#------------------------------------------------------------------------------ #$Date: 2025-08-18 23:52:38 +0100 (Mon, 18 Aug 2025) $ #$Revision: 301791 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/60/2006075.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_2006075 loop_ _publ_author_name 'Castellari, C.' 'Ottani, S.' _publ_section_title ; Anti-Inflammatory Drugs. V. [Tris-(2-hydroxymethyl)methyl]ammonium 2-[(2,6-Dichlorophenyl)amino]phenylacetate (TRISH. D) ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 482 _journal_page_last 486 _journal_paper_doi 10.1107/S0108270196013649 _journal_volume 53 _journal_year 1997 _chemical_formula_moiety 'C4 H11 N O3' _chemical_formula_structural '(C H2 O H)3 C N H2' _chemical_formula_sum 'C4 H11 N O3' _chemical_formula_weight 121.14 _chemical_name_common TRIS _chemical_name_systematic ; Tris(2-hydroxymethyl)aminomethane ; _space_group_IT_number 33 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2c -2n' _symmetry_space_group_name_H-M 'P n a 21' _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 8.8435(10) _cell_length_b 8.7911(10) _cell_length_c 7.7906(10) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 25 _cell_measurement_theta_min 9 _cell_volume 605.67(12) _computing_cell_refinement 'CAD4 software' _computing_data_collection 'CAD4 software (Enraf-Nonius, 1989)' _computing_data_reduction 'MolEN (Fair, 1990)' _computing_molecular_graphics 'SCHAKAL92 (Keller, 1992)' _computing_publication_material SHELXL93 _computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _diffrn_ambient_temperature 298(2) _diffrn_measurement_device 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method 'profile data from \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_sigmaI/netI 0.0364 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 2527 _diffrn_reflns_theta_max 26.94 _diffrn_reflns_theta_min 3.27 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 160 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.112 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.328 _exptl_crystal_density_meas ? _exptl_crystal_description spherical _exptl_crystal_F_000 264 _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.30 _refine_diff_density_max 0.198 _refine_diff_density_min -0.174 _refine_ls_abs_structure_details 'Flack (1983)' _refine_ls_abs_structure_Flack -1.0(10) _refine_ls_extinction_coef none _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.042 _refine_ls_goodness_of_fit_obs 1.045 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 119 _refine_ls_number_reflns 1302 _refine_ls_number_restraints 26 _refine_ls_restrained_S_all 1.075 _refine_ls_restrained_S_obs 1.037 _refine_ls_R_factor_all 0.0352 _refine_ls_R_factor_obs 0.0320 _refine_ls_shift/esd_max -0.082 _refine_ls_shift/esd_mean 0.008 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0586P)^2^+0.0353P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.0883 _refine_ls_wR_factor_obs 0.0837 _reflns_number_observed 1259 _reflns_number_total 1307 _reflns_observed_criterion >2sigma(I) _cod_data_source_file na1262.cif _cod_data_source_block TRIS _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w = 1/[\s^2^(Fo^2^)+(0.0586P)^2^+0.0353P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1/[\s^2^(Fo^2^)+(0.0586P)^2^+0.0353P] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_database_code 2006075 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 C1 0.0229(5) -0.0003(4) 0.0020(4) 0.0290(5) -0.0056(4) 0.0315(5) N1 0.0323(5) 0.0010(4) 0.0018(4) 0.0367(5) 0.0012(4) 0.0369(5) C2 0.0268(5) 0.0006(4) 0.0082(5) 0.0311(6) -0.0108(5) 0.0536(8) C3 0.0276(5) 0.0018(5) -0.0016(5) 0.0430(6) -0.0122(5) 0.0369(6) C4 0.0269(5) -0.0040(5) 0.0009(4) 0.0340(5) -0.0016(5) 0.0420(6) O1 0.0241(4) -0.0015(4) 0.0021(4) 0.0577(6) 0.0049(4) 0.0384(5) O2 0.0309(5) -0.0071(4) 0.0268(6) 0.0425(5) -0.0196(6) 0.1069(11) O3 0.0298(5) 0.0154(5) -0.0028(4) 0.0905(8) -0.0009(5) 0.0344(5) loop_ _atom_site_label _atom_site_occupancy _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 _atom_site_refinement_flags _atom_site_type_symbol C1 1 0.29867(13) -0.03142(12) 0.81531(14) 0.0278(2) Uani d D C N1 1 0.35101(13) -0.13791(13) 0.94823(14) 0.0353(3) Uani d D N H1 1 0.4234(21) -0.1837(20) 0.9038(24) 0.043(4) Uiso d D H H2 1 0.2907(27) -0.2062(26) 0.9592(32) 0.074(7) Uiso d D H C2 1 0.15007(13) 0.03882(14) 0.8738(2) 0.0371(3) Uani d D C H3 1 0.1683(23) 0.0898(20) 0.9822(23) 0.046(5) Uiso d D H H4 1 0.1135(24) 0.1104(19) 0.7852(23) 0.044(4) Uiso d D H C3 1 0.27792(14) -0.11680(14) 0.6459(2) 0.0358(3) Uani d D C H5 1 0.3740(18) -0.1585(19) 0.6128(21) 0.036(4) Uiso d D H H6 1 0.2042(22) -0.1965(20) 0.6644(28) 0.055(5) Uiso d D H C4 1 0.41641(13) 0.09415(14) 0.7968(2) 0.0343(3) Uani d D C H7 1 0.3870(23) 0.1607(18) 0.7030(23) 0.045(4) Uiso d D H H8 1 0.4187(19) 0.1485(17) 0.9057(19) 0.036(4) Uiso d D H O1 1 0.56194(11) 0.03176(12) 0.76089(13) 0.0401(3) Uani d D O H9 1 0.5922(24) 0.0577(22) 0.6664(28) 0.049(5) Uiso d D H O2 1 0.04316(12) -0.07831(12) 0.8984(2) 0.0601(4) Uani d D O H10 1 -0.0328(23) -0.0434(23) 0.9320(34) 0.058(6) Uiso d D H O3 1 0.23145(12) -0.0183(2) 0.51105(14) 0.0516(3) Uani d D O H11 1 0.2888(22) -0.0270(21) 0.4267(27) 0.044(5) Uiso d D H 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' 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 N1 C1 C2 108.60(10) yes N1 C1 C4 108.20(10) yes C2 C1 C4 108.93(9) ? N1 C1 C3 109.40(10) yes C2 C1 C3 110.72(10) ? C4 C1 C3 110.84(10) ? C1 N1 H1 104.9(13) ? C1 N1 H2 109.9(18) ? H1 N1 H2 101.(2) ? O2 C2 C1 108.86(9) ? O2 C2 H3 109.3(12) ? C1 C2 H3 107.8(12) ? O2 C2 H4 109.9(12) ? C1 C2 H4 109.4(12) ? H3 C2 H4 111.6(15) ? O3 C3 C1 111.92(10) ? O3 C3 H5 106.8(10) ? C1 C3 H5 108.2(10) ? O3 C3 H6 110.8(13) ? C1 C3 H6 108.0(13) ? H5 C3 H6 111.0(15) ? O1 C4 C1 110.88(10) ? O1 C4 H7 109.0(12) ? C1 C4 H7 109.0(12) ? O1 C4 H8 109.9(10) ? C1 C4 H8 106.7(9) ? H7 C4 H8 111.4(13) ? C4 O1 H9 111.4(15) ? C2 O2 H10 109.5(15) ? C3 O3 H11 110.5(14) ? 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 C1 N1 . 1.471(2) yes C1 C2 . 1.522(1) yes C1 C4 . 1.524(2) yes C1 C3 . 1.529(2) yes N1 H1 . 0.83(2) ? N1 H2 . 0.81(2) ? C2 O2 . 1.411(2) yes C2 H3 . 0.97(2) ? C2 H4 . 0.99(2) ? C3 O3 . 1.422(2) yes C3 H5 . 0.961(15) ? C3 H6 . 0.97(2) ? C4 O1 . 1.427(2) yes C4 H7 . 0.97(2) ? C4 H8 . 0.974(14) ? O1 H9 . 0.82(2) ? O2 H10 . 0.78(2) ? O3 H11 . 0.83(2) ? 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 N1 C1 C2 O2 -59.69(15) C4 C1 C2 O2 -177.37(12) C3 C1 C2 O2 60.5(2) N1 C1 C3 O3 -178.30(9) C2 C1 C3 O3 61.99(12) C4 C1 C3 O3 -59.01(12) N1 C1 C4 O1 55.54(13) C2 C1 C4 O1 173.48(11) C3 C1 C4 O1 -64.48(13) loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 ChemSpider 6257 2 PubChem 6503