#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2006948.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_2006948 loop_ _publ_author_name 'Hosomi, H.' 'Ito, Y.' 'Ohba, S.' _publ_section_title ; Ammonium and Isopropylammonium Salts of the Fumaric Acid Dianion ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 142 _journal_page_last 145 _journal_volume 54 _journal_year 1998 _chemical_formula_iupac '2C3 H7 N H3 1+ , C4 H2 O4 2-' _chemical_formula_moiety '(C3 H7 N H3 1+)2, (C4 H2 O4 2-)' _chemical_formula_sum 'C10 H22 N2 O4' _chemical_formula_weight 234.30 _chemical_name_systematic ; ? ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_type_scat_source IntTabIV _cell_angle_alpha 90.00000 _cell_angle_beta 99.550(10) _cell_angle_gamma 90.00000 _cell_formula_units_Z 2 _cell_length_a 7.236(2) _cell_length_b 6.275(2) _cell_length_c 15.460(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 298 _cell_measurement_theta_max 15.0 _cell_measurement_theta_min 14.2 _cell_volume 692.2(3) _computing_cell_refinement 'AFC/MSC Diffractometer Control System' _computing_data_collection 'AFC/MSC Diffractometer Control System (Rigaku Corporation, 1993)' _computing_data_reduction 'local programs' _computing_molecular_graphics CRYSTAN-GM _computing_publication_material CRYSTAN-GM _computing_structure_refinement CRYSTAN-GM _computing_structure_solution 'CRYSTAN-GM (Edwards et al., 1996)' _diffrn_measurement_device_type 'Rigaku AFC-5' _diffrn_measurement_method \w _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.014 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 2164 _diffrn_reflns_theta_max 30.0 _diffrn_standards_decay_% 10.7 _diffrn_standards_interval_count 100 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.086 _exptl_absorpt_correction_type none _exptl_crystal_colour Colourless _exptl_crystal_density_diffrn 1.124 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Plate-like _exptl_crystal_F_000 256 _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.6 _exptl_crystal_size_min 0.2 _refine_diff_density_max 0.16 _refine_diff_density_min -0.17 _refine_ls_extinction_method None _refine_ls_goodness_of_fit_obs 0.97 _refine_ls_hydrogen_treatment refall _refine_ls_number_parameters 117 _refine_ls_number_reflns 1258 _refine_ls_R_factor_obs 0.055 _refine_ls_shift/esd_max 0.05 _refine_ls_shift/esd_mean 0.0066 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.000225F^2^]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_obs 0.045 _reflns_number_observed 1258 _reflns_number_total 2020 _reflns_threshold_expression '|F~o~| > 3\s(|F~o~|)' _[local]_cod_data_source_file oa1034.cif _[local]_cod_data_source_block II _[local]_cod_cif_authors_sg_H-M 'P 21/n ' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_cell_volume 692.3(3) _cod_database_code 2006948 loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z -X,-Y,-Z -X+0.5,+Y+0.5,-Z+0.5 +X+0.5,-Y+0.5,+Z+0.5 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 0.0925(4) 0.0467(3) 0.0513(3) 0.0138(3) 0.0394(3) 0.0075(3) O2 0.1011(5) 0.0369(3) 0.0806(4) -.0061(3) 0.0560(4) 0.0028(3) N3 0.0637(5) 0.0360(4) 0.0463(4) 0.0006(3) 0.0258(3) -.0019(3) C4 0.0521(4) 0.0423(4) 0.0434(4) 0.0035(4) 0.0203(3) 0.0061(3) C5 0.0520(5) 0.0338(4) 0.0411(4) -.0022(3) 0.0145(3) 0.0023(3) C6 0.0672(6) 0.0678(6) 0.0527(5) 0.0015(5) 0.0107(4) -.0003(4) C7 0.0761(8) 0.0909(9) 0.1024(10) 0.0348(7) 0.0100(7) -.0034(7) C8 0.0820(9) 0.0952(9) 0.1256(12) -.0271(7) 0.0275(9) -.0302(9) 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_occupancy O1 0.19240(8) -0.00410(8) 0.84680(3) 0.0640(2) Uij 1.000 O2 0.13830(8) 0.29040(8) 0.91750(4) 0.0743(2) Uij 1.000 N3 0.17740(10) 0.08590(10) 0.66790(5) 0.0499(2) Uij 1.000 C4 0.13200(10) 0.09410(10) 0.90750(5) 0.0461(2) Uij 1.000 C5 0.04510(10) -0.03910(10) 0.97000(4) 0.0429(2) Uij 1.000 C6 -0.02510(10) 0.0940(2) 0.62810(6) 0.0637(3) Uij 1.000 C7 -0.1217(2) 0.2556(2) 0.67760(9) 0.0919(5) Uij 1.000 C8 -0.1075(2) -0.1253(2) 0.62930(10) 0.1063(6) Uij 1.000 H3A 0.2390(10) -0.0220(10) 0.6412(5) 0.065(2) Uiso 1.000 H3B 0.1878(9) 0.0600(10) 0.7295(5) 0.055(2) Uiso 1.000 H3C 0.2400(10) 0.2190(10) 0.6613(5) 0.076(3) Uiso 1.000 H5 0.0558(9) -0.1820(10) 0.9655(4) 0.045(2) Uiso 1.000 H6 -0.0250(10) 0.1360(10) 0.5674(6) 0.082(3) Uiso 1.000 H7A -0.071(2) 0.397(2) 0.6722(7) 0.129(5) Uiso 1.000 H7B -0.1090(10) 0.210(2) 0.7391(8) 0.124(4) Uiso 1.000 H7C -0.252(2) 0.274(2) 0.6534(6) 0.106(4) Uiso 1.000 H8A -0.0900(10) -0.158(2) 0.6965(7) 0.119(4) Uiso 1.000 H8B -0.233(2) -0.113(2) 0.6067(7) 0.120(5) Uiso 1.000 H8C -0.0400(10) -0.225(2) 0.5985(7) 0.113(4) Uiso 1.000 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 C4 O2 . . 124.60(10) yes O1 C4 C5 . . 116.30(10) yes O2 C4 C5 . . 119.10(10) yes C4 C5 C5 . 2_557 124.00(10) yes N3 C6 C7 . . 108.60(10) yes N3 C6 C8 . . 109.20(10) yes C7 C6 C8 . . 113.00(10) yes C6 N3 H3A . . 110.4(5) no C6 N3 H3B . . 109.0(4) no C6 N3 H3C . . 111.8(6) no H3A N3 H3B . . 110.5(7) no H3A N3 H3C . . 108.1(7) no H3B N3 H3C . . 107.0(7) no C4 C5 H5 . . 117.1(5) no C5 C5 H5 2_557 . 118.9(5) no N3 C6 H6 . . 104.2(5) no C7 C6 H6 . . 112.4(6) no C8 C6 H6 . . 109.0(6) no C6 C7 H7A . . 110.8(7) no C6 C7 H7B . . 108.5(7) no C6 C7 H7C . . 112.9(7) no H7A C7 H7B . . 112.1(10) no H7A C7 H7C . . 102.8(10) no H7B C7 H7C . . 109.7(9) no C6 C8 H8A . . 102.2(7) no C6 C8 H8B . . 106.7(7) no C6 C8 H8C . . 110.5(7) no H8A C8 H8B . . 109.9(10) no H8A C8 H8C . . 112.0(9) no H8B C8 H8C . . 114.7(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 O1 C4 . 1.2600(10) yes O2 C4 . 1.2410(10) yes N3 C6 . 1.493(2) yes C4 C5 . 1.4930(10) yes C5 C5 2_557 1.3150(10) yes C6 C7 . 1.510(2) yes C6 C8 . 1.501(2) yes N3 H3A . 0.941(8) no N3 H3B . 0.957(8) no N3 H3C . 0.963(10) no C5 H5 . 0.902(8) no C6 H6 . 0.976(10) no C7 H7A . 0.969(14) no C7 H7B . 0.983(12) no C7 H7C . 0.962(11) no C8 H8A . 1.046(12) no C8 H8B . 0.921(12) no C8 H8C . 0.967(11) 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 N3 H3A O2 3_546 0.941(8) 1.809(8) 2.7470(10) 174.7(8) N3 H3B O1 . 0.957(8) 1.852(8) 2.8070(10) 175.6(8) N3 H3C O1 3_556 0.963(10) 1.815(9) 2.7620(10) 167.2(8)