#------------------------------------------------------------------------------ #$Date: 2016-02-20 00:53:41 +0000 (Sat, 20 Feb 2016) $ #$Revision: 176768 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/20/2102025.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_2102025 loop_ _publ_author_name 'O'Leary, Brian' 'Spalding, Trevor R.' 'Ferguson, George' 'Glidewell, Christopher' _publ_section_title ; Oligosiloxanediols as building blocks for supramolecular chemistry: hydrogen-bonded adducts with amines form supramolecular structures in zero, one and two dimensions ; _journal_issue 2 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 273 _journal_page_last 286 _journal_paper_doi 10.1107/S0108768199013051 _journal_volume 56 _journal_year 2000 _chemical_formula_moiety 'C24 H22 O3 Si2, C4 H4 N2' _chemical_formula_sum 'C28 H26 N2 O3 Si2' _chemical_formula_weight 494.69 _chemical_name_systematic ; 1,1,3,3-Tetraphenyldisiloxane-1,3-diol--pyrimidine (1/1) ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _cell_angle_alpha 76.000(7) _cell_angle_beta 84.438(9) _cell_angle_gamma 86.372(12) _cell_formula_units_Z 1 _cell_length_a 6.4358(5) _cell_length_b 10.2497(12) _cell_length_c 10.4056(10) _cell_measurement_reflns_used 25 _cell_measurement_temperature 294.0(10) _cell_measurement_theta_max 17.00 _cell_measurement_theta_min 9.50 _cell_volume 662.32(11) _computing_cell_refinement 'SET4 & CELDIM in CAD-4-PC Software (Enraf-Nonius, 1992)' _computing_data_collection 'CAD-4-PC Software (Enraf-Nonius, 1992)' _computing_data_reduction 'DATRD2 in NRCVAX96 (Gabe et al., 1989)' _computing_molecular_graphics 'NRCVAX96, ORTEP (Johnson, 1976), PLATON (Spek, 1998)' _computing_publication_material 'NRCVAX96, SHELXL97 and WordPerfect macro PREP8 (Ferguson, 1998)' _computing_structure_refinement 'NRCVAX96 and SHELXL97 (Sheldrick, 1997b)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997a)' _diffrn_ambient_temperature 294.0(10) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \q/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .000 _diffrn_reflns_av_sigmaI/netI .0158 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 2876 _diffrn_reflns_theta_full 26.91 _diffrn_reflns_theta_max 26.91 _diffrn_reflns_theta_min 2.02 _diffrn_standards_decay_% 'no decay, variation 0.6' _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu .165 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 1.0000 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.240 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 260 _exptl_crystal_size_max .38 _exptl_crystal_size_mid .38 _exptl_crystal_size_min .36 _refine_diff_density_max .319 _refine_diff_density_min -.388 _refine_ls_extinction_coef .028(6) _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 162 _refine_ls_number_reflns 2876 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.051 _refine_ls_R_factor_all .0521 _refine_ls_R_factor_gt .0423 _refine_ls_shift/su_max .001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0802P)^2^+0.1328P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .1311 _reflns_number_gt 2389 _reflns_number_total 2876 _reflns_threshold_expression >2\s(I) _cod_data_source_file cf0008.cif _cod_data_source_block sila7 _cod_database_code 2102025 _cod_database_fobs_code 2102025 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Si1 .33183(7) .62355(4) .49509(4) .03787(17) Uani d . 1 . . Si O1 .5000 .5000 .5000 .0586(5) Uani d S 1 . . O O2 .1068(2) .57096(15) .56611(12) .0587(4) Uani d . 1 . . O C11 .4219(3) .74260(16) .58478(16) .0421(4) Uani d . 1 . . C C12 .6167(3) .7299(2) .6341(2) .0606(5) Uani d . 1 . . C C13 .6794(4) .8222(3) .6996(3) .0790(7) Uani d . 1 . . C C14 .5506(5) .9287(2) .7148(2) .0777(7) Uani d . 1 . . C C15 .3589(5) .9449(2) .6665(2) .0782(7) Uani d . 1 . . C C16 .2941(4) .8528(2) .6024(2) .0612(5) Uani d . 1 . . C C21 .2984(3) .70585(16) .31810(16) .0439(4) Uani d . 1 . . C C22 .4665(4) .7173(2) .22184(19) .0601(5) Uani d . 1 . . C C23 .4423(5) .7836(3) .0905(2) .0811(7) Uani d . 1 . . C C24 .2534(6) .8397(3) .0542(2) .0866(8) Uani d . 1 . . C C25 .0845(5) .8300(3) .1465(2) .0834(8) Uani d . 1 . . C C26 .1064(4) .7636(2) .2780(2) .0619(5) Uani d . 1 . . C C31 .0314(7) .5298(3) .8579(4) .1176(11) Uani d P .50 . . C N31 .0314(7) .5298(3) .8579(4) .1176(11) Uani d P .50 . . N C32 .1845(6) .5240(4) .9357(5) .1137(10) Uani d P .75 . . C N32 .1845(6) .5240(4) .9357(5) .1137(10) Uani d P .25 . . N N33 .1605(8) .4972(4) 1.0694(5) .1304(15) Uani d P .25 . . N C33 .1605(8) .4972(4) 1.0694(5) .1304(15) Uani d P .75 . . C H1 .0558 .5278 .5210 .088 Uiso calc PR .50 A 1 H H2 .0974 .5756 .6441 .088 Uiso calc PR .50 A 2 H H12 .7072 .6583 .6232 .073 Uiso calc R 1 . . H H13 .8099 .8110 .7331 .095 Uiso calc R 1 . . H H14 .5933 .9905 .7582 .093 Uiso calc R 1 . . H H15 .2712 1.0180 .6766 .094 Uiso calc R 1 . . H H16 .1625 .8649 .5704 .073 Uiso calc R 1 . . H H22 .5968 .6800 .2457 .072 Uiso calc R 1 . . H H23 .5559 .7897 .0273 .097 Uiso calc R 1 . . H H24 .2386 .8848 -.0337 .104 Uiso calc R 1 . . H H25 -.0448 .8679 .1211 .100 Uiso calc R 1 . . H H26 -.0087 .7577 .3401 .074 Uiso calc R 1 . . H H31 .0486 .5481 .7726 .141 Uiso calc PR .50 . . H H32 .3086 .5385 .8980 .136 Uiso calc PR .75 . . H H33 .2777 .4967 1.1153 .156 Uiso calc PR .75 . . H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Si1 .0418(3) .0352(2) .0357(2) -.00002(16) -.00378(16) -.00693(16) O1 .0737(13) .0396(9) .0648(11) .0157(8) -.0203(10) -.0159(8) O2 .0567(8) .0806(10) .0407(7) -.0245(7) .0025(6) -.0151(6) C11 .0510(9) .0366(8) .0378(8) -.0023(6) .0003(6) -.0087(6) C12 .0566(11) .0621(12) .0703(13) -.0015(9) -.0107(9) -.0278(10) C13 .0832(16) .0856(17) .0786(16) -.0235(13) -.0159(13) -.0309(13) C14 .122(2) .0599(13) .0584(13) -.0284(14) .0014(13) -.0255(10) C15 .123(2) .0483(11) .0650(13) .0084(12) .0069(14) -.0248(10) C16 .0721(13) .0517(11) .0608(12) .0116(9) -.0039(10) -.0195(9) C21 .0534(9) .0382(8) .0393(8) .0019(7) -.0058(7) -.0075(6) C22 .0674(12) .0604(12) .0478(10) -.0011(9) .0040(9) -.0076(8) C23 .107(2) .0822(17) .0455(11) -.0082(15) .0151(12) -.0061(11) C24 .135(3) .0733(15) .0436(11) .0053(16) -.0175(14) .0040(10) C25 .0995(19) .0772(16) .0670(15) .0206(14) -.0328(14) -.0004(12) C26 .0648(12) .0621(12) .0533(11) .0120(10) -.0109(9) -.0047(9) C31 .122(3) .093(2) .145(3) -.017(2) -.033(2) -.033(2) N31 .122(3) .093(2) .145(3) -.017(2) -.033(2) -.033(2) C32 .106(2) .099(2) .140(3) -.0061(18) -.013(2) -.034(2) N32 .106(2) .099(2) .140(3) -.0061(18) -.013(2) -.034(2) N33 .160(4) .093(2) .153(4) .001(2) -.090(3) -.029(2) C33 .160(4) .093(2) .153(4) .001(2) -.090(3) -.029(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si .0817 .0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 0 1 4 -2 -1 2 -5 4 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 Si1 O2 . . 110.91(6) no O1 Si1 C11 . . 109.66(6) no O2 Si1 C11 . . 108.03(7) no O1 Si1 C21 . . 108.34(6) no O2 Si1 C21 . . 108.17(8) no C11 Si1 C21 . . 111.73(7) no Si1 O1 Si1 2_666 . 180.0 y C12 C11 C16 . . 116.80(18) no C12 C11 Si1 . . 123.06(14) no C16 C11 Si1 . . 120.12(15) no C11 C12 C13 . . 121.4(2) no C14 C13 C12 . . 120.2(2) no C13 C14 C15 . . 120.0(2) no C14 C15 C16 . . 120.3(2) no C15 C16 C11 . . 121.4(2) no C22 C21 C26 . . 117.58(17) no C22 C21 Si1 . . 121.17(14) no C26 C21 Si1 . . 121.19(14) no C23 C22 C21 . . 120.9(2) no C24 C23 C22 . . 120.3(2) no C23 C24 C25 . . 120.2(2) no C24 C25 C26 . . 120.0(2) no C25 C26 C21 . . 120.9(2) no C32 C31 C33 . 2_567 112.1(4) no C32 C31 N33 . 2_567 112.1(4) no C33 C31 N33 2_567 2_567 .0020(10) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Si1 O1 . 1.6074(5) y Si1 O2 . 1.623(2) y Si1 C11 . 1.8550(17) no Si1 C21 . 1.8579(16) no O1 Si1 2_666 1.6074(5) no C11 C12 . 1.387(3) no C11 C16 . 1.393(2) no C12 C13 . 1.391(3) no C13 C14 . 1.359(4) no C14 C15 . 1.362(4) no C15 C16 . 1.384(3) no C21 C22 . 1.391(3) no C21 C26 . 1.393(3) no C22 C23 . 1.390(3) no C23 C24 . 1.359(4) no C24 C25 . 1.371(4) no C25 C26 . 1.389(3) no C31 C32 . 1.324(5) no C31 C33 2_567 1.391(6) no C31 N33 2_567 1.391(6) no N33 N31 2_567 1.391(6) no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O2 H1 O2 2_566 .82 1.92 2.736(2) 170 yes O2 H2 N31 . .82 2.17 2.959(4) 163 yes C31 H31 O2 . .86 2.10 2.959(4) 174 yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag O1 Si1 C11 C12 6.43(17) no O2 Si1 C11 C12 127.41(16) no C21 Si1 C11 C12 -113.72(17) no O1 Si1 C11 C16 -175.23(13) no O2 Si1 C11 C16 -54.24(16) no C21 Si1 C11 C16 64.63(17) no C16 C11 C12 C13 .9(3) no Si1 C11 C12 C13 179.28(17) no C11 C12 C13 C14 -1.0(4) no C12 C13 C14 C15 .4(4) no C13 C14 C15 C16 .3(4) no C14 C15 C16 C11 -.4(4) no C12 C11 C16 C15 -.2(3) no Si1 C11 C16 C15 -178.64(17) no O1 Si1 C21 C22 -36.21(16) no O2 Si1 C21 C22 -156.51(15) no C11 Si1 C21 C22 84.71(17) no O1 Si1 C21 C26 146.69(15) no O2 Si1 C21 C26 26.39(18) no C11 Si1 C21 C26 -92.39(17) no C26 C21 C22 C23 -.2(3) no Si1 C21 C22 C23 -177.43(18) no C21 C22 C23 C24 .6(4) no C22 C23 C24 C25 -.7(4) no C23 C24 C25 C26 .5(4) no C24 C25 C26 C21 -.2(4) no C22 C21 C26 C25 .1(3) no Si1 C21 C26 C25 177.26(18) no