#------------------------------------------------------------------------------ #$Date: 2010-05-06 08:38:22 +0300 (Thu, 06 May 2010) $ #$Revision: 1153 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2101849.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_2101849 _journal_name_full 'Acta Crystallographica, Section B' _journal_volume 53 loop_ _publ_author_name 'Pinkerton, A. Alan' _publ_section_title ' ?' _journal_issue 3 _journal_page_first 504 _journal_page_last 512 _journal_year 1997 _chemical_formula_sum 'C2 H11 N11 O9' _chemical_formula_weight 333.18 _chemical_name_systematic ' ?' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _atom_type_scat_source IntTabIV _cell_angle_alpha 90.000(9) _cell_angle_beta 90.000(10) _cell_angle_gamma 90.000(8) _cell_formula_units_Z 4 _cell_length_a 6.4201(6) _cell_length_b 13.4080(10) _cell_length_c 14.584(2) _cell_measurement_reflns_used 91 _cell_measurement_temperature 294.0(10) _cell_measurement_theta_max 14 _cell_measurement_theta_min 9 _cell_volume 1255.4(4) _computing_cell_refinement CAD4_(Enraf-Nonius,_1977) _computing_data_collection CAD4_(Enraf-Nonius,_1977) _computing_data_reduction PROCESS_MolEN_(Fair,_1990) _computing_molecular_graphics ORTEP_(Johnson,_1976) _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) _computing_structure_refinement LSFM_MolEN_(Fair,_1990) _computing_structure_solution Direct_methods_(SIR;_Burla_et_al.,_1989) _diffrn_ambient_temperature 294 _diffrn_measurement_device Enraf_Nonius_CAD4 _diffrn_measurement_method \q/2\q _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.030 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 1462 _diffrn_reflns_theta_max 25.97 _diffrn_reflns_theta_min 2.06 _diffrn_standards_decay_% 77.31 _diffrn_standards_interval_time 50 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.16 _exptl_absorpt_correction_T_max 0.9784 _exptl_absorpt_correction_T_min 0.8915 _exptl_absorpt_correction_type '\y scans (North, Phillips & Mathews, 1968)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.76 _exptl_crystal_description tabular _exptl_crystal_F_000 688 _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.24 _refine_diff_density_max 0.41 _refine_diff_density_min -0.24 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 2.565 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_matrix_type full _refine_ls_number_parameters 205 _refine_ls_number_reflns 992 _refine_ls_number_restraints 38 _refine_ls_R_factor_all 0.087 _refine_ls_R_factor_obs 0.040 _refine_ls_shift/esd_max 0.001 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme 'w = 1/\s^2^(F)' _refine_ls_wR_factor_obs 0.032 _reflns_number_observed 992 _reflns_number_total 1439 _reflns_observed_criterion >3.0\s(I) _[local]_cod_data_source_file bk0035.cif 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 O1 0.7839(7) -0.2174(2) 0.0337(2) 0.0650(10) Uani ? O2 0.8055(6) -0.2011(2) 0.1792(2) 0.0610(10) Uani ? O3 0.9628(5) -0.0717(2) -0.0450(2) 0.0434(9) Uani ? O4 0.8943(5) 0.0680(2) 0.0206(2) 0.0410(9) Uani ? O5 0.3361(5) -0.0874(2) 0.1207(2) 0.0530(10) Uani ? O6 0.3511(6) 0.0380(2) 0.2144(2) 0.0500(10) Uani ? O7 0.3949(6) 0.2054(2) 0.0018(2) 0.0490(10) Uani ? O8 0.2300(5) 0.1954(2) 0.1322(2) 0.0437(9) Uani ? O9 0.4366(5) -0.1227(2) 0.3400(2) 0.0482(9) Uani ? N1 0.8097(6) -0.1663(2) 0.1017(2) 0.0420(10) Uani ? N2 0.8286(6) -0.0637(2) 0.1011(2) 0.0330(10) Uani ? N3 0.8961(6) -0.0240(2) 0.0208(2) 0.0340(10) Uani ? N4 0.3446(5) 0.0024(2) 0.1359(2) 0.0350(10) Uani ? N5 0.3603(6) 0.0567(2) 0.0585(2) 0.0340(10) Uani ? N6 0.3258(6) 0.1587(2) 0.0679(2) 0.0330(10) Uani ? N7 0.7561(6) 0.1932(2) 0.1731(2) 0.0350(10) Uani ? N8 0.7253(6) 0.2108(2) 0.3274(2) 0.0390(10) Uani ? N9 0.8456(6) 0.0614(2) 0.2645(2) 0.0283(9) Uani ? N10 0.9236(5) -0.0769(2) 0.3495(2) 0.0350(10) Uani ? N11 1.0474(6) 0.0742(2) 0.3968(2) 0.0400(10) Uani ? C1 0.7751(7) 0.1575(3) 0.2557(3) 0.0290(10) Uani ? C2 0.9400(7) 0.0196(3) 0.3400(2) 0.0280(10) Uani ? H1 0.7931 0.1534 0.1217 0.0449 Uiso calc H2 0.7053 0.2590 0.1641 0.0449 Uiso calc H3 0.7401 0.1836 0.3871 0.0501 Uiso calc H4 0.6742 0.2768 0.3197 0.0501 Uiso calc H5 0.8273 0.0191 0.2129 0.0368 Uiso calc H6 0.9862 -0.1092 0.4006 0.0452 Uiso calc H7 0.8491 -0.1149 0.3054 0.0452 Uiso calc H8 1.1117 0.0444 0.4487 0.0522 Uiso calc H9 1.0613 0.1438 0.3864 0.0522 Uiso calc H10 0.5341 -0.1109 0.3857 0.0627 Uiso calc H11 0.4117 -0.0641 0.3077 0.0627 Uiso calc 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 0.125(4) 0.035(2) 0.035(2) -0.013(2) 0.001(2) -0.0050(10) O2 0.101(3) 0.049(2) 0.033(2) -0.003(2) -0.001(2) 0.010(2) O3 0.060(2) 0.040(2) 0.0310(10) -0.006(2) 0.012(2) -0.0120(10) O4 0.059(2) 0.0260(10) 0.0380(10) -0.002(2) 0.009(2) -0.0030(10) O5 0.074(2) 0.0230(10) 0.062(2) -0.009(2) -0.002(2) 0.005(2) O6 0.078(2) 0.047(2) 0.0260(10) 0.002(2) 0.004(2) 0.0060(10) O7 0.067(2) 0.039(2) 0.042(2) 0.003(2) 0.011(2) 0.016(2) O8 0.053(2) 0.040(2) 0.039(2) 0.010(2) 0.008(2) -0.008(2) O9 0.060(2) 0.038(2) 0.047(2) -0.009(2) -0.025(2) 0.003(2) N1 0.056(3) 0.033(2) 0.036(2) 0.002(2) 0.003(2) 0.003(2) N2 0.048(2) 0.025(2) 0.027(2) 0.002(2) 0.004(2) 0.000(2) N3 0.031(2) 0.039(2) 0.031(2) -0.002(2) -0.002(2) -0.001(2) N4 0.030(2) 0.035(2) 0.038(2) 0.002(2) 0.001(2) 0.006(2) N5 0.052(2) 0.025(2) 0.025(2) 0.005(2) 0.002(2) 0.001(2) N6 0.034(2) 0.032(2) 0.034(2) 0.002(2) -0.008(2) 0.001(2) N7 0.051(3) 0.027(2) 0.025(2) 0.008(2) 0.000(2) 0.002(2) N8 0.064(3) 0.025(2) 0.026(2) 0.014(2) 0.003(2) 0.002(2) N9 0.039(2) 0.024(2) 0.022(2) 0.007(2) -0.002(2) -0.0020(10) N10 0.041(2) 0.026(2) 0.038(2) 0.005(2) -0.008(2) 0.003(2) N11 0.054(3) 0.031(2) 0.035(2) 0.009(2) -0.019(2) -0.002(2) C1 0.029(3) 0.029(2) 0.030(2) 0.004(2) -0.001(2) 0.003(2) C2 0.031(3) 0.031(2) 0.022(2) 0.011(2) 0.003(2) -0.002(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag O1 N1 1.216(5) yes O2 N1 1.223(5) yes O3 N3 1.229(4) yes O4 N3 1.234(4) yes O5 N4 1.226(4) yes O6 N4 1.241(4) yes O7 N6 1.232(5) yes O8 N6 1.225(5) yes O9 H10 0.9278 no O9 H11 0.9298 no N1 N2 1.381(5) yes N2 N3 1.358(5) yes N4 N5 1.347(5) yes N5 N6 1.392(5) yes N7 C1 1.302(5) yes N7 H1 0.9500 no N7 H2 0.9500 no N8 C1 1.306(5) yes N8 H3 0.9500 no N8 H4 0.9500 no N9 C1 1.373(5) yes N9 C2 1.376(5) yes N9 H5 0.9500 no N10 C2 1.306(5) yes N10 H6 0.9500 no N10 H7 0.9500 no N11 C2 1.303(5) yes N11 H8 0.9500 no N11 H9 0.9500 no O1 H3 2.1905 no O1 H9 2.4097 no O2 H7 2.1911 no O2 H9 2.4435 no O3 H3 2.2201 no O4 H1 1.9763 no O4 H10 2.1011 no O5 H4 2.0180 no O6 H11 1.9683 no O7 H6 2.1038 no O9 H2 1.8303 no O9 H10 0.9278 no O9 H11 0.9298 no H1 O4 1.9763 no H1 N7 0.9500 no H1 N9 2.4439 no H2 O9 1.8303 no H2 N7 0.9500 no H2 N8 2.4697 no H3 O1 2.1905 no H3 O3 2.2201 no H3 N8 0.9500 no H3 N11 2.4624 no H4 O5 2.0180 no H4 N7 2.4714 no H4 N8 0.9500 no H5 N2 1.9720 no H5 N7 2.4488 no H5 N9 0.9500 no H5 N10 2.4512 no H6 O7 2.1038 no H6 N10 0.9500 no H6 N11 2.4905 no H7 O2 2.1911 no H7 N9 2.4375 no H7 N10 0.9500 no H8 N5 2.1051 no H8 N10 2.4893 no H8 N11 0.9500 no H9 O1 2.4097 no H9 O2 2.4435 no H9 N8 2.4905 no H9 N11 0.9500 no H10 O4 2.1011 no H10 O9 0.9278 no H11 O6 1.9683 no H11 O9 0.9298 no 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 H10 O9 H11 109.68 yes O1 N1 O2 122.4(4) yes O1 N1 N2 124.6(4) yes O2 N1 N2 112.7(4) yes N1 N2 N3 115.0(4) yes O3 N3 O4 121.5(4) yes O3 N3 N2 125.5(4) yes O4 N3 N2 113.0(4) yes O5 N4 O6 123.1(4) yes O5 N4 N5 112.5(4) yes O6 N4 N5 124.3(4) yes N4 N5 N6 115.9(4) yes O7 N6 O8 125.1(4) yes O7 N6 N5 111.4(4) yes O8 N6 N5 123.4(4) yes C1 N7 H1 120.00 no C1 N7 H2 120.00 no H1 N7 H2 120.00 no C1 N8 H3 120.00 no C1 N8 H4 120.00 no H3 N8 H4 120.00 no C1 N9 C2 127.1(4) yes C1 N9 H5 116.47 no C2 N9 H5 116.47 no C2 N10 H6 120.00 no C2 N10 H7 120.00 no H6 N10 H7 120.00 no C2 N11 H8 120.00 no C2 N11 H9 120.00 no H8 N11 H9 120.00 no N7 C1 N8 121.1(4) yes N7 C1 N9 117.6(4) yes N8 C1 N9 121.3(4) yes N9 C2 N10 116.9(4) yes N9 C2 N11 120.9(4) yes N10 C2 N11 122.2(4) yes O4 H1 N7 174.79 no O4 H1 N9 107.35 no N7 H1 N9 69.28 no O9 H2 N7 168.75 no O9 H2 N8 106.52 no N7 H2 N8 66.87 no O1 H3 O3 70.32 no O1 H3 N8 144.03 no O1 H3 N11 97.10 no O3 H3 N8 127.59 no O3 H3 N11 92.39 no N8 H3 N11 111.21 no O5 H4 N7 142.08 no O5 H4 N8 143.17 no N7 H4 N8 66.78 no N2 H5 N7 109.95 no N2 H5 N9 172.14 no N2 H5 N10 112.04 no N7 H5 N9 69.00 no N7 H5 N10 137.77 no N9 H5 N10 68.79 no O7 H6 N10 169.23 no O7 H6 N11 124.29 no N10 H6 N11 66.44 no O2 H7 N9 107.74 no O2 H7 N10 156.39 no N9 H7 N10 69.55 no N5 H8 N10 93.58 no N5 H8 N11 155.97 no N10 H8 N11 66.50 no O1 H9 O2 52.24 no O1 H9 N8 104.23 no O1 H9 N11 136.06 no O2 H9 N8 81.99 no O2 H9 N11 158.74 no N8 H9 N11 109.17 no O4 H10 O9 150.07 no O6 H11 O9 166.36 no _cod_database_code 2101849