#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2006947.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_2006947 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 '2N H4 1+, C4 H2 O4 2-' _chemical_formula_moiety '(N H4 1+)2, (C4 H2 O4 2-)' _chemical_formula_sum 'C4 H10 N2 O4' _chemical_formula_weight 150.13 _chemical_name_systematic ; ? ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_type_scat_source IntTabIV _cell_angle_alpha 90.00000 _cell_angle_beta 92.46(3) _cell_angle_gamma 90.00000 _cell_formula_units_Z 2 _cell_length_a 3.733(3) _cell_length_b 8.009(2) _cell_length_c 11.508(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 298 _cell_measurement_theta_max 14.9 _cell_measurement_theta_min 14.1 _cell_volume 343.7(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 \q-2\q _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.009 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 1146 _diffrn_reflns_theta_max 30.0 _diffrn_standards_decay_% 6.1 _diffrn_standards_interval_count 100 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.129 _exptl_absorpt_correction_type none _exptl_crystal_colour Colourless _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Prism _exptl_crystal_F_000 160 _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.4 _refine_diff_density_max 0.26 _refine_diff_density_min -0.31 _refine_ls_extinction_method None _refine_ls_goodness_of_fit_obs 1.06 _refine_ls_hydrogen_treatment refall _refine_ls_number_parameters 66 _refine_ls_number_reflns 908 _refine_ls_R_factor_obs 0.040 _refine_ls_shift/esd_max 0.02 _refine_ls_shift/esd_mean 0.0024 _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 0.048 _reflns_number_observed 908 _reflns_number_total 1008 _reflns_threshold_expression '|F~o~| > 3\s(|F~o~|)' _[local]_cod_data_source_file oa1034.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/c ' _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_database_code 2006947 loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z -X,-Y,-Z -X,+Y+0.5,-Z+0.5 +X,-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 0.0479(2) 0.02180(10) 0.02380(10) -.00040(10) 0.01430(10) -.00090(10) O2 0.0447(2) 0.01850(10) 0.02530(10) -.00620(10) 0.01040(10) 0.00200(10) N3 0.0304(2) 0.02430(10) 0.02360(10) -.00130(10) 0.00710(10) -.00240(10) C4 0.02410(10) 0.01710(10) 0.02190(10) -.00080(10) 0.00430(10) 0.00050(10) C5 0.0308(2) 0.01620(10) 0.0254(2) -.00220(10) 0.00670(10) 0.00170(10) 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 0.11270(7) 0.26340(3) 0.30750(2) 0.03120(10) Uij 1.000 O2 -0.07190(7) 0.18730(3) 0.48060(2) 0.02950(10) Uij 1.000 N3 0.50400(8) -0.04600(4) 0.34760(3) 0.02620(10) Uij 1.000 C4 0.02290(8) 0.29600(4) 0.40990(3) 0.02100(10) Uij 1.000 C5 0.03340(9) 0.47490(4) 0.44720(3) 0.02410(10) Uij 1.000 H3A 0.6690(10) 0.0063(6) 0.3983(4) 0.0580(10) Uiso 1.000 H3B 0.619(2) -0.1084(7) 0.2874(4) 0.0440(10) Uiso 1.000 H3C 0.373(2) -0.1101(7) 0.3912(5) 0.043(2) Uiso 1.000 H3D 0.3640(10) 0.0398(6) 0.3140(4) 0.0500(10) Uiso 1.000 H5 0.0870(10) 0.5496(6) 0.3928(4) 0.0440(10) 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 . . 123.70(10) yes O1 C4 C5 . . 117.40(10) yes O2 C4 C5 . . 118.90(10) yes C4 C5 C5 . 2_566 123.70(10) yes H3A N3 H3B . . 112.1(5) no H3A N3 H3C . . 106.0(5) no H3A N3 H3D . . 105.7(5) no H3B N3 H3C . . 112.4(5) no H3B N3 H3D . . 109.8(5) no H3C N3 H3D . . 110.5(5) no C4 C5 H5 . . 116.3(4) no C5 C5 H5 2_566 . 120.0(4) 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 . 1.2660(10) yes O2 C4 . 1.2530(10) yes C4 C5 . 1.4960(10) yes C5 C5 2_566 1.3140(10) yes N3 H3A . 0.931(5) no N3 H3B . 0.970(6) no N3 H3C . 0.881(6) no N3 H3D . 0.936(5) no C5 H5 . 0.895(6) 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 1_655 0.931(5) 1.963(5) 2.8520(10) 159.1(5) N3 H3B O1 3_645 0.970(6) 1.828(5) 2.7900(10) 170.8(5) N3 H3C O2 2_556 0.881(6) 1.991(6) 2.8400(10) 161.5(5) N3 H3D O1 . 0.936(5) 2.022(5) 2.9030(10) 156.2(5)