 0.0195(2) 0.00553(19) 0.00102(19) 0.00460(19) O1 0.0307(8) 0.0393(9) 0.0542(11) 0.0204(8) 0.0017(8) 0.0099(7) C1 0.0224(9) 0.0213(9) 0.0185(8) 0.0059(7) 0.0035(7) 0.0021(7) C2 0.0218(9) 0.0239(9) 0.0193(8) 0.0071(7) 0.0052(7) 0.0015(7) C3 0.0255(9) 0.0274(10) 0.0222(9) 0.0032(8) 0.0024(7) 0.0020(8) C4 0.0323(11) 0.0295(11) 0.0301(10) -0.0012(9) 0.0063(9) 0.0051(9) C5 0.0286(11) 0.0336(12) 0.0366(12) 0.0062(9) 0.0094(9) 0.0100(9) C6 0.0213(9) 0.0344(11) 0.0340(11) 0.0093(9) 0.0057(8) 0.0048(8) C7 0.0193(9) 0.0277(10) 0.0239(9) 0.0067(7) 0.0052(7) 0.0008(7) C8 0.0193(8) 0.0268(10) 0.0249(9) 0.0066(8) 0.0034(7) -0.0003(7) C9 0.0232(10) 0.0346(12) 0.0347(11) 0.0051(9) -0.0013(8) -0.0019(8) C10 0.0312(11) 0.0392(13) 0.0306(11) 0.0024(10) -0.0040(9) -0.0068(9) C11 0.0397(12) 0.0283(11) 0.0274(10) 0.0003(8) 0.0014(9) -0.0026(9) C12 0.0305(10) 0.0241(10) 0.0274(10) 0.0034(8) 0.0035(8) 0.0027(8) C13 0.0226(9) 0.0221(9) 0.0220(8) 0.0064(7) 0.0040(7) -0.0012(7) C14 0.0158(8) 0.0272(9) 0.0193(8) 0.0049(7) 0.0005(6) 0.0020(7) C15 0.0197(8) 0.0287(10) 0.0222(9) 0.0034(7) 0.0046(7) -0.0005(7) C16 0.0286(10) 0.0303(11) 0.0261(10) 0.0018(8) 0.0064(8) -0.0022(8) C17 0.0392(12) 0.0381(13) 0.0273(10) -0.0045(9) 0.0103(9) -0.0048(10) C18 0.0466(14) 0.0466(15) 0.0231(10) 0.0015(10) 0.0119(9) -0.0077(11) C19 0.0375(12) 0.0414(13) 0.0243(10) 0.0088(9) 0.0085(9) -0.0034(10) C20 0.0219(9) 0.0306(10) 0.0224(9) 0.0062(8) 0.0039(7) -0.0020(7) C21 0.0199(9) 0.0288(10) 0.0245(9) 0.0093(8) 0.0024(7) -0.0011(7) C22 0.0304(11) 0.0308(11) 0.0314(11) 0.0105(9) 0.0052(8) -0.0005(8) C23 0.0412(13) 0.0270(11) 0.0388(12) 0.0076(9) 0.0066(10) -0.0027(9) C24 0.0411(12) 0.0269(11) 0.0312(11) 0.0012(9) 0.0049(9) -0.0010(9) C25 0.0269(10) 0.0272(10) 0.0251(9) 0.0033(8) 0.0023(8) 0.0004(8) C26 0.0164(8) 0.0255(9) 0.0225(9) 0.0057(7) 0.0003(7) -0.0008(7) C27 0.0325(11) 0.0257(10) 0.0284(10) 0.0070(8) 0.0025(8) 0.0087(8) C28 0.0572(16) 0.0270(11) 0.0386(13) 0.0118(10) 0.0104(11) 0.0072(11) C29 0.0297(10) 0.0292(10) 0.0219(9) 0.0079(8) -0.0018(8) 0.0046(8) C30 0.0356(12) 0.0394(13) 0.0397(13) 0.0037(10) -0.0114(10) 0.0089(10) C31 0.0497(16) 0.0322(13) 0.0665(19) 0.0144(13) 0.0116(14) 0.0116(11) C32 0.090(3) 0.060(2) 0.113(3) 0.032(2) 0.047(3) 0.047(2) C33A 0.039(2) 0.064(3) 0.113(6) 0.053(4) 0.018(3) 0.023(2) C33B 0.039(2) 0.064(3) 0.113(6) 0.053(4) 0.018(3) 0.023(2) C34 0.0349(14) 0.081(2) 0.079(2) 0.0428(19) -0.0030(15) 0.0187(15) B1 0.0471(17) 0.060(2) 0.0308(13) 0.0165(13) -0.0118(13) -0.0195(15) C35 0.050(4) 0.055(5) 0.083(7) -0.030(4) -0.018(4) 0.011(4) C36 0.0312(13) 0.036(2) 0.047(2) 0.0057(17) 0.0039(13) 0.0129(15) C37 0.0312(13) 0.036(2) 0.047(2) 0.0057(17) 0.0039(13) 0.0129(15) C38 0.046(2) 0.051(2) 0.054(2) 0.0273(18) 0.0148(16) 0.0032(17) C39 0.046(2) 0.051(2) 0.054(2) 0.0273(18) 0.0148(16) 0.0032(17) C40 0.046(2) 0.051(2) 0.054(2) 0.0273(18) 0.0148(16) 0.0032(17) C41 0.0312(13) 0.036(2) 0.047(2) 0.0057(17) 0.0039(13) 0.0129(15) _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 Nd1 O1 2.4284(17) . ? Nd1 B1 2.604(3) . ? Nd1 C1 2.6472(19) . ? Nd1 C14 2.6827(18) . ? Nd1 C2 2.7416(19) . ? Nd1 C13 2.752(2) . ? Nd1 C15 2.752(2) . ? Nd1 C26 2.8119(18) . ? Nd1 C7 2.892(2) . ? Nd1 C20 2.898(2) . ? Nd1 C8 2.903(2) . ? Nd1 C21 2.933(2) . ? Nd1 H1B 2.46(3) . ? Nd1 H2B 2.58(3) . ? Nd1 H3B 2.28(3) . ? Si1 C1 1.865(2) . ? Si1 C14 1.870(2) . ? Si1 C27 1.883(2) . ? Si1 C29 1.887(2) . ? O1 C31 1.460(3) . ? O1 C34 1.467(3) . ? C1 C2 1.450(3) . ? C1 C13 1.451(3) . ? C2 C3 1.424(3) . ? C2 C7 1.433(3) . ? C3 C4 1.374(3) . ? C3 H3 0.9500 . ? C4 C5 1.407(3) . ? C4 H4 0.9500 . ? C5 C6 1.373(3) . ? C5 H5 0.9500 . ? C6 C7 1.409(3) . ? C6 H6 0.9500 . ? C7 C8 1.434(3) . ? C8 C9 1.414(3) . ? C8 C13 1.435(3) . ? C9 C10 1.370(3) . ? C9 H9 0.9500 . ? C10 C11 1.410(3) . ? C10 H10 0.9500 . ? C11 C12 1.376(3) . ? C11 H11 0.9500 . ? C12 C13 1.424(3) . ? C12 H12 0.9500 . ? C14 C15 1.452(3) . ? C14 C26 1.452(3) . ? C15 C16 1.423(3) . ? C15 C20 1.433(3) . ? C16 C17 1.374(3) . ? C16 H16 0.9500 . ? C17 C18 1.405(4) . ? C17 H17 0.9500 . ? C18 C19 1.371(4) . ? C18 H18 0.9500 . ? C19 C20 1.414(3) . ? C19 H19 0.9500 . ? C20 C21 1.437(3) . ? C21 C22 1.410(3) . ? C21 C26 1.436(3) . ? C22 C23 1.367(3) . ? C22 H22 0.9500 . ? C23 C24 1.407(3) . ? C23 H23 0.9500 . ? C24 C25 1.374(3) . ? C24 H24 0.9500 . ? C25 C26 1.423(3) . ? C25 H25 0.9500 . ? C27 C28 1.531(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.535(3) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.489(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33B 1.275(12) . ? C32 C33A 1.624(10) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C32 H32C 0.9900 . ? C32 H32D 0.9900 . ? C33A C34 1.418(7) . ? C33A H33A 0.9900 . ? C33A H33B 0.9900 . ? C33B C34 1.659(12) . ? C33B H33C 0.9900 . ? C33B H33D 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C34 H34C 0.9900 . ? C34 H34D 0.9900 . ? B1 H1B 1.09(3) . ? B1 H2B 1.16(3) . ? B1 H3B 1.13(3) . ? B1 H4B 1.13(3) . ? C35 C36 1.466(15) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.32(2) . ? C36 C41 1.38(3) . ? C37 C38 1.37(2) . ? C37 H37 0.9500 . ? C38 C39 1.399(14) . ? C38 H38 0.9500 . ? C39 C40 1.429(14) . ? C39 H39 0.9500 . ? C40 C41 1.34(2) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Nd1 B1 91.30(10) . . ? O1 Nd1 C1 122.56(6) . . ? B1 Nd1 C1 127.96(9) . . ? O1 Nd1 C14 127.35(6) . . ? B1 Nd1 C14 126.03(10) . . ? C1 Nd1 C14 65.66(6) . . ? O1 Nd1 C2 91.42(6) . . ? B1 Nd1 C2 136.97(9) . . ? C1 Nd1 C2 31.15(6) . . ? C14 Nd1 C2 84.14(6) . . ? O1 Nd1 C13 127.44(6) . . ? B1 Nd1 C13 97.42(9) . . ? C1 Nd1 C13 31.09(6) . . ? C14 Nd1 C13 87.17(6) . . ? C2 Nd1 C13 49.33(6) . . ? O1 Nd1 C15 134.98(6) . . ? B1 Nd1 C15 95.37(10) . . ? C1 Nd1 C15 86.79(6) . . ? C14 Nd1 C15 30.96(6) . . ? C2 Nd1 C15 112.22(6) . . ? C13 Nd1 C15 95.76(6) . . ? O1 Nd1 C26 97.17(6) . . ? B1 Nd1 C26 133.47(9) . . ? C1 Nd1 C26 84.26(6) . . ? C14 Nd1 C26 30.53(6) . . ? C2 Nd1 C26 88.65(6) . . ? C13 Nd1 C26 112.43(6) . . ? C15 Nd1 C26 48.58(6) . . ? O1 Nd1 C7 79.95(6) . . ? B1 Nd1 C7 109.86(9) . . ? C1 Nd1 C7 50.38(6) . . ? C14 Nd1 C7 112.58(6) . . ? C2 Nd1 C7 29.32(5) . . ? C13 Nd1 C7 48.33(6) . . ? C15 Nd1 C7 137.16(6) . . ? C26 Nd1 C7 116.67(6) . . ? O1 Nd1 C20 107.71(6) . . ? B1 Nd1 C20 86.08(9) . . ? C1 Nd1 C20 114.19(6) . . ? C14 Nd1 C20 50.14(6) . . ? C2 Nd1 C20 133.24(6) . . ? C13 Nd1 C20 124.50(6) . . ? C15 Nd1 C20 29.25(6) . . ? C26 Nd1 C20 47.75(6) . . ? C7 Nd1 C20 162.48(6) . . ? O1 Nd1 C8 99.95(6) . . ? B1 Nd1 C8 89.10(9) . . ? C1 Nd1 C8 50.23(6) . . ? C14 Nd1 C8 114.43(6) . . ? C2 Nd1 C8 48.20(6) . . ? C13 Nd1 C8 29.24(5) . . ? C15 Nd1 C8 124.57(6) . . ? C26 Nd1 C8 133.46(6) . . ? C7 Nd1 C8 28.65(6) . . ? C20 Nd1 C8 152.01(6) . . ? O1 Nd1 C21 87.63(6) . . ? B1 Nd1 C21 106.89(9) . . ? C1 Nd1 C21 112.25(6) . . ? C14 Nd1 C21 49.79(6) . . ? C2 Nd1 C21 116.14(6) . . ? C13 Nd1 C21 136.94(6) . . ? C15 Nd1 C21 47.88(6) . . ? C26 Nd1 C21 28.86(6) . . ? C7 Nd1 C21 141.32(6) . . ? C20 Nd1 C21 28.52(6) . . ? C8 Nd1 C21 162.24(6) . . ? O1 Nd1 H1B 75.5(8) . . ? B1 Nd1 H1B 24.6(8) . . ? C1 Nd1 H1B 152.5(8) . . ? C14 Nd1 H1B 122.6(8) . . ? C2 Nd1 H1B 153.1(8) . . ? C13 Nd1 H1B 122.0(8) . . ? C15 Nd1 H1B 93.2(8) . . ? C26 Nd1 H1B 115.9(8) . . ? C7 Nd1 H1B 123.9(8) . . ? C20 Nd1 H1B 73.6(8) . . ? C8 Nd1 H1B 110.2(8) . . ? C21 Nd1 H1B 87.2(8) . . ? O1 Nd1 H2B 79.1(7) . . ? B1 Nd1 H2B 25.9(7) . . ? C1 Nd1 H2B 117.0(8) . . ? C14 Nd1 H2B 149.1(7) . . ? C2 Nd1 H2B 113.9(8) . . ? C13 Nd1 H2B 86.9(8) . . ? C15 Nd1 H2B 120.0(7) . . ? C26 Nd1 H2B 157.1(8) . . ? C7 Nd1 H2B 85.2(8) . . ? C20 Nd1 H2B 111.4(8) . . ? C8 Nd1 H2B 69.2(8) . . ? C21 Nd1 H2B 128.3(8) . . ? H1B Nd1 H2B 41.1(11) . . ? O1 Nd1 H3B 116.9(9) . . ? B1 Nd1 H3B 25.6(8) . . ? C1 Nd1 H3B 109.4(9) . . ? C14 Nd1 H3B 104.4(8) . . ? C2 Nd1 H3B 131.3(9) . . ? C13 Nd1 H3B 82.8(9) . . ? C15 Nd1 H3B 76.0(8) . . ? C26 Nd1 H3B 122.7(9) . . ? C7 Nd1 H3B 113.9(9) . . ? C20 Nd1 H3B 77.3(9) . . ? C8 Nd1 H3B 86.5(9) . . ? C21 Nd1 H3B 104.5(9) . . ? H1B Nd1 H3B 44.6(11) . . ? H2B Nd1 H3B 44.7(11) . . ? C1 Si1 C14 101.35(8) . . ? C1 Si1 C27 111.13(10) . . ? C14 Si1 C27 113.36(10) . . ? C1 Si1 C29 111.67(9) . . ? C14 Si1 C29 113.88(10) . . ? C27 Si1 C29 105.63(9) . . ? C1 Si1 Nd1 50.18(6) . . ? C14 Si1 Nd1 51.30(5) . . ? C27 Si1 Nd1 123.58(7) . . ? C29 Si1 Nd1 130.69(7) . . ? C31 O1 C34 109.3(2) . . ? C31 O1 Nd1 127.36(14) . . ? C34 O1 Nd1 122.90(19) . . ? C2 C1 C13 104.45(16) . . ? C2 C1 Si1 125.76(14) . . ? C13 C1 Si1 127.74(14) . . ? C2 C1 Nd1 78.02(11) . . ? C13 C1 Nd1 78.44(11) . . ? Si1 C1 Nd1 97.05(8) . . ? C3 C2 C7 117.44(18) . . ? C3 C2 C1 132.08(18) . . ? C7 C2 C1 110.45(17) . . ? C3 C2 Nd1 114.21(14) . . ? C7 C2 Nd1 81.17(11) . . ? C1 C2 Nd1 70.83(10) . . ? C4 C3 C2 119.75(19) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 122.0(2) . . ? C3 C4 H4 119.0 . . ? C5 C4 H4 119.0 . . ? C6 C5 C4 120.1(2) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C7 119.24(19) . . ? C5 C6 H6 120.4 . . ? C7 C6 H6 120.4 . . ? C6 C7 C2 121.38(19) . . ? C6 C7 C8 131.23(19) . . ? C2 C7 C8 107.31(17) . . ? C6 C7 Nd1 121.75(15) . . ? C2 C7 Nd1 69.52(11) . . ? C8 C7 Nd1 76.08(11) . . ? C9 C8 C7 130.80(19) . . ? C9 C8 C13 121.62(19) . . ? C7 C8 C13 107.53(17) . . ? C9 C8 Nd1 122.31(15) . . ? C7 C8 Nd1 75.26(12) . . ? C13 C8 Nd1 69.55(11) . . ? C10 C9 C8 119.1(2) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? C9 C10 C11 120.3(2) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C12 C11 C10 121.9(2) . . ? C12 C11 H11 119.1 . . ? C10 C11 H11 119.1 . . ? C11 C12 C13 120.0(2) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C12 C13 C8 117.12(18) . . ? C12 C13 C1 132.65(18) . . ? C8 C13 C1 110.21(17) . . ? C12 C13 Nd1 115.00(14) . . ? C8 C13 Nd1 81.21(12) . . ? C1 C13 Nd1 70.46(11) . . ? C15 C14 C26 104.08(17) . . ? C15 C14 Si1 126.73(15) . . ? C26 C14 Si1 126.81(14) . . ? C15 C14 Nd1 77.17(10) . . ? C26 C14 Nd1 79.66(10) . . ? Si1 C14 Nd1 95.74(7) . . ? C16 C15 C20 117.77(19) . . ? C16 C15 C14 131.6(2) . . ? C20 C15 C14 110.64(18) . . ? C16 C15 Nd1 114.97(13) . . ? C20 C15 Nd1 81.03(12) . . ? C14 C15 Nd1 71.88(10) . . ? C17 C16 C15 119.5(2) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C16 C17 C18 122.0(2) . . ? C16 C17 H17 119.0 . . ? C18 C17 H17 119.0 . . ? C19 C18 C17 120.6(2) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C18 C19 C20 118.9(2) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? C19 C20 C15 121.2(2) . . ? C19 C20 C21 131.4(2) . . ? C15 C20 C21 107.36(17) . . ? C19 C20 Nd1 120.45(14) . . ? C15 C20 Nd1 69.72(11) . . ? C21 C20 Nd1 77.07(12) . . ? C22 C21 C26 121.65(19) . . ? C22 C21 C20 130.8(2) . . ? C26 C21 C20 107.22(18) . . ? C22 C21 Nd1 124.64(14) . . ? C26 C21 Nd1 70.90(11) . . ? C20 C21 Nd1 74.41(11) . . ? C23 C22 C21 118.9(2) . . ? C23 C22 H22 120.6 . . ? C21 C22 H22 120.6 . . ? C22 C23 C24 120.6(2) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C25 C24 C23 121.8(2) . . ? C25 C24 H24 119.1 . . ? C23 C24 H24 119.1 . . ? C24 C25 C26 119.8(2) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C25 C26 C21 117.17(19) . . ? C25 C26 C14 132.19(19) . . ? C21 C26 C14 110.60(17) . . ? C25 C26 Nd1 119.20(13) . . ? C21 C26 Nd1 80.24(11) . . ? C14 C26 Nd1 69.81(10) . . ? C28 C27 Si1 111.82(16) . . ? C28 C27 H27A 109.3 . . ? Si1 C27 H27A 109.3 . . ? C28 C27 H27B 109.3 . . ? Si1 C27 H27B 109.3 . . ? H27A C27 H27B 107.9 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 Si1 113.70(16) . . ? C30 C29 H29A 108.8 . . ? Si1 C29 H29A 108.8 . . ? C30 C29 H29B 108.8 . . ? Si1 C29 H29B 108.8 . . ? H29A C29 H29B 107.7 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O1 C31 C32 106.1(3) . . ? O1 C31 H31A 110.5 . . ? C32 C31 H31A 110.5 . . ? O1 C31 H31B 110.5 . . ? C32 C31 H31B 110.5 . . ? H31A C31 H31B 108.7 . . ? C33B C32 C31 112.7(5) . . ? C33B C32 C33A 30.9(5) . . ? C31 C32 C33A 102.1(3) . . ? C33B C32 H32A 80.5 . . ? C31 C32 H32A 111.3 . . ? C33A C32 H32A 111.3 . . ? C33B C32 H32B 126.9 . . ? C31 C32 H32B 111.3 . . ? C33A C32 H32B 111.3 . . ? H32A C32 H32B 109.2 . . ? C33B C32 H32C 109.1 . . ? C31 C32 H32C 109.1 . . ? C33A C32 H32C 86.7 . . ? H32A C32 H32C 130.3 . . ? H32B C32 H32C 26.6 . . ? C33B C32 H32D 109.1 . . ? C31 C32 H32D 109.1 . . ? C33A C32 H32D 138.2 . . ? H32A C32 H32D 30.9 . . ? H32B C32 H32D 82.5 . . ? H32C C32 H32D 107.8 . . ? C34 C33A C32 102.4(4) . . ? C34 C33A H33A 111.3 . . ? C32 C33A H33A 111.3 . . ? C34 C33A H33B 111.3 . . ? C32 C33A H33B 111.3 . . ? H33A C33A H33B 109.2 . . ? C32 C33B C34 107.4(6) . . ? C32 C33B H33C 110.2 . . ? C34 C33B H33C 110.2 . . ? C32 C33B H33D 110.2 . . ? C34 C33B H33D 110.2 . . ? H33C C33B H33D 108.5 . . ? C33A C34 O1 108.8(4) . . ? C33A C34 C33B 30.5(4) . . ? O1 C34 C33B 100.0(4) . . ? C33A C34 H34A 109.9 . . ? O1 C34 H34A 109.9 . . ? C33B C34 H34A 86.7 . . ? C33A C34 H34B 109.9 . . ? O1 C34 H34B 109.9 . . ? C33B C34 H34B 138.4 . . ? H34A C34 H34B 108.3 . . ? C33A C34 H34C 81.5 . . ? O1 C34 H34C 111.8 . . ? C33B C34 H34C 111.8 . . ? H34A C34 H34C 129.8 . . ? H34B C34 H34C 30.1 . . ? C33A C34 H34D 129.2 . . ? O1 C34 H34D 111.8 . . ? C33B C34 H34D 111.8 . . ? H34A C34 H34D 26.5 . . ? H34B C34 H34D 83.5 . . ? H34C C34 H34D 109.5 . . ? Nd1 B1 H1B 70.0(17) . . ? Nd1 B1 H2B 75.9(16) . . ? H1B B1 H2B 104(2) . . ? Nd1 B1 H3B 60.7(17) . . ? H1B B1 H3B 109(2) . . ? H2B B1 H3B 110(2) . . ? Nd1 B1 H4B 176.9(16) . . ? H1B B1 H4B 110(2) . . ? H2B B1 H4B 107(2) . . ? H3B B1 H4B 117(2) . . ? C37 C36 C41 116.2(14) . . ? C37 C36 C35 122.4(13) . . ? C41 C36 C35 120.9(12) . . ? C36 C37 C38 125(2) . . ? C36 C37 H37 117.7 . . ? C38 C37 H37 117.7 . . ? C37 C38 C39 119.6(14) . . ? C37 C38 H38 120.2 . . ? C39 C38 H38 120.2 . . ? C38 C39 C40 115.5(12) . . ? C38 C39 H39 122.3 . . ? C40 C39 H39 122.3 . . ? C41 C40 C39 121.0(13) . . ? C41 C40 H40 119.5 . . ? C39 C40 H40 119.5 . . ? C40 C41 C36 122.1(19) . . ? C40 C41 H41 118.9 . . ? C36 C41 H41 118.9 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.05 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.747 _refine_diff_density_min -1.286 _refine_diff_density_rms 0.089 #===END #compound 3c data_gc350 _database_code_depnum_ccdc_archive 'CCDC 772844' #TrackingRef '- 2010_cortial_njc.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H34 B Nd O Si' _chemical_formula_weight 629.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P21/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 8.747(1) _cell_length_b 34.629(1) _cell_length_c 9.214(1) _cell_angle_alpha 90.00 _cell_angle_beta 92.708(1) _cell_angle_gamma 90.00 _cell_volume 2787.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 3209 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 34.972 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.500 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1276 _exptl_absorpt_coefficient_mu 1.930 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5124 _exptl_absorpt_correction_T_max 0.8015 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _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 KappaCCD _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 22172 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6121 _reflns_number_gt 5494 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0640P)^2^+15.8201P] 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 6121 _refine_ls_number_parameters 356 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0583 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1543 _refine_ls_wR_factor_gt 0.1495 _refine_ls_goodness_of_fit_ref 1.202 _refine_ls_restrained_S_all 1.202 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.45718(3) 0.117424(8) 0.14309(3) 0.02192(12) Uani 1 1 d . B . Si1 Si 0.26137(17) 0.18432(5) 0.33600(16) 0.0236(3) Uani 1 1 d . . . O1 O 0.3518(5) 0.06744(14) -0.0200(5) 0.0345(10) Uani 1 1 d . . . B1 B 0.7304(9) 0.0936(3) 0.0876(9) 0.0385(16) Uani 1 1 d . . . H1B H 0.727(10) 0.118(2) 0.169(9) 0.046 Uiso 1 1 d . . . H2B H 0.669(9) 0.075(2) 0.136(9) 0.046 Uiso 1 1 d . . . H3B H 0.850(9) 0.084(2) 0.064(8) 0.046 Uiso 1 1 d . . . H4B H 0.670(9) 0.100(2) -0.018(8) 0.046 Uiso 1 1 d . . . C1 C 0.3249(7) 0.18602(17) 0.1473(6) 0.0269(11) Uani 1 1 d . B . C2 C 0.4759(7) 0.19612(17) 0.1031(6) 0.0261(11) Uani 1 1 d . . . C3 C 0.5970(6) 0.21645(17) 0.1745(6) 0.0271(11) Uani 1 1 d . B . H3 H 0.5888 0.2248 0.2720 0.032 Uiso 1 1 calc R . . C4 C 0.7264(7) 0.2240(2) 0.1019(7) 0.0358(14) Uani 1 1 d . . . H4 H 0.8061 0.2386 0.1491 0.043 Uiso 1 1 calc R B . C5 C 0.7453(7) 0.2106(2) -0.0415(7) 0.0355(14) Uani 1 1 d . B . H5 H 0.8374 0.2159 -0.0884 0.043 Uiso 1 1 calc R . . C6 C 0.6314(7) 0.19028(19) -0.1118(6) 0.0302(12) Uani 1 1 d . . . H6 H 0.6439 0.1812 -0.2078 0.036 Uiso 1 1 calc R B . C7 C 0.4950(7) 0.18271(18) -0.0420(6) 0.0275(12) Uani 1 1 d . B . C8 C 0.3527(7) 0.1653(2) -0.0937(6) 0.0305(13) Uani 1 1 d . . . C9 C 0.3048(7) 0.14984(19) -0.2287(6) 0.0310(13) Uani 1 1 d . B . H9 H 0.3732 0.1485 -0.3057 0.037 Uiso 1 1 calc R . . C10 C 0.1561(8) 0.1365(2) -0.2479(6) 0.0338(13) Uani 1 1 d . . . H10 H 0.1220 0.1261 -0.3392 0.041 Uiso 1 1 calc R B . C11 C 0.0545(7) 0.1382(2) -0.1337(6) 0.0356(14) Uani 1 1 d . B . H11 H -0.0468 0.1287 -0.1495 0.043 Uiso 1 1 calc R . . C12 C 0.0987(7) 0.15331(19) 0.0008(6) 0.0312(12) Uani 1 1 d . . . H12 H 0.0294 0.1537 0.0770 0.037 Uiso 1 1 calc R B . C13 C 0.2488(6) 0.16812(17) 0.0232(6) 0.0244(11) Uani 1 1 d . B . C14 C 0.0607(7) 0.1991(2) 0.3714(7) 0.0350(14) Uani 1 1 d . B . H14A H 0.0110 0.2148 0.2928 0.042 Uiso 1 1 calc R A 1 H14B H -0.0058 0.1774 0.3989 0.042 Uiso 1 1 calc R A 1 C15A C 0.1241(16) 0.2224(5) 0.4986(17) 0.039(5) Uani 0.49(3) 1 d P B 1 H15A H 0.1146 0.2085 0.5916 0.047 Uiso 0.49(3) 1 calc PR B 1 H15B H 0.0731 0.2479 0.5043 0.047 Uiso 0.49(3) 1 calc PR B 1 C15B C 0.1367(16) 0.2380(5) 0.418(2) 0.041(5) Uani 0.51(3) 1 d P B 2 H15C H 0.1316 0.2569 0.3375 0.050 Uiso 0.51(3) 1 calc PR B 2 H15D H 0.0867 0.2492 0.5027 0.050 Uiso 0.51(3) 1 calc PR B 2 C16 C 0.3004(7) 0.22678(19) 0.4579(7) 0.0342(13) Uani 1 1 d . B . H16A H 0.3754 0.2218 0.5395 0.041 Uiso 1 1 calc R C 1 H16B H 0.3239 0.2510 0.4064 0.041 Uiso 1 1 calc R C 1 C17 C 0.3341(6) 0.13599(18) 0.3936(5) 0.0253(11) Uani 1 1 d . B . C18 C 0.4905(7) 0.12827(18) 0.4377(5) 0.0250(11) Uani 1 1 d . . . C19 C 0.6128(6) 0.15256(19) 0.4870(6) 0.0281(12) Uani 1 1 d . B . H19 H 0.6001 0.1798 0.4866 0.034 Uiso 1 1 calc R . . C20 C 0.7491(7) 0.13665(19) 0.5351(6) 0.0306(13) Uani 1 1 d . . . H20 H 0.8289 0.1532 0.5714 0.037 Uiso 1 1 calc R B . C21 C 0.7747(7) 0.0964(2) 0.5324(6) 0.0335(13) Uani 1 1 d . B . H21 H 0.8702 0.0864 0.5682 0.040 Uiso 1 1 calc R . . C22 C 0.6627(7) 0.0714(2) 0.4785(6) 0.0321(13) Uani 1 1 d . . . H22 H 0.6814 0.0445 0.4717 0.039 Uiso 1 1 calc R B . C23 C 0.5201(6) 0.08731(17) 0.4342(6) 0.0245(11) Uani 1 1 d . B . C24 C 0.3765(6) 0.06880(18) 0.3884(6) 0.0260(11) Uani 1 1 d . . . C25 C 0.3326(7) 0.02952(18) 0.3764(6) 0.0305(12) Uani 1 1 d . B . H25 H 0.4067 0.0095 0.3860 0.037 Uiso 1 1 calc R . . C26 C 0.1806(7) 0.02103(19) 0.3508(7) 0.0347(14) Uani 1 1 d . . . H26 H 0.1496 -0.0052 0.3454 0.042 Uiso 1 1 calc R B . C27 C 0.0698(7) 0.0501(2) 0.3322(7) 0.0331(13) Uani 1 1 d . B . H27 H -0.0346 0.0431 0.3160 0.040 Uiso 1 1 calc R . . C28 C 0.1098(6) 0.08843(19) 0.3371(6) 0.0289(12) Uani 1 1 d . . . H28 H 0.0346 0.1078 0.3188 0.035 Uiso 1 1 calc R B . C29 C 0.2644(6) 0.09869(17) 0.3698(6) 0.0250(11) Uani 1 1 d . B . C30 C 0.4255(10) 0.0532(3) -0.1497(8) 0.053(2) Uani 1 1 d . B . H30A H 0.5220 0.0396 -0.1218 0.063 Uiso 1 1 calc R . . H30B H 0.4490 0.0749 -0.2150 0.063 Uiso 1 1 calc R . . C31 C 0.3151(13) 0.0263(3) -0.2229(10) 0.074(3) Uani 1 1 d . . . H31A H 0.3066 0.0316 -0.3286 0.089 Uiso 1 1 calc R B . H31B H 0.3486 -0.0008 -0.2080 0.089 Uiso 1 1 calc R . . C32 C 0.1677(12) 0.0328(3) -0.1577(11) 0.072(3) Uani 1 1 d . B . H32A H 0.1086 0.0085 -0.1539 0.087 Uiso 1 1 calc R . . H32B H 0.1063 0.0522 -0.2140 0.087 Uiso 1 1 calc R . . C33 C 0.2076(9) 0.0472(3) -0.0093(8) 0.050(2) Uani 1 1 d . B . H33A H 0.1274 0.0649 0.0237 0.060 Uiso 1 1 calc R . . H33B H 0.2187 0.0254 0.0601 0.060 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 Nd1 0.02307(18) 0.02479(19) 0.01781(16) -0.00051(10) -0.00010(11) 0.00108(10) Si1 0.0232(7) 0.0256(8) 0.0221(7) -0.0030(6) 0.0014(5) -0.0006(6) O1 0.036(2) 0.038(3) 0.030(2) -0.0101(19) 0.0033(17) -0.0009(19) B1 0.034(4) 0.045(5) 0.037(4) 0.003(3) 0.001(3) 0.009(3) C1 0.032(3) 0.025(3) 0.023(2) 0.003(2) -0.003(2) -0.002(2) C2 0.032(3) 0.023(3) 0.023(2) 0.004(2) -0.001(2) 0.000(2) C3 0.027(3) 0.027(3) 0.027(3) 0.003(2) -0.003(2) -0.002(2) C4 0.030(3) 0.043(4) 0.033(3) 0.009(3) -0.004(2) -0.004(3) C5 0.029(3) 0.040(4) 0.038(3) 0.011(3) 0.005(2) 0.000(3) C6 0.033(3) 0.035(3) 0.023(3) 0.005(2) 0.005(2) -0.001(2) C7 0.028(3) 0.033(3) 0.021(2) 0.005(2) 0.000(2) 0.001(2) C8 0.024(3) 0.042(4) 0.025(3) 0.004(2) -0.004(2) 0.002(2) C9 0.035(3) 0.040(3) 0.019(2) 0.009(2) 0.004(2) -0.002(3) C10 0.041(3) 0.040(4) 0.020(3) 0.001(2) -0.001(2) -0.003(3) C11 0.028(3) 0.048(4) 0.030(3) 0.000(3) -0.002(2) -0.003(3) C12 0.031(3) 0.034(3) 0.027(3) 0.002(2) -0.003(2) 0.002(2) C13 0.021(2) 0.030(3) 0.022(2) 0.002(2) -0.0033(19) 0.006(2) C14 0.029(3) 0.039(4) 0.037(3) 0.000(3) 0.007(2) 0.004(3) C15A 0.045(8) 0.044(9) 0.029(8) -0.004(7) 0.012(6) 0.006(6) C15B 0.039(7) 0.041(9) 0.045(10) -0.004(7) 0.010(6) 0.011(6) C16 0.038(3) 0.033(3) 0.031(3) -0.007(3) -0.003(2) 0.004(3) C17 0.027(3) 0.033(3) 0.016(2) -0.003(2) 0.0027(19) 0.000(2) C18 0.030(3) 0.031(3) 0.014(2) 0.004(2) 0.0003(19) -0.002(2) C19 0.025(3) 0.035(3) 0.025(3) -0.004(2) -0.001(2) -0.010(2) C20 0.034(3) 0.037(3) 0.022(3) -0.001(2) 0.001(2) -0.007(3) C21 0.029(3) 0.042(4) 0.029(3) 0.009(3) -0.001(2) 0.002(3) C22 0.031(3) 0.039(4) 0.026(3) 0.005(2) 0.000(2) -0.002(3) C23 0.026(3) 0.030(3) 0.017(2) 0.000(2) -0.0014(19) -0.003(2) C24 0.022(3) 0.033(3) 0.022(2) 0.004(2) 0.000(2) 0.000(2) C25 0.031(3) 0.030(3) 0.030(3) 0.004(2) -0.003(2) -0.002(2) C26 0.034(3) 0.031(3) 0.038(3) 0.004(3) -0.005(3) -0.009(3) C27 0.025(3) 0.040(4) 0.035(3) -0.006(3) -0.001(2) -0.006(2) C28 0.020(3) 0.039(3) 0.027(3) -0.002(2) -0.002(2) -0.001(2) C29 0.024(3) 0.031(3) 0.020(2) -0.001(2) -0.0009(19) 0.000(2) C30 0.057(5) 0.064(5) 0.037(4) -0.021(4) 0.007(3) 0.011(4) C31 0.101(8) 0.073(7) 0.049(5) -0.038(5) 0.012(5) -0.022(6) C32 0.072(6) 0.072(7) 0.070(6) -0.031(5) -0.015(5) -0.009(5) C33 0.048(4) 0.059(5) 0.043(4) -0.016(4) 0.003(3) -0.027(4) _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 Nd1 O1 2.444(4) . ? Nd1 B1 2.602(8) . ? Nd1 C1 2.643(6) . ? Nd1 C17 2.671(5) . ? Nd1 C13 2.727(5) . ? Nd1 C18 2.743(5) . ? Nd1 C2 2.756(6) . ? Nd1 C29 2.822(5) . ? Nd1 C8 2.855(6) . ? Nd1 C7 2.860(6) . ? Nd1 C23 2.906(5) . ? Nd1 C24 2.931(6) . ? Nd1 H1B 2.36(8) . ? Nd1 H2B 2.36(8) . ? Nd1 H4B 2.51(8) . ? Si1 C1 1.851(6) . ? Si1 C17 1.859(6) . ? Si1 C16 1.871(6) . ? Si1 C14 1.871(6) . ? Si1 C15B 2.301(13) . ? Si1 C15A 2.366(13) . ? O1 C33 1.451(8) . ? O1 C30 1.470(8) . ? B1 H1B 1.13(8) . ? B1 H2B 0.95(8) . ? B1 H3B 1.13(8) . ? B1 H4B 1.11(8) . ? C1 C13 1.436(7) . ? C1 C2 1.443(8) . ? C2 C3 1.408(8) . ? C2 C7 1.432(8) . ? C3 C4 1.367(8) . ? C3 H3 0.9500 . ? C4 C5 1.417(9) . ? C4 H4 0.9500 . ? C5 C6 1.360(9) . ? C5 H5 0.9500 . ? C6 C7 1.407(8) . ? C6 H6 0.9500 . ? C7 C8 1.444(8) . ? C8 C9 1.400(8) . ? C8 C13 1.445(8) . ? C9 C10 1.384(9) . ? C9 H9 0.9500 . ? C10 C11 1.411(8) . ? C10 H10 0.9500 . ? C11 C12 1.383(8) . ? C11 H11 0.9500 . ? C12 C13 1.415(8) . ? C12 H12 0.9500 . ? C14 C15A 1.508(15) . ? C14 C15B 1.555(17) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15A C16 1.611(16) . ? C15A H15A 0.9900 . ? C15A H15B 0.9900 . ? C15B C16 1.511(15) . ? C15B H15C 0.9900 . ? C15B H15D 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.434(8) . ? C17 C29 1.440(8) . ? C18 C19 1.418(8) . ? C18 C23 1.442(8) . ? C19 C20 1.368(9) . ? C19 H19 0.9500 . ? C20 C21 1.410(10) . ? C20 H20 0.9500 . ? C21 C22 1.382(9) . ? C21 H21 0.9500 . ? C22 C23 1.406(8) . ? C22 H22 0.9500 . ? C23 C24 1.455(8) . ? C24 C25 1.416(8) . ? C24 C29 1.431(8) . ? C25 C26 1.371(8) . ? C25 H25 0.9500 . ? C26 C27 1.402(9) . ? C26 H26 0.9500 . ? C27 C28 1.373(9) . ? C27 H27 0.9500 . ? C28 C29 1.417(7) . ? C28 H28 0.9500 . ? C30 C31 1.480(12) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.465(14) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.481(11) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? 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 O1 Nd1 B1 88.7(2) . . ? O1 Nd1 C1 119.52(16) . . ? B1 Nd1 C1 134.0(2) . . ? O1 Nd1 C17 123.09(16) . . ? B1 Nd1 C17 131.1(2) . . ? C1 Nd1 C17 64.95(18) . . ? O1 Nd1 C13 88.93(16) . . ? B1 Nd1 C13 136.7(2) . . ? C1 Nd1 C13 30.98(16) . . ? C17 Nd1 C13 84.62(17) . . ? O1 Nd1 C18 136.47(17) . . ? B1 Nd1 C18 100.5(2) . . ? C1 Nd1 C18 83.61(17) . . ? C17 Nd1 C18 30.69(17) . . ? C13 Nd1 C18 110.53(17) . . ? O1 Nd1 C2 129.88(16) . . ? B1 Nd1 C2 103.1(2) . . ? C1 Nd1 C2 30.92(17) . . ? C17 Nd1 C2 84.63(18) . . ? C13 Nd1 C2 49.60(17) . . ? C18 Nd1 C2 89.58(17) . . ? O1 Nd1 C29 94.08(15) . . ? B1 Nd1 C29 131.2(2) . . ? C1 Nd1 C29 85.32(17) . . ? C17 Nd1 C29 30.25(17) . . ? C13 Nd1 C29 92.09(16) . . ? C18 Nd1 C29 48.54(16) . . ? C2 Nd1 C29 111.57(17) . . ? O1 Nd1 C8 80.98(17) . . ? B1 Nd1 C8 107.3(2) . . ? C1 Nd1 C8 50.59(17) . . ? C17 Nd1 C8 113.15(18) . . ? C13 Nd1 C8 29.89(16) . . ? C18 Nd1 C8 133.80(18) . . ? C2 Nd1 C8 48.92(17) . . ? C29 Nd1 C8 121.21(16) . . ? O1 Nd1 C7 104.13(16) . . ? B1 Nd1 C7 90.0(2) . . ? C1 Nd1 C7 50.32(17) . . ? C17 Nd1 C7 112.81(18) . . ? C13 Nd1 C7 48.96(17) . . ? C18 Nd1 C7 118.16(17) . . ? C2 Nd1 C7 29.48(16) . . ? C29 Nd1 C7 135.48(17) . . ? C8 Nd1 C7 29.27(16) . . ? O1 Nd1 C23 111.28(16) . . ? B1 Nd1 C23 86.1(2) . . ? C1 Nd1 C23 111.89(17) . . ? C17 Nd1 C23 49.85(17) . . ? C13 Nd1 C23 134.33(16) . . ? C18 Nd1 C23 29.41(17) . . ? C2 Nd1 C23 117.93(16) . . ? C29 Nd1 C23 47.77(15) . . ? C8 Nd1 C23 162.43(18) . . ? C7 Nd1 C23 144.26(16) . . ? O1 Nd1 C24 88.27(16) . . ? B1 Nd1 C24 103.1(2) . . ? C1 Nd1 C24 112.55(17) . . ? C17 Nd1 C24 49.49(17) . . ? C13 Nd1 C24 120.11(16) . . ? C18 Nd1 C24 48.21(17) . . ? C2 Nd1 C24 133.56(17) . . ? C29 Nd1 C24 28.72(16) . . ? C8 Nd1 C24 147.41(16) . . ? C7 Nd1 C24 162.27(17) . . ? C23 Nd1 C24 28.86(15) . . ? O1 Nd1 H1B 114(2) . . ? B1 Nd1 H1B 26(2) . . ? C1 Nd1 H1B 115.3(19) . . ? C17 Nd1 H1B 111(2) . . ? C13 Nd1 H1B 132.9(19) . . ? C18 Nd1 H1B 81(2) . . ? C2 Nd1 H1B 86.5(18) . . ? C29 Nd1 H1B 124(2) . . ? C8 Nd1 H1B 110.7(19) . . ? C7 Nd1 H1B 84.8(19) . . ? C23 Nd1 H1B 76(2) . . ? C24 Nd1 H1B 102(2) . . ? O1 Nd1 H2B 79.6(19) . . ? B1 Nd1 H2B 21(2) . . ? C1 Nd1 H2B 154(2) . . ? C17 Nd1 H2B 121.4(19) . . ? C13 Nd1 H2B 154(2) . . ? C18 Nd1 H2B 93.7(19) . . ? C2 Nd1 H2B 124(2) . . ? C29 Nd1 H2B 112(2) . . ? C8 Nd1 H2B 124(2) . . ? C7 Nd1 H2B 111(2) . . ? C23 Nd1 H2B 71.9(19) . . ? C24 Nd1 H2B 83(2) . . ? H1B Nd1 H2B 39(3) . . ? O1 Nd1 H4B 74.7(18) . . ? B1 Nd1 H4B 25.0(18) . . ? C1 Nd1 H4B 124.1(19) . . ? C17 Nd1 H4B 155.4(18) . . ? C13 Nd1 H4B 114.5(18) . . ? C18 Nd1 H4B 124.8(18) . . ? C2 Nd1 H4B 96.1(19) . . ? C29 Nd1 H4B 150.4(19) . . ? C8 Nd1 H4B 84.6(18) . . ? C7 Nd1 H4B 74.1(19) . . ? C23 Nd1 H4B 110.3(18) . . ? C24 Nd1 H4B 122.1(19) . . ? H1B Nd1 H4B 45(3) . . ? H2B Nd1 H4B 40(3) . . ? C1 Si1 C17 100.5(3) . . ? C1 Si1 C16 119.0(3) . . ? C17 Si1 C16 119.1(3) . . ? C1 Si1 C14 118.7(3) . . ? C17 Si1 C14 120.5(3) . . ? C16 Si1 C14 80.0(3) . . ? C1 Si1 C15B 116.9(5) . . ? C17 Si1 C15B 142.6(5) . . ? C16 Si1 C15B 40.9(4) . . ? C14 Si1 C15B 42.2(4) . . ? C1 Si1 C15A 139.6(5) . . ? C17 Si1 C15A 119.9(5) . . ? C16 Si1 C15A 42.7(4) . . ? C14 Si1 C15A 39.6(4) . . ? C15B Si1 C15A 22.9(5) . . ? C1 Si1 Nd1 49.82(19) . . ? C17 Si1 Nd1 50.73(16) . . ? C16 Si1 Nd1 139.5(2) . . ? C14 Si1 Nd1 140.4(2) . . ? C15B Si1 Nd1 166.6(5) . . ? C15A Si1 Nd1 170.5(5) . . ? C33 O1 C30 108.0(5) . . ? C33 O1 Nd1 127.2(4) . . ? C30 O1 Nd1 124.8(4) . . ? Nd1 B1 H1B 65(4) . . ? Nd1 B1 H2B 65(5) . . ? H1B B1 H2B 99(6) . . ? Nd1 B1 H3B 179(4) . . ? H1B B1 H3B 114(6) . . ? H2B B1 H3B 116(6) . . ? Nd1 B1 H4B 73(4) . . ? H1B B1 H4B 113(6) . . ? H2B B1 H4B 107(6) . . ? H3B B1 H4B 108(6) . . ? C13 C1 C2 106.0(5) . . ? C13 C1 Si1 125.9(4) . . ? C2 C1 Si1 126.3(4) . . ? C13 C1 Nd1 77.7(3) . . ? C2 C1 Nd1 78.9(3) . . ? Si1 C1 Nd1 97.8(2) . . ? C3 C2 C7 118.6(5) . . ? C3 C2 C1 131.9(5) . . ? C7 C2 C1 109.5(5) . . ? C3 C2 Nd1 118.7(4) . . ? C7 C2 Nd1 79.3(3) . . ? C1 C2 Nd1 70.2(3) . . ? C4 C3 C2 119.3(6) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 122.0(6) . . ? C3 C4 H4 119.0 . . ? C5 C4 H4 119.0 . . ? C6 C5 C4 119.9(6) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C7 119.8(6) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C6 C7 C2 120.4(5) . . ? C6 C7 C8 131.6(5) . . ? C2 C7 C8 107.9(5) . . ? C6 C7 Nd1 123.0(4) . . ? C2 C7 Nd1 71.2(3) . . ? C8 C7 Nd1 75.2(3) . . ? C9 C8 C7 132.1(6) . . ? C9 C8 C13 121.1(5) . . ? C7 C8 C13 106.7(5) . . ? C9 C8 Nd1 122.0(4) . . ? C7 C8 Nd1 75.6(3) . . ? C13 C8 Nd1 70.1(3) . . ? C10 C9 C8 118.7(5) . . ? C10 C9 H9 120.6 . . ? C8 C9 H9 120.6 . . ? C9 C10 C11 120.8(6) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C12 C11 C10 121.6(6) . . ? C12 C11 H11 119.2 . . ? C10 C11 H11 119.2 . . ? C11 C12 C13 119.1(6) . . ? C11 C12 H12 120.5 . . ? C13 C12 H12 120.5 . . ? C12 C13 C1 131.6(5) . . ? C12 C13 C8 118.6(5) . . ? C1 C13 C8 109.8(5) . . ? C12 C13 Nd1 115.0(4) . . ? C1 C13 Nd1 71.3(3) . . ? C8 C13 Nd1 80.0(3) . . ? C15A C14 C15B 35.2(7) . . ? C15A C14 Si1 88.2(6) . . ? C15B C14 Si1 83.9(6) . . ? C15A C14 H14A 114.0 . . ? C15B C14 H14A 83.9 . . ? Si1 C14 H14A 114.0 . . ? C15A C14 H14B 114.0 . . ? C15B C14 H14B 146.5 . . ? Si1 C14 H14B 114.0 . . ? H14A C14 H14B 111.2 . . ? C14 C15A C16 100.9(8) . . ? C14 C15A Si1 52.2(5) . . ? C16 C15A Si1 52.0(4) . . ? C14 C15A H15A 111.6 . . ? C16 C15A H15A 111.6 . . ? Si1 C15A H15A 110.0 . . ? C14 C15A H15B 111.6 . . ? C16 C15A H15B 111.6 . . ? Si1 C15A H15B 140.6 . . ? H15A C15A H15B 109.4 . . ? C16 C15B C14 103.4(9) . . ? C16 C15B Si1 54.1(5) . . ? C14 C15B Si1 53.9(5) . . ? C16 C15B H15C 111.1 . . ? C14 C15B H15C 111.1 . . ? Si1 C15B H15C 106.9 . . ? C16 C15B H15D 111.1 . . ? C14 C15B H15D 111.1 . . ? Si1 C15B H15D 144.1 . . ? H15C C15B H15D 109.1 . . ? C15B C16 C15A 34.4(7) . . ? C15B C16 Si1 85.0(6) . . ? C15A C16 Si1 85.2(6) . . ? C15B C16 H16A 144.6 . . ? C15A C16 H16A 114.4 . . ? Si1 C16 H16A 114.4 . . ? C15B C16 H16B 83.2 . . ? C15A C16 H16B 114.4 . . ? Si1 C16 H16B 114.4 . . ? H16A C16 H16B 111.6 . . ? C18 C17 C29 105.5(5) . . ? C18 C17 Si1 123.9(4) . . ? C29 C17 Si1 128.8(4) . . ? C18 C17 Nd1 77.4(3) . . ? C29 C17 Nd1 80.6(3) . . ? Si1 C17 Nd1 96.7(2) . . ? C19 C18 C17 132.5(6) . . ? C19 C18 C23 117.2(5) . . ? C17 C18 C23 110.3(5) . . ? C19 C18 Nd1 116.2(4) . . ? C17 C18 Nd1 71.9(3) . . ? C23 C18 Nd1 81.6(3) . . ? C20 C19 C18 119.8(6) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C19 C20 C21 121.9(6) . . ? C19 C20 H20 119.1 . . ? C21 C20 H20 119.1 . . ? C22 C21 C20 121.0(6) . . ? C22 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? C21 C22 C23 117.6(6) . . ? C21 C22 H22 121.2 . . ? C23 C22 H22 121.2 . . ? C22 C23 C18 122.4(5) . . ? C22 C23 C24 130.8(6) . . ? C18 C23 C24 106.7(5) . . ? C22 C23 Nd1 122.4(4) . . ? C18 C23 Nd1 69.0(3) . . ? C24 C23 Nd1 76.5(3) . . ? C25 C24 C29 120.2(5) . . ? C25 C24 C23 132.3(5) . . ? C29 C24 C23 107.1(5) . . ? C25 C24 Nd1 124.5(4) . . ? C29 C24 Nd1 71.4(3) . . ? C23 C24 Nd1 74.6(3) . . ? C26 C25 C24 118.5(6) . . ? C26 C25 H25 120.8 . . ? C24 C25 H25 120.8 . . ? C25 C26 C27 121.7(6) . . ? C25 C26 H26 119.1 . . ? C27 C26 H26 119.1 . . ? C28 C27 C26 121.1(6) . . ? C28 C27 H27 119.4 . . ? C26 C27 H27 119.4 . . ? C27 C28 C29 119.2(6) . . ? C27 C28 H28 120.4 . . ? C29 C28 H28 120.4 . . ? C28 C29 C24 119.1(5) . . ? C28 C29 C17 130.6(6) . . ? C24 C29 C17 110.3(5) . . ? C28 C29 Nd1 119.9(4) . . ? C24 C29 Nd1 79.9(3) . . ? C17 C29 Nd1 69.1(3) . . ? O1 C30 C31 106.3(7) . . ? O1 C30 H30A 110.5 . . ? C31 C30 H30A 110.5 . . ? O1 C30 H30B 110.5 . . ? C31 C30 H30B 110.5 . . ? H30A C30 H30B 108.7 . . ? C32 C31 C30 106.5(7) . . ? C32 C31 H31A 110.4 . . ? C30 C31 H31A 110.4 . . ? C32 C31 H31B 110.4 . . ? C30 C31 H31B 110.4 . . ? H31A C31 H31B 108.6 . . ? C31 C32 C33 104.9(7) . . ? C31 C32 H32A 110.8 . . ? C33 C32 H32A 110.8 . . ? C31 C32 H32B 110.8 . . ? C33 C32 H32B 110.8 . . ? H32A C32 H32B 108.8 . . ? O1 C33 C32 105.5(7) . . ? O1 C33 H33A 110.6 . . ? C32 C33 H33A 110.6 . . ? O1 C33 H33B 110.6 . . ? C32 C33 H33B 110.6 . . ? H33A C33 H33B 108.8 . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 1.878 _refine_diff_density_min -1.871 _refine_diff_density_rms 0.182 #===END