#------------------------------------------------------------------------------ #$Date: 2016-02-20 00:53:41 +0000 (Sat, 20 Feb 2016) $ #$Revision: 176768 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/20/2102024.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_2102024 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, C5 H5 N' _chemical_formula_sum 'C29 H27 N O3 Si2' _chemical_formula_weight 493.70 _chemical_name_systematic ; 1,1,3,3-Tetraphenyldisiloxane-1,3-diol--pyridine (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 74.645(11) _cell_angle_beta 81.968(13) _cell_angle_gamma 85.511(11) _cell_formula_units_Z 1 _cell_length_a 6.4469(15) _cell_length_b 10.2837(15) _cell_length_c 10.6088(15) _cell_measurement_reflns_used 25 _cell_measurement_temperature 294.0(10) _cell_measurement_theta_max 19.00 _cell_measurement_theta_min 10.00 _cell_volume 671.0(2) _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 .0176 _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 2899 _diffrn_reflns_theta_full 26.88 _diffrn_reflns_theta_max 26.88 _diffrn_reflns_theta_min 2.00 _diffrn_standards_decay_% 'no decay, variation 2.9' _diffrn_standards_interval_time 120 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu .162 _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 1.222 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 260 _exptl_crystal_size_max .35 _exptl_crystal_size_mid .35 _exptl_crystal_size_min .33 _refine_diff_density_max .295 _refine_diff_density_min -.258 _refine_ls_extinction_coef .034(5) _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 163 _refine_ls_number_reflns 2899 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.069 _refine_ls_R_factor_all .0489 _refine_ls_R_factor_gt .0403 _refine_ls_shift/su_max .000 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0522P)^2^+0.1916P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .1094 _reflns_number_gt 2449 _reflns_number_total 2899 _reflns_threshold_expression >2\s(I) _cod_data_source_file cf0008.cif _cod_data_source_block sila6 _cod_database_code 2102024 _cod_database_fobs_code 2102024 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_group _atom_site_type_symbol Si1 .33028(7) .62363(4) .49582(4) .03472(15) Uani d . 1 . Si O1 .5000 .5000 .5000 .0533(5) Uani d S 1 . O O2 .1014(2) .57049(15) .56521(11) .0543(3) Uani d P 1 . O C11 .4150(3) .73920(16) .58522(15) .0395(3) Uani d . 1 . C C12 .6050(3) .7218(2) .63580(19) .0547(5) Uani d . 1 . C C13 .6656(4) .8117(2) .6995(2) .0713(6) Uani d . 1 . C C14 .5397(5) .9205(2) .7125(2) .0729(7) Uani d . 1 . C C15 .3511(5) .9413(2) .6639(2) .0752(7) Uani d . 1 . C C16 .2877(4) .85129(19) .60049(19) .0582(5) Uani d . 1 . C C21 .3102(3) .71147(15) .32045(15) .0404(4) Uani d . 1 . C C22 .4845(3) .72227(19) .22522(17) .0532(4) Uani d . 1 . C C23 .4705(4) .7935(2) .0954(2) .0717(6) Uani d . 1 . C C24 .2840(5) .8548(2) .0595(2) .0811(8) Uani d . 1 . C C25 .1106(4) .8451(3) .1507(2) .0807(7) Uani d . 1 . C C26 .1224(3) .7743(2) .28057(19) .0600(5) Uani d . 1 . C N31 .0305(4) .5302(3) .8578(3) .0952(8) Uani d P .50 . N C32 .1757(5) .5528(3) .9314(4) .1131(12) Uani d . 1 . C C33 .1445(5) .5239(3) 1.0681(4) .1077(11) Uani d . 1 . C C31 .0305(4) .5302(3) .8578(3) .0952(8) Uani d P .50 -1 C H1 .0547 .5287 .5202 .081 Uiso calc PR .50 . H H2 .0954 .5576 .6453 .081 Uiso calc PR .50 . H H12 .6939 .6483 .6268 .066 Uiso calc R 1 . H H13 .7933 .7972 .7335 .086 Uiso calc R 1 . H H14 .5817 .9809 .7545 .087 Uiso calc R 1 . H H15 .2647 1.0158 .6732 .090 Uiso calc R 1 . H H16 .1588 .8662 .5680 .070 Uiso calc R 1 . H H22 .6121 .6812 .2488 .064 Uiso calc R 1 . H H23 .5882 .7996 .0328 .086 Uiso calc R 1 . H H24 .2753 .9031 -.0273 .097 Uiso calc R 1 . H H25 -.0162 .8862 .1257 .097 Uiso calc R 1 . H H26 .0032 .7686 .3419 .072 Uiso calc R 1 . H H31 .0490 .5485 .7732 .114 Uiso calc PR .50 . H H32 .3015 .5894 .8877 .136 Uiso calc R 1 . H H33 .2504 .5429 1.1110 .129 Uiso calc R 1 . 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 .0367(2) .0342(2) .0326(2) -.00223(16) -.00517(16) -.00672(16) O1 .0660(12) .0377(9) .0603(11) .0112(8) -.0217(9) -.0166(8) O2 .0482(7) .0757(9) .0396(6) -.0232(6) -.0002(5) -.0126(6) C11 .0467(9) .0371(8) .0333(7) -.0037(7) -.0001(6) -.0089(6) C12 .0529(11) .0593(11) .0603(11) -.0020(9) -.0121(9) -.0274(9) C13 .0743(15) .0833(16) .0683(14) -.0214(12) -.0143(11) -.0327(12) C14 .111(2) .0614(13) .0537(12) -.0303(13) .0022(12) -.0263(10) C15 .117(2) .0453(11) .0634(13) .0074(12) .0043(13) -.0247(10) C16 .0680(13) .0508(10) .0562(11) .0107(9) -.0066(9) -.0186(9) C21 .0498(9) .0368(8) .0348(8) -.0023(7) -.0074(7) -.0082(6) C22 .0581(11) .0557(11) .0431(9) -.0072(9) -.0006(8) -.0093(8) C23 .0943(18) .0727(14) .0424(10) -.0192(13) .0090(11) -.0095(10) C24 .125(2) .0705(15) .0404(11) -.0011(14) -.0210(13) .0040(10) C25 .0962(19) .0791(16) .0592(13) .0225(14) -.0325(13) -.0003(11) C26 .0623(12) .0640(12) .0491(10) .0133(10) -.0143(9) -.0076(9) N31 .0744(16) .0770(16) .130(2) -.0169(13) .0008(15) -.0234(15) C32 .078(2) .097(2) .146(3) -.0284(17) .024(2) -.012(2) C33 .084(2) .090(2) .151(3) -.0225(17) -.018(2) -.027(2) C31 .0744(16) .0770(16) .130(2) -.0169(13) .0008(15) -.0234(15) 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 0 5 3 2 4 2 3 4 0 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 . . 111.11(6) no O1 Si1 C21 . . 108.16(6) no O2 Si1 C21 . . 108.49(7) no O1 Si1 C11 . . 109.18(6) no O2 Si1 C11 . . 108.64(7) no C21 Si1 C11 . . 111.27(7) no Si1 O1 Si1 . 2_666 180.0 y C12 C11 C16 . . 117.12(17) no C12 C11 Si1 . . 122.93(13) no C16 C11 Si1 . . 119.93(14) no C11 C12 C13 . . 121.49(19) no C14 C13 C12 . . 120.3(2) no C13 C14 C15 . . 120.0(2) no C14 C15 C16 . . 120.3(2) no C15 C16 C11 . . 120.8(2) no C26 C21 C22 . . 117.52(16) no C26 C21 Si1 . . 121.15(14) no C22 C21 Si1 . . 121.27(13) no C23 C22 C21 . . 121.0(2) no C24 C23 C22 . . 120.1(2) no C25 C24 C23 . . 120.1(2) no C24 C25 C26 . . 120.4(2) no C25 C26 C21 . . 121.0(2) no C33 N31 C32 2_567 . 113.0(3) no N31 C32 C33 . . 123.3(3) no C31 C33 N31 2_567 2_567 .0(2) no C31 C33 C32 2_567 . 123.7(3) no N31 C33 C32 2_567 . 123.7(3) 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 . 1.6067(5) y Si1 O2 . 1.621(2) y Si1 C21 . 1.8582(16) no Si1 C11 . 1.8584(16) no O1 Si1 2_666 1.6067(5) no C11 C12 . 1.385(2) no C11 C16 . 1.394(2) no C12 C13 . 1.387(3) no C13 C14 . 1.356(3) no C14 C15 . 1.366(4) no C15 C16 . 1.394(3) no C21 C26 . 1.392(3) no C21 C22 . 1.392(2) no C22 C23 . 1.390(3) no C23 C24 . 1.368(4) no C24 C25 . 1.364(4) no C25 C26 . 1.387(3) no N31 C33 2_567 1.349(4) no N31 C32 . 1.369(5) no C32 C33 . 1.390(5) no C33 C31 2_567 1.349(4) no C33 N31 2_567 1.349(4) 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 1.94 2.755(2) 170 yes O2 H2 N31 . .82 2.18 2.995(3) 172 yes C31 H31 O2 . .86 2.14 2.995(3) 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_site_symmetry_1 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag O1 Si1 C11 C12 . . 4.84(16) no O2 Si1 C11 C12 . . 126.16(15) no C21 Si1 C11 C12 . . -114.47(16) no O1 Si1 C11 C16 . . -176.98(13) no O2 Si1 C11 C16 . . -55.66(16) no C21 Si1 C11 C16 . . 63.71(16) no C16 C11 C12 C13 . . .3(3) no Si1 C11 C12 C13 . . 178.55(16) no C11 C12 C13 C14 . . -.7(3) no C12 C13 C14 C15 . . .7(3) no C13 C14 C15 C16 . . -.3(4) no C14 C15 C16 C11 . . -.2(3) no C12 C11 C16 C15 . . .1(3) no Si1 C11 C16 C15 . . -178.17(16) no O1 Si1 C21 C26 . . 148.46(15) no O2 Si1 C21 C26 . . 27.83(17) no C11 Si1 C21 C26 . . -91.62(17) no O1 Si1 C21 C22 . . -34.52(15) no O2 Si1 C21 C22 . . -155.15(14) no C11 Si1 C21 C22 . . 85.40(15) no C26 C21 C22 C23 . . .2(3) no Si1 C21 C22 C23 . . -176.97(15) no C21 C22 C23 C24 . . .2(3) no C22 C23 C24 C25 . . -.6(4) no C23 C24 C25 C26 . . .6(4) no C24 C25 C26 C21 . . -.2(4) no C22 C21 C26 C25 . . -.2(3) no Si1 C21 C26 C25 . . 176.96(18) no C33 N31 C32 C33 2_567 . -.5(5) no N31 C32 C33 C31 . 2_567 .5(6) no N31 C32 C33 N31 . 2_567 .5(6) no