#------------------------------------------------------------------------------ #$Date: 2015-01-23 14:30:19 +0200 (Fri, 23 Jan 2015) $ #$Revision: 130086 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/10/55/2105516.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_2105516 loop_ _publ_author_name 'Ferguson, G.' 'Glidewell, C.' 'Gregson, R. M.' 'Meehan, P. R.' 'Patterson, I. L. J.' _publ_section_title ; Formation of One-Dimensional Chains, Two-Dimensional Bilayers and a Three-Dimensional Diamondoid Architecture in Hydrogen-Bonded Adducts of 4,4'-Biphenol with 1,4-Diazabicyclo[2.2.2]octane and 1,2-Diaminoethane ; _journal_issue 2 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 151 _journal_page_last 161 _journal_paper_doi 10.1107/S0108768197010148 _journal_volume 54 _journal_year 1998 _chemical_formula_moiety '(C12 H10 O2) . (C2 H8 N2)' _chemical_formula_sum 'C14 H18 N2 O2' _chemical_formula_weight 246.30 _chemical_name_systematic ; 4,4'-Biphenol--1,2-diaminoethane (1/1) ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yab' _symmetry_space_group_name_H-M 'P 1 21/a 1' _cell_angle_alpha 90.00 _cell_angle_beta 99.962(7) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 8.2121(5) _cell_length_b 5.3401(3) _cell_length_c 14.6014(9) _cell_measurement_reflns_used 25 _cell_measurement_temperature 294.0(10) _cell_measurement_theta_max 21.73 _cell_measurement_theta_min 13.07 _cell_volume 630.67(7) _computing_cell_refinement 'SET4 and CELDIM (Enraf-Nonius, 1992)' _computing_data_collection 'CAD4 (Enraf-Nonius, 1992)' _computing_data_reduction 'DATRD2 in NRCVAX94 (Gabe et al., 1989)' _computing_molecular_graphics 'NRCVAX94, ORTEP (Johnson, 1976), PLATON (Spek, 1996a), PLUTON (Spek 1996b)' _computing_publication_material 'NRCVAX94, SHELXL93 and WordPerfect macro PREPCIF (Ferguson, 1997)' _computing_structure_refinement 'NRCVAX94 and SHELXL93 (Sheldrick, 1993)' _computing_structure_solution 'SOLVER in NRCVAX94' _diffrn_ambient_temperature 294.0(10) _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 MoK\a _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.018 _diffrn_reflns_av_sigmaI/netI 0.0509 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 1703 _diffrn_reflns_theta_max 27.40 _diffrn_reflns_theta_min 2.83 _diffrn_standards_decay_% '4.9, allowed for by scaling' _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.088 _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 1.297 _exptl_crystal_density_meas ? _exptl_crystal_description lath _exptl_crystal_F_000 264 _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.208 _refine_diff_density_min -0.199 _refine_ls_extinction_coef 0.157(17) _refine_ls_extinction_method 'SHELXL93 (Sheldrick, 1993)' _refine_ls_goodness_of_fit_all 1.017 _refine_ls_goodness_of_fit_obs 1.266 _refine_ls_hydrogen_treatment 'riding (C-H 0.93-0.97, N-H 0.89, O-H 0.82\%A)' _refine_ls_matrix_type full _refine_ls_number_parameters 85 _refine_ls_number_reflns 1438 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.017 _refine_ls_restrained_S_obs 1.266 _refine_ls_R_factor_all 0.1035 _refine_ls_R_factor_obs 0.0478 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme ;calc w = 1/[\s^2^(Fo^2^) + (0.0786P)^2^], where P = (Fo^2^ + 2Fc^2^)/3 ; _refine_ls_wR_factor_all 0.1446 _refine_ls_wR_factor_obs 0.1297 _reflns_number_observed 784 _reflns_number_total 1438 _reflns_observed_criterion I>2\s(I) _[local]_cod_data_source_file ab0381.cif _[local]_cod_data_source_block 3 _[local]_cod_cif_authors_sg_H-M 'P 21/a' _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas ; _cod_database_code 2105516 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x+1/2, -y+1/2, z' 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 O1 0.0616(10) 0.0472(10) 0.0364(8) -0.0064(8) 0.0097(6) -0.0002(6) C11 0.0381(10) 0.0358(11) 0.0346(10) 0.0045(9) 0.0041(7) 0.0015(8) C12 0.0515(12) 0.0346(12) 0.0400(11) -0.0054(10) 0.0054(9) -0.0067(8) C13 0.0468(12) 0.0305(12) 0.0461(11) -0.0078(9) 0.0079(9) 0.0000(8) C14 0.0290(8) 0.0279(9) 0.0369(9) 0.0038(8) 0.0022(7) 0.0019(7) C15 0.0456(11) 0.0341(12) 0.0419(11) -0.0094(10) 0.0005(8) -0.0008(8) C16 0.0486(12) 0.0416(13) 0.0390(11) -0.0105(10) 0.0074(9) 0.0037(9) N1 0.0469(9) 0.0499(12) 0.0335(8) 0.0010(9) 0.0001(7) 0.0005(7) C1 0.0491(12) 0.085(2) 0.0411(12) 0.0000(14) 0.0053(9) 0.0118(12) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol O1 0.0549(2) 0.0142(3) -0.33168(9) 0.0483(4) Uani d . 1 O C11 0.0439(2) 0.0146(4) -0.23889(12) 0.0364(5) Uani d . 1 C C12 -0.0451(3) -0.1745(4) -0.20540(13) 0.0423(5) Uani d . 1 C C13 -0.0616(3) -0.1796(4) -0.11318(13) 0.0412(5) Uani d . 1 C C14 0.0098(2) 0.0013(4) -0.04973(11) 0.0317(4) Uani d . 1 C C15 0.1014(3) 0.1868(4) -0.08521(13) 0.0414(5) Uani d . 1 C C16 0.1181(2) 0.1937(4) -0.17770(12) 0.0431(5) Uani d . 1 C N1 0.1591(2) 0.4610(3) -0.39278(10) 0.0443(5) Uani d . 1 N C1 0.0895(3) 0.5035(6) -0.49116(15) 0.0589(7) Uani d . 1 C H1 0.0905 0.1497 -0.3458 0.072 Uiso calc R 1 H H12 -0.0940 -0.2990 -0.24550 0.051 Uiso calc R 1 H H13 -0.1225 -0.3082 -0.09245 0.049 Uiso calc R 1 H H15 0.1529 0.3097 -0.04524 0.050 Uiso calc R 1 H H16 0.1799 0.3204 -0.19882 0.052 Uiso calc R 1 H H1A 0.2688 0.4533 -0.3858 0.066 Uiso calc R 1 H H1B 0.1302 0.5864 -0.3588 0.066 Uiso calc R 1 H H1D 0.1261 0.6652 -0.50998 0.071 Uiso calc R 1 H H1E 0.1311 0.3764 -0.52858 0.071 Uiso calc R 1 H 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' N N 0.0061 0.0033 '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' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 0 -7 -3 1 0 0 2 -3 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 C11 C12 . . 118.4(2) yes O1 C11 C16 . . 122.9(2) yes C12 C11 C16 . . 118.6(2) yes C11 C12 C13 . . 120.5(2) yes C12 C13 C14 . . 122.3(2) yes C13 C14 C14 . 3 122.5(2) yes C13 C14 C15 . . 115.9(2) yes C15 C14 C14 . 3 121.6(2) yes C14 C15 C16 . . 122.2(2) yes C11 C16 C15 . . 120.5(2) yes C1 C1 N1 3_564 . 112.4(2) yes 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 O1 C11 . 1.373(2) yes C11 C12 . 1.384(3) yes C11 C16 . 1.377(3) yes C12 C13 . 1.377(3) yes C13 C14 . 1.396(3) yes C14 C15 . 1.397(3) yes C14 C14 3 1.489(3) yes C15 C16 . 1.381(3) yes N1 C1 . 1.469(3) yes C1 C1 3_564 1.448(4) 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 C11 C12 C13 . . -179.0(2) yes C16 C11 C12 C13 . . 1.3(3) yes C11 C12 C13 C14 . . -0.3(3) yes C12 C13 C14 C15 . . -0.9(3) yes C12 C13 C14 C14 . 3 179.1(2) yes C13 C14 C15 C16 . . 1.1(3) yes C14 C14 C15 C16 3 . -178.8(2) yes O1 C11 C16 C15 . . 179.2(2) yes C12 C11 C16 C15 . . -1.1(3) yes C14 C15 C16 C11 . . -0.1(3) yes