#------------------------------------------------------------------------------ #$Date: 2013-12-28 14:58:47 +0100 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/34/2003405.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2003405 loop_ _publ_author_name 'Mitzel, N. W.' 'Riede, J.' 'Schier, A.' 'Schmidbaur, H.' _publ_section_title ; Tris(p-tolylsilyl)amine ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 756 _journal_page_last 758 _journal_volume 51 _journal_year 1995 _chemical_formula_sum 'C21 H27 N Si3' _chemical_formula_weight 377.71 _space_group_IT_number 4 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _atom_type_scat_source IntTabIV _cell_angle_alpha 90 _cell_angle_beta 90.67(1) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 9.710(1) _cell_length_b 7.386(1) _cell_length_c 15.236(1) _cell_measurement_reflns_used 25 _cell_measurement_temperature 193 _cell_measurement_theta_max 19 _cell_measurement_theta_min 15 _cell_volume 1092.6(2) _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \q/2\q _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 4776 _diffrn_reflns_theta_max 27 _diffrn_standards_decay_% 1.3 _diffrn_standards_interval_count 100 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.22 _exptl_absorpt_correction_type none _exptl_crystal_colour Colourless _exptl_crystal_density_diffrn 1.148 _exptl_crystal_description Needle _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _refine_diff_density_max 0.31 _refine_diff_density_min -0.36 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 0.411 _refine_ls_number_parameters 249 _refine_ls_number_reflns 4530 _refine_ls_R_factor_obs 0.0280 _refine_ls_shift/esd_max 0.000 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme unit _refine_ls_wR_factor_obs 0.0304 _reflns_number_observed 4530 _reflns_number_total 4698 _reflns_observed_criterion F>4\s(F) _[local]_cod_data_source_file se1070.cif _[local]_cod_data_source_block se1070a _[local]_cod_cif_authors_sg_H-M 'P 21' _[local]_cod_cif_authors_sg_Hall 'P 2y1' _[local]_cod_chemical_formula_sum_orig 'C21 H27 N1 Si3' _cod_original_cell_volume 1092.6 _cod_database_code 2003405 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y+1/2,-z loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Si1 .78888(4) .00260 .37506(3) .031 Si2 .85867(5) -.3144(1) .26074(3) .033 Si3 .82527(6) .0552(1) .18173(4) .046 N .8325(2) -.0834(2) .2736(1) .033 C11 .5988(2) .0070(3) .3900(1) .026 C12 .5078(2) -.0710(2) .3293(1) .029 C13 .3668(2) -.0709(3) .3428(1) .030 C14 .3123(2) .0048(3) .4181(1) .029 C15 .4018(2) .0827(3) .4789(1) .030 C16 .5425(2) .0849(3) .4648(1) .029 C10 .1591(2) .0002(3) .4335(1) .042 C21 1.0409(2) -.3935(2) .2632(1) .029 C22 1.0970(2) -.4768(3) .3378(1) .033 C23 1.2322(2) -.5372(3) .3395(1) .033 C24 1.3164(2) -.5166(3) .2671(1) .031 C25 1.2612(2) -.4364(3) .1923(1) .031 C26 1.1257(2) -.3761(3) .1902(1) .031 C20 1.4646(2) -.5794(3) .2705(2) .043 C31 .9893(2) .0474(3) .1202(1) .033 C32 1.1104(2) .1114(3) .1589(1) .040 C33 1.2351(2) .0958(3) .1168(1) .043 C34 1.2433(2) .0184(3) .0341(1) .039 C35 1.1220(2) -.0430(3) -.0051(1) .037 C36 .9974(2) -.0297(3) .0369(1) .036 C30 1.3798(2) -.0003(4) -.0113(2) .062 H1 .849(2) -.114(3) .444(1) .047(6) H2 .842(2) .185(4) .389(2) .070(8) H3 .789(2) -.392(3) .325(1) .048(6) H4 .801(3) -.356(4) .181(2) .068(8) H5 .711(2) .004(4) .122(1) .064(7) H6 .780(3) .227(4) .211(2) .088(9) H12 .54400 -.13410 .27730 .05 H13 .30260 -.12700 .29880 .05 H15 .37070 .14340 .53210 .05 H16 .60460 .14440 .50740 .05 H22 1.04460 -.48410 .39380 .05 H23 1.27200 -.59540 .38900 .05 H25 1.30960 -.43660 .13460 .05 H26 1.09020 -.31480 .13870 .05 H32 1.12350 .16430 .21970 .05 H33 1.32210 .14190 .14050 .05 H35 1.12360 -.07590 -.06300 .05 H36 .90260 -.06930 .01250 .05 H101 .13190 -.11580 .46020 .08 H102 .1114(2) .0147(3) .3784(1) .08 H103 .1349(2) .0975(3) .4721(1) .08 H201 1.46840 -.69300 .30810 .08 H202 1.5218(2) -.4869(3) .2961(2) .08 H203 1.4958(2) -.6060(3) .2123(2) .08 H301 1.45590 -.01160 .02480 .08 H302 1.3925(2) .1052(4) -.0471(2) .08 H303 1.3752(2) -.1058(4) -.0479(2) .08 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag Si1 N Si2 120.00(10) yes Si2 N Si3 119.50(10) yes Si3 N Si1 119.80(10) yes N Si1 C11 111.70(10) yes N Si2 C21 116.50(10) yes N Si3 C31 111.20(10) yes C12 C11 C16 117.40(10) yes C11 C12 C13 121.3(2) yes C12 C13 C14 120.7(2) yes C13 C14 C15 118.50(10) yes C14 C15 C16 120.8(2) yes C15 C16 C11 121.3(2) yes C22 C21 C26 117.4(2) yes C21 C22 C23 121.1(2) yes C22 C23 C24 121.0(2) yes C23 C24 C25 118.1(2) yes C24 C25 C26 120.9(2) yes C25 C26 C21 121.1(2) yes C32 C31 C36 117.9(2) yes C31 C32 C33 121.0(2) yes C32 C33 C34 121.1(2) yes C33 C34 C35 117.9(2) yes C34 C35 C36 121.4(2) yes C35 C36 C31 120.7(2) yes C12 C11 Si1 122.10(10) yes C16 C11 Si1 120.40(10) yes C10 C14 C13 120.4(2) yes C10 C14 C15 121.1(2) yes C22 C21 Si2 121.00(10) yes C26 C21 Si2 121.60(10) yes C20 C24 C23 120.6(2) yes C20 C24 C25 121.1(2) yes C32 C31 Si3 120.00(10) yes C36 C31 Si3 122.00(10) yes C30 C34 C33 121.0(2) yes C30 C34 C35 121.2(2) yes H1 Si1 N 108.6(8) no H1 Si1 C11 108.1(8) no H2 Si1 N 112.5(9) no H2 Si1 C11 109.0(10) no H3 Si2 N 105.5(9) no H3 Si2 C21 110.0(9) no H4 Si2 N 105.0(10) no H4 Si2 C21 109.0(10) no H5 Si3 N 112.0(10) no H5 Si3 C31 108.8(9) no H6 Si3 N 107.0(10) no H6 Si3 C31 117.0(10) no H12 C12 C11 119.9(2) no H12 C12 C13 118.7(2) no H13 C13 C12 120.6(2) no H13 C13 C14 118.7(2) no H15 C15 C14 123.2(2) no H15 C15 C16 116.0(2) no H16 C16 C11 118.7(2) no H16 C16 C15 120.1(2) no H101 C10 C14 110.7(2) no H102 C10 C14 109.20(10) no H103 C10 C14 109.20(10) no H22 C22 C21 121.4(2) no H22 C22 C23 117.2(2) no H23 C23 C22 122.6(2) no H23 C23 C24 116.3(2) no H25 C25 C24 122.7(2) no H25 C25 C26 115.7(2) no H26 C26 C21 118.8(2) no H26 C26 C25 119.9(2) no H201 C20 C24 107.5(2) no H202 C20 C24 110.00(10) no H203 C20 C24 110.00(10) no H32 C32 C31 128.0(2) no H32 C32 C33 110.8(2) no H33 C33 C32 123.9(2) no H33 C33 C34 114.9(2) no H35 C35 C34 118.5(2) no H35 C35 C36 119.4(2) no H36 C36 C31 112.6(2) no H36 C36 C35 126.6(2) no H301 C30 C34 116.0(2) no H302 C30 C34 107.80(10) no H303 C30 C34 107.80(10) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag N Si1 1.728(2) yes N Si2 1.736(2) yes N Si3 1.735(2) yes Si1 C11 1.862(2) yes Si2 C21 1.864(2) yes Si3 C31 1.858(2) yes C11 C12 1.397(2) yes C12 C13 1.387(2) yes C13 C14 1.386(2) yes C14 C15 1.388(2) yes C15 C16 1.385(2) yes C11 C16 1.394(2) yes C21 C22 1.397(2) yes C22 C23 1.386(2) yes C23 C24 1.389(2) yes C24 C25 1.387(2) yes C25 C26 1.390(2) yes C21 C26 1.397(2) yes C31 C32 1.392(3) yes C32 C33 1.382(3) yes C33 C34 1.386(3) yes C34 C35 1.390(2) yes C35 C36 1.385(3) yes C31 C36 1.395(3) yes C14 C10 1.509(2) yes C24 C20 1.513(2) yes C34 C30 1.508(3) yes Si1 H1 1.47(2) no Si1 H2 1.46(3) no Si2 H3 1.32(2) no Si2 H4 1.37(2) no Si3 H5 1.48(2) no Si3 H6 1.42(3) no C12 H12 0.987(2) no C13 H13 1.000(2) no C15 H15 0.978(2) no C16 H16 0.985(2) no C10 H101 0.986(2) no C10 H102 0.9600(10) no C10 H103 960.0(10) no C22 H22 1.000(2) no C23 H23 0.947(2) no C25 H25 1.002(2) no C26 H26 0.966(2) no C20 H201 1.017(2) no C20 H202 0.9600(10) no C20 H203 0.9600(10) no C32 H32 1.012(2) no C33 H33 0.977(2) no C35 H35 0.915(2) no C36 H36 1.031(2) no C30 H301 0.919(2) no C30 H302 0.9600(10) no C30 H303 0.9600(10) no _journal_paper_doi 10.1107/S0108270194012163