#------------------------------------------------------------------------------ #$Date: 2011-09-17 21:27:16 +0100 (Sat, 17 Sep 2011) $ #$Revision: 26029 $ #$URL: svn://www.crystallography.net/cod/cif/2/2204515.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_2204515 loop_ _publ_author_name 'Ravikumar, B.' 'Athimoolam, S.' 'Rajaram, R. K.' _publ_section_title ; L-Ornithinium sulfate monohydrate ; _journal_issue 11 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first o2093 _journal_page_last o2095 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac 'C5 H14 N2 O2 2+ , SO4 2- , H2 O' _chemical_formula_moiety 'C5 H14 N2 O2 2+ , SO4 2- , H2 O' _chemical_formula_sum 'C5 H16 N2 O7 S' _chemical_formula_weight 248.26 _chemical_name_common 'L-ornithinium sulfate monohydrate' _chemical_name_systematic ; L-ornithinium sulfate monohydrate ; _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 6.1589(2) _cell_length_b 9.682(6) _cell_length_c 18.714(6) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 14.22 _cell_measurement_theta_min 11.30 _cell_volume 1115.9(8) _computing_cell_refinement 'CAD-4 EXPRESS' _computing_data_collection 'CAD-4 EXPRESS (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997) and PLATON (Spek, 1999)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Nonius MACH 3' _diffrn_measurement_method \w/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0224 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_number 1399 _diffrn_reflns_theta_full 25 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_min 2.18 _diffrn_standards_decay_% none _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.311 _exptl_absorpt_correction_T_max 0.940 _exptl_absorpt_correction_T_min 0.911 _exptl_absorpt_correction_type '\y scan' _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.478 _exptl_crystal_density_meas 1.475(5) _exptl_crystal_density_method 'flotation, using a mixture of CCl~4~ and xylene' _exptl_crystal_description needle _exptl_crystal_F_000 528 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _refine_diff_density_max 0.734 _refine_diff_density_min -0.370 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 137 _refine_ls_number_reflns 1172 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.060 _refine_ls_R_factor_all 0.0665 _refine_ls_R_factor_gt 0.0587 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.1120P)^2^+1.3829P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1628 _refine_ls_wR_factor_ref 0.1707 _reflns_number_gt 1043 _reflns_number_total 1172 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file hg6090.cif _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' 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 ; _cod_database_code 2204515 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol S 0.8970(2) 1.08983(15) 0.38083(7) 0.0351(4) Uani d . 1 S O1 0.9854(11) 0.9625(6) 0.4097(3) 0.0727(17) Uani d . 1 O O2 1.0139(15) 1.1997(7) 0.4173(4) 0.115(3) Uani d . 1 O O3 0.6680(9) 1.0937(11) 0.3919(3) 0.113(3) Uani d . 1 O O4 0.9426(8) 1.0964(5) 0.3028(2) 0.0601(13) Uani d . 1 O O1B 0.2449(8) 0.7737(5) 0.3687(2) 0.0521(12) Uani d . 1 O H1 0.1294 0.8153 0.3654 0.078 Uiso calc R 1 H O1A 0.3372(7) 0.8776(4) 0.2665(2) 0.0484(11) Uani d . 1 O C1 0.3527(10) 0.7842(5) 0.3081(3) 0.0348(12) Uani d . 1 C C2 0.5051(9) 0.6633(5) 0.2972(3) 0.0339(12) Uani d . 1 C H2 0.4232 0.5770 0.3018 0.041 Uiso calc R 1 H N1 0.5922(8) 0.6736(5) 0.2243(2) 0.0386(11) Uani d . 1 N H1A 0.6823 0.6034 0.2162 0.058 Uiso calc R 1 H H1B 0.6637 0.7529 0.2195 0.058 Uiso calc R 1 H H1C 0.4834 0.6707 0.1930 0.058 Uiso calc R 1 H C3 0.6955(10) 0.6628(6) 0.3514(3) 0.0445(15) Uani d . 1 C H3A 0.8313 0.6545 0.3255 0.053 Uiso calc R 1 H H3B 0.6974 0.7502 0.3767 0.053 Uiso calc R 1 H C4 0.6799(10) 0.5474(7) 0.4048(3) 0.0402(14) Uani d . 1 C H4A 0.6739 0.4599 0.3797 0.048 Uiso calc R 1 H H4B 0.5467 0.5573 0.4320 0.048 Uiso calc R 1 H C5 0.8739(10) 0.5466(6) 0.4563(3) 0.0387(13) Uani d . 1 C H5A 1.0081 0.5514 0.4292 0.046 Uiso calc R 1 H H5B 0.8668 0.6269 0.4872 0.046 Uiso calc R 1 H N2 0.8728(8) 0.4213(5) 0.4996(2) 0.0411(11) Uani d . 1 N H2A 0.9861 0.4222 0.5291 0.062 Uiso calc R 1 H H2B 0.8809 0.3478 0.4712 0.062 Uiso calc R 1 H H2C 0.7506 0.4177 0.5249 0.062 Uiso calc R 1 H OW 0.8602(8) 0.9016(5) 0.2011(3) 0.0576(12) Uani d . 1 O HW1 0.8924 0.9492 0.2398 0.050 Uiso d . 1 H HW2 0.9610 0.8420 0.2106 0.050 Uiso d . 1 H 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 S 0.0301(6) 0.0376(7) 0.0377(7) 0.0008(6) -0.0022(6) -0.0016(6) O1 0.091(5) 0.066(3) 0.060(3) 0.023(3) 0.008(3) 0.007(3) O2 0.122(7) 0.079(4) 0.143(6) -0.001(4) -0.041(6) -0.062(4) O3 0.036(3) 0.242(10) 0.061(3) 0.025(5) 0.012(2) 0.048(5) O4 0.059(3) 0.071(3) 0.050(2) -0.009(3) 0.012(2) 0.001(2) O1B 0.050(3) 0.053(3) 0.054(3) 0.010(2) 0.013(2) 0.012(2) O1A 0.045(2) 0.038(2) 0.062(3) 0.0102(19) 0.004(2) 0.014(2) C1 0.034(3) 0.031(2) 0.040(3) -0.002(2) -0.002(2) 0.000(2) C2 0.031(3) 0.022(2) 0.050(3) -0.002(2) -0.010(3) 0.004(2) N1 0.033(2) 0.035(2) 0.048(2) 0.007(2) -0.006(2) -0.007(2) C3 0.041(3) 0.034(3) 0.059(4) -0.003(3) -0.020(3) 0.004(3) C4 0.030(3) 0.055(3) 0.036(3) -0.002(3) -0.006(2) 0.006(3) C5 0.038(3) 0.047(3) 0.032(2) -0.002(3) -0.003(3) 0.000(2) N2 0.035(2) 0.054(3) 0.034(2) 0.000(3) -0.006(2) 0.001(2) OW 0.047(2) 0.051(2) 0.075(3) 0.003(2) 0.003(2) -0.006(2) 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 O3 S O2 113.7(6) ? O3 S O1 109.8(5) ? O2 S O1 105.1(4) ? O3 S O4 109.2(3) ? O2 S O4 109.6(4) ? O1 S O4 109.3(3) ? C1 O1B H1 109.5 ? O1A C1 O1B 125.3(6) y O1A C1 C2 123.1(5) y O1B C1 C2 111.6(5) y N1 C2 C1 107.4(4) ? N1 C2 C3 109.4(5) ? C1 C2 C3 112.5(5) ? N1 C2 H2 109.2 ? C1 C2 H2 109.2 ? C3 C2 H2 109.2 ? C2 N1 H1A 109.5 ? C2 N1 H1B 109.5 ? H1A N1 H1B 109.5 ? C2 N1 H1C 109.5 ? H1A N1 H1C 109.5 ? H1B N1 H1C 109.5 ? C4 C3 C2 112.9(5) ? C4 C3 H3A 109.0 ? C2 C3 H3A 109.0 ? C4 C3 H3B 109.0 ? C2 C3 H3B 109.0 ? H3A C3 H3B 107.8 ? C3 C4 C5 111.9(5) ? C3 C4 H4A 109.2 ? C5 C4 H4A 109.2 ? C3 C4 H4B 109.2 ? C5 C4 H4B 109.2 ? H4A C4 H4B 107.9 ? N2 C5 C4 110.4(5) ? N2 C5 H5A 109.6 ? C4 C5 H5A 109.6 ? N2 C5 H5B 109.6 ? C4 C5 H5B 109.6 ? H5A C5 H5B 108.1 ? C5 N2 H2A 109.5 ? C5 N2 H2B 109.5 ? H2A N2 H2B 109.5 ? C5 N2 H2C 109.5 ? H2A N2 H2C 109.5 ? H2B N2 H2C 109.5 ? HW1 OW HW2 91.1 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag S O3 1.426(6) ? S O2 1.455(7) ? S O1 1.452(5) ? S O4 1.489(5) ? O1B C1 1.319(7) y O1B H1 0.8200 ? O1A C1 1.197(7) y C1 C2 1.514(8) ? C2 N1 1.469(7) ? C2 C3 1.550(8) ? C2 H2 0.9800 ? N1 H1A 0.8900 ? N1 H1B 0.8900 ? N1 H1C 0.8900 ? C3 C4 1.502(8) ? C3 H3A 0.9700 ? C3 H3B 0.9700 ? C4 C5 1.535(8) ? C4 H4A 0.9700 ? C4 H4B 0.9700 ? C5 N2 1.458(7) ? C5 H5A 0.9700 ? C5 H5B 0.9700 ? N2 H2A 0.8900 ? N2 H2B 0.8900 ? N2 H2C 0.8900 ? OW HW1 0.881 ? OW HW2 0.866 ? 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 O1B H1 O1 1_455 0.82 1.87 2.546(7) 139 N1 H1A O1A 4_645 0.89 2.21 2.903(6) 134 N1 H1A O4 4_745 0.89 2.34 3.003(7) 132 N1 H1B OW . 0.89 1.91 2.790(7) 169 N1 H1C O3 4_645 0.89 1.99 2.810(7) 153 N2 H2A O3 3_566 0.89 1.86 2.729(7) 165 N2 H2B O2 1_545 0.89 1.94 2.781(8) 158 N2 H2C O2 3_466 0.89 2.14 2.945(10) 150 N2 H2C O1 3_466 0.89 2.35 3.136(8) 148 OW HW1 O4 . 0.88 1.88 2.726(7) 162 OW HW2 O4 4_745 0.87 2.46 3.195(7) 143 OW HW2 O1A 1_655 0.87 2.57 3.191(7) 130 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 _geom_torsion_publ_flag O1A C1 C2 N1 -9.3(8) y O1B C1 C2 N1 171.8(5) y O1A C1 C2 C3 111.1(6) ? O1B C1 C2 C3 -67.8(7) ? N1 C2 C3 C4 -130.3(5) y C1 C2 C3 C4 110.4(6) y C2 C3 C4 C5 178.2(5) y C3 C4 C5 N2 -170.8(5) y