############################################################################## # # # This CIF contains the data in a paper accepted for publication in # # Acta Crystallographica Section C. It conforms to the requirements of # # Notes for Authors for Acta Crystallographica Section C, and has been # # peer reviewed under the auspices of the IUCr Commission on Journals. # # # # Full details of the Crystallographic Information File format # # are given in the paper "The Crystallographic Information File (CIF): # # a New Standard Archive File for Crystallography" by S. R. Hall, F. H. # # Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685]. # # # # The current version of the core CIF dictionary is obtainable from # # ftp://ftp.iucr.org/pub/cif_core.dic. # # # # Software is freely available for graphical display of the structure(s) # # in this CIF. For information consult the CIF software page # # http://www.iucr.org/resources/cif/software. # # # # This file may be used for bona fide research purposes within the # # scientific community so long as proper attribution is given to the journal # # article from which it was obtained. # # # ############################################################################## data_hh1008_text _audit_creation_method 'IUCr checking CIFGEN version 2.1' _journal_date_recd_electronic 1992-02-20 _journal_date_accepted 1992-06-25 _journal_name_full 'Acta Crystallographica, Section C' _journal_year 1992 _journal_volume 48 _journal_issue 11 _journal_page_first 2090 _journal_page_last 2092 _journal_paper_category DO _journal_coeditor_code HH1008 loop_ _publ_author_name 'Schaefer, W.P.' 'Subramanian, V.' 'Myers, A.G.' data_hh1008_structure_1_of_1 _chemical_formula_moiety ? _chemical_formula_sum 'C19 H29 N1 O3 Si1' _chemical_formula_weight 347.53 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21 1' _symmetry_space_group_name_Hall 'P 2y1' _cell_length_a 6.562(4) _cell_length_b 20.473(11) _cell_length_c 15.202(6) _cell_angle_alpha 90. _cell_angle_beta 94.73 _cell_angle_gamma 90. _cell_volume 2035.3(18) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14 _cell_measurement_theta_max 16 _cell_measurement_temperature 293 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.18 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.13 _exptl_crystal_density_meas ? _exptl_absorpt_coefficient_mu 0.125 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_radiation_type 'MoK\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method '\w' _diffrn_reflns_number 7473 _diffrn_reflns_av_R_equivalents 0.026 _diffrn_reflns_theta_max 25 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 150 _diffrn_standards_decay_% 'slight linear decay' _reflns_number_total 3685 _reflns_number_observed 3685 _reflns_observed_criterion ? _refine_ls_structure_factor_coef Fsqd loop_ _refine_ls_R_factor_obs '0.043 for F~o~^2^>0' '0.034 for F~o~^2^>3\s(F~o~^2^)' _refine_ls_wR_factor_obs 0.05 _refine_ls_goodness_of_fit_obs 1.72 _refine_ls_number_reflns 3685 _refine_ls_number_parameters 432 _refine_ls_hydrogen_treatment 'noref' _refine_ls_weighting_scheme '1/[\s^2^(F~o~^2^)+(0.014I)^2^]' _refine_ls_shift/esd_max 0.01 _refine_diff_density_max 0.19 _refine_diff_density_min -0.19 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Sia .8192(2) .5709 .22860(10) .0480(2) O1a .8906(3) .63840(10) .1832(2) .0479{6) O2a .8445(4) .50840(10) .1626(2) .0506(6) C1a .7693(5) .6772(2) .1200(2) .0432(8) C2a .7234(6) .7420(2) .1616(2) .0521(9) C3a .8751(7) .7767(2) .2091(3) .0728(12) C4a .8357(10) .8370(3) .2444(4) .0998(17) C5a .6416(12) .8636(3) .2314(4) .1039(19) C6a .4920(9) .8302(3) .1847(4) .1000(17) C7a .5299(7) .7698(2) .1495(3) .0762(13) C8a .8889(5) .6864(2) .0381(2) .0447(8) C9a .7724(6) .7268(2) -.0332(2) .0622(10) Na .9627(4) .62440(10) .0035(2) .0392(6) C10a 1.1854(5) .6178(2) .0095(2) .0522(9) C11a .8283(5) .5798(2) -.0321(2) .0414(8) O3a .6415(3) .58790(10) -.0300(2) .0586(7) C12a .9030(5) .5187(2) -.0757(2) .0434(8) C13a .7700(6) .5051(2) -.1603(3) .0609(10) C14a .8975(6) .4602(2) -.0114(3) .0546(10) C15a 1.0609(6) .4611(2) .0626(3) .0523(10) C16a 1.2705(7) .4359(2) .0445(3) .0811(13) C17a 1.0295(6) .4844(2) .1412(3) .0533(10) C18a .5445(6) .5720(2) .2467(3) .0799(12) C19a .9895(7) .5606(2) .3304(3) .0705(11) Sib .19390(10) .72990(10) .49650(10) .0421(2) O1b .2820(3) .66530(10) .54990(10) .0423(5) O2b .2422(3) .79650(10) .5547(2) .0492(6) C1b .1829(4) .6315(2) .6176(2) .0371(7) C2b .1220(5) .5642(2) .5847(2) .0417(7) C3b .2651(6) .5238(2) .5515(3) .0611(10) C4b .2135(8) .4604(2) .5254(3) .0773(13) C5b .0176(9) .4381(2) .5319(3) .0833(16) C6b -.1246(8) .4777(2) .5634(4) .0882(15) C7b -.0724(6) .5405(2) .5903(3) .0675(11) C8b .3321(4) .6274(2) .7002(2) .0387(7) C9b .2464(6) .5896(2) .7750(2) .0546(9) Nb .4128(3) .69160(10) .7301(2) .0358(6) C10b .6341(5) .6988(2) .7282(2) .0451(8) C11b .2842(5) .7366(2) .7591(2) .0406(7) O3b .0980(3) .72670(10) .7558(2) .0591(7) C12b .3670(5) .8013(2) .7979(2) .0458(8) C13b .2527(6) .8191(2) .8777(3) .0656(11) C14b .3402(6) .8541(2) .7260(3) .0554(10) C15b .4870(5) .8482(2) .6558(3) .0512(9) C16b .7008(6) .8737(2) .6771(3) .0732(12) C17b .4357(5) .8206(2) .5791(2) .0495(9) C18b -.0888(5) .7296(2) .4781(3) .0633(10) C19b .3273(6) .7321(2) .3951(2) .0647(10) H1a .6424 .6563 .1026 ? H2a 1.0103 .7588 .2177 ? H3a .9402 .8610 .2773 ? H4a .6138 .9048 .2532 ? H5a .3572 .8483 .1765 ? H6a .4223 .7466 .1172 ? H7a 1.0051 .7115 .0577 ? H8a .8535 .7308 -.0819 ? H9a .7452 .7686 -.0106 ? H10a .6479 .7054 -.0515 ? H11a 1.2211 .5768 -.0137 ? H12a 1.2371 .6206 .0698 ? H13a 1.2425 .6519 -.0229 ? H14a 1.0399 .5249 -.0898 ? H15a .8185 .4666 -.1870 ? H16a .7791 .5409 -.1994 ? H17a .6333 .4991 -.1470 ? H18a .7694 .4605 .0132 ? H19a .9124 .4213 -.0438 ? H20a 1.3585 .4393 .0970 ? H21a 1.3213 .4615 -.0006 ? H22a 1.2583 .3918 .0266 ? H23a 1.1406 .4848 .1858 ? H24a .4674 .5769 .1917 ? H25a .5180 .6066 .2849 ? H26a .5099 .5314 .2727 ? H27a 1.1274 .5608 .3165 ? H28a .9595 .5204 .3578 ? H29a .9677 .5956 .3699 ? H1b .0632 .6539 .6317 ? H2b .4009 .5397 .5452 ? H3b .3170 .4324 .5049 ? H4b -.0184 .3946 .5143 ? H5b -.2616 .4621 .5651 ? H6b -.1733 .5674 .6134 ? H7b .4449 .6033 .6820 ? H8b .3450 .5887 .8243 ? H9b .2154 .5463 .7561 ? H10b .1256 .6104 .7911 ? H11b .6745 .7412 .7485 ? H12b .6712 .6931 .6695 ? H13b .7020 .6669 .7655 ? H14b .5091 .7979 .8163 ? H15b .3034 .8592 .9012 ? H16b .2712 .7856 .9201 ? H17b .1111 .8235 .8589 ? H18b .2035 .8504 .6990 ? H19b .3563 .8954 .7537 ? H20b .7777 .8676 .6278 ? H21b .7621 .8510 .7266 ? H22b .6937 .9191 .6903 ? H23b .5375 .8167 .5379 ? H24b .4711 .7323 .4099 ? H25b .2893 .7702 .3623 ? H26b .2918 .6945 .3604 ? H27b -.1461 .7281 .5329 ? H28b -.1302 .6916 .4443 ? H29b -.1327 .7673 .4462 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Sia O1a 1.630 Sia O2a 1.644 Sia C18a 1.846 Sia C19a 1.845 O1a C1a 1.435(4) O2a C17a 1.372(4) C1a C2a 1.512(5) C1a C8a 1.536(5) C1a H1a 0.953 C2a C3a 1.378(6) C2a C7a 1.390(6) C3a C4a 1.379(7) C3a H2a 0.959 C4a C5a 1.383(8) C4a H3a 0.951 C5a C6a 1.350(8) C5a H4a 0.931 C6a C7a 1.378(7) C6a H5a 0.958 C7a H6a 0.952 C8a C9a 1.518(5) C8a Na 1.472(4) C8a H7a 0.947 C9a H8a 0.950 C9a H9a 0.945 C9a H10a 0.948 Na C10a 1.463(4) Na C11a 1.351(4) C10a H11a 0.947 C10a H12a 0.953 C10a H13a 0.950 C11a O3a 1.240(4) C11a C12a 1.517(5) C12a C13a 1.518(5) C12a C14a 1.548(5) C12a H14a 0.950 C13a H15a 0.952 C13a H16a 0.949 C13a H17a 0.943 C14a C15a 1.489(5) C14a H18a 0.947 C14a H19a 0.946 C15a C16a 1.515(6) C15a C17a 1.319(5) C16a H20a 0.949 C16a H21a 0.945 C16a H22a 0.944 C17a H23a 0.953 C18a H24a 0.945 C18a H25a 0.941 C18a H26a 0.957 C19a H27a 0.946 C19a H28a 0.949 C19a H29a 0.954 Sib O1b 1.633(2) Sib O2b 1.641(3) Sib C18b 1.853(4) Sib C19b 1.835(4) O1b C1b 1.439(4) O2b C17b 1.384(4) C1b C2b 1.508(4) C1b C8b 1.531(4) C1b H1b 0.950 C2b C3b 1.378(5) C2b C7b 1.374(5) C3b C4b 1.391(6) C3b H2b 0.961 C4b C5b 1.375(7) C4b H3b 0.960 C5b C6b 1.352(7) C5b H4b 0.955 C6b C7b 1.384(6) C6b H5b 0.956 C7b H6b 0.950 C8b C9b 1.520(5) C8b Nb 1.474(4) C8b H7b 0.950 C9b H8b 0.949 C9b H9b 0.949 C9b H10b 0.950 Nb C10b 1.462(4) Nb C11b 1.348(4) C10b H11b 0.951 C10b H12b 0.952 C10b H13b 0.951 C11b O3b 1.235(4) C11b C12b 1.532(5) C12b C13b 1.523(5) C12b C14b 1.536(5) C12b H14b 0.953 C13b H15b 0.946 C13b H16b 0.941 C13b H17b 0.953 C14b C15b 1.501(5) C14b H18b 0.958 C14b H19b 0.947 C15b C16b 1.507(6) C15b C17b 1.314(5) C16b H20b 0.946 C16b H21b 0.945 C16b H22b 0.953 C17b H23b 0.955 C18b H27b 0.942 C18b H28b 0.959 C18b H29b 0.945 C19b H24b 0.952 C19b H25b 0.949 C19b H26b 0.951 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O2a Sia O1a 110.8 C18a Sia O1a 111.8 C19a Sia O1a 106.1 C18a Sia O2a 104.4 C19a Sia O2a 109.8 C19a Sia C18a 114.1 C1a O1a Sia 126.1 C17a O2a Sia 124.0 C2a C1a O1a 108.9(3) C8a C1a O1a 108.6(2) C8a C1a C2a 111.3(3) C9a C8a C1a 112.6(3) Na C8a C1a 112.8(3) Na C8a C9a 112.1(3) C10a Na C8a 114.5(2) C11a Na C8a 120.2(3) C11a Na C10a 125.3(3) O3a C11a Na 120.9(3) C12a C11a Na 120.6(3) C12a C11a O3a 118.5(3) C13a C12a C11a 109.7(3) C14a C12a C11a 109.7(3) C14a C12a C13a 110.6(3) C15a C14a C12a 114.5(3) C16a C15a C14a 117.8(3) C17a C15a C14a 122.2(3) C17a C15a C16a 120.0(4) C15a C17a O2a 123.4(3) O2b Sib O1b 111.10(10) C18b Sib O1b 112.40(10) C19b Sib O1b 105.3(2) C18b Sib O2b 103.3(2) C19b Sib O2b 110.4(2) C19b Sib C18b 114.5(2) C1b O1b Sib 125.7(2) C17b O2b Sib 125.0(2) C2b C1b O1b 109.0(2) C8b C1b O1b 108.5(2) C8b C1b C2b 110.9(2) C9b C8b C1b 113.0(3) Nb C8b C1b 113.2(2) Nb C8b C9b 111.7(3) C10b Nb C8b 114.6(2) C11b Nb C8b 119.4(2) C11b Nb C10b 125.9(3) O3b C11b Nb 121.3(3) C12b C11b Nb 120.4(3) C12b C11b O3b 118.4(3) C13b C12b C11b 109.3(3) C14b C12b C11b 108.6(3) C14b C12b C13b 111.4(3) C16b C15b C14b 117.4(3) C17b C15b C14b 122.2(3) C17b C15b C16b 120.4(3) C15b C17b O2b 123.6(3)