#------------------------------------------------------------------------------ #$Date: 2016-02-19 14:29:56 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176759 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/69/2006948.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, Hiroyuki' 'Ito, Yoshikatsu' 'Ohba, Shigeru' _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_paper_doi 10.1107/S0108270197013796 _journal_volume 54 _journal_year 1998 _chemical_formula_iupac '(C3 H7 N H3)2 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 .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 .045 _reflns_number_observed 1258 _reflns_number_total 2020 _reflns_threshold_expression '|F~o~| > 3\s(|F~o~|)' _cod_data_source_file oa1034.cif _cod_data_source_block II _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_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_atom_site_thermal_displace_type' tag value 'Uij' was replaced with 'Uani' value 8 times. Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 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_original_sg_symbol_H-M 'P 21/n' _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 .0925(4) .0467(3) .0513(3) .0138(3) .0394(3) .0075(3) O2 .1011(5) .0369(3) .0806(4) -.0061(3) .0560(4) .0028(3) N3 .0637(5) .0360(4) .0463(4) .0006(3) .0258(3) -.0019(3) C4 .0521(4) .0423(4) .0434(4) .0035(4) .0203(3) .0061(3) C5 .0520(5) .0338(4) .0411(4) -.0022(3) .0145(3) .0023(3) C6 .0672(6) .0678(6) .0527(5) .0015(5) .0107(4) -.0003(4) C7 .0761(8) .0909(9) .1024(10) .0348(7) .0100(7) -.0034(7) C8 .0820(9) .0952(9) .1256(12) -.0271(7) .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 .19240(8) -.00410(8) .84680(3) .0640(2) Uani 1.000 O2 .13830(8) .29040(8) .91750(4) .0743(2) Uani 1.000 N3 .17740(10) .08590(10) .66790(5) .0499(2) Uani 1.000 C4 .13200(10) .09410(10) .90750(5) .0461(2) Uani 1.000 C5 .04510(10) -.03910(10) .97000(4) .0429(2) Uani 1.000 C6 -.02510(10) .0940(2) .62810(6) .0637(3) Uani 1.000 C7 -.1217(2) .2556(2) .67760(9) .0919(5) Uani 1.000 C8 -.1075(2) -.1253(2) .62930(10) .1063(6) Uani 1.000 H3A .2390(10) -.0220(10) .6412(5) .065(2) Uiso 1.000 H3B .1878(9) .0600(10) .7295(5) .055(2) Uiso 1.000 H3C .2400(10) .2190(10) .6613(5) .076(3) Uiso 1.000 H5 .0558(9) -.1820(10) .9655(4) .045(2) Uiso 1.000 H6 -.0250(10) .1360(10) .5674(6) .082(3) Uiso 1.000 H7A -.071(2) .397(2) .6722(7) .129(5) Uiso 1.000 H7B -.1090(10) .210(2) .7391(8) .124(4) Uiso 1.000 H7C -.252(2) .274(2) .6534(6) .106(4) Uiso 1.000 H8A -.0900(10) -.158(2) .6965(7) .119(4) Uiso 1.000 H8B -.233(2) -.113(2) .6067(7) .120(5) Uiso 1.000 H8C -.0400(10) -.225(2) .5985(7) .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_1 _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 . . .941(8) no N3 H3B . . .957(8) no N3 H3C . . .963(10) no C5 H5 . . .902(8) no C6 H6 . . .976(10) no C7 H7A . . .969(14) no C7 H7B . . .983(12) no C7 H7C . . .962(11) no C8 H8A . . 1.046(12) no C8 H8B . . .921(12) no C8 H8C . . .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)