#------------------------------------------------------------------------------ #$Date: 2015-04-02 12:22:18 +0100 (Thu, 02 Apr 2015) $ #$Revision: 134621 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/72/2007201.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_2007201 loop_ _publ_author_name 'Ravichandran, S.' 'Dattagupta, J. K.' 'Chakrabarti, Chandana' _publ_section_title ; D-Phenylglycine Hydrochloride ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 499 _journal_page_last 501 _journal_paper_doi 10.1107/S0108270197014674 _journal_volume 54 _journal_year 1998 _chemical_formula_iupac 'C8 H10 N O2 + , Cl -' _chemical_formula_moiety 'C8 H10 Cl N O2' _chemical_formula_sum 'C8 H10 Cl N O2' _chemical_formula_weight 187.625 _chemical_name_common 'D-PHENYLGLYCINE HYDROCHLORIDE' _chemical_name_systematic ; D-\a-Aminophenyl acetic acid hydrochloride ; _space_group_IT_number 19 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 5.4376(5) _cell_length_b 7.2577(8) _cell_length_c 22.773(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 25 _cell_measurement_theta_min 3 _cell_volume 898.72(15) _computing_cell_refinement 'CAD-4 software' _computing_data_collection 'CAD-4 software (Enraf Nonius, 1989)' _computing_data_reduction 'SDP (Enraf Nonius, 1985)' _computing_molecular_graphics 'ORTEX2.1a (McArdle, 1993) ' _computing_publication_material SHELXL93 _computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1985)' _diffrn_ambient_temperature 293(2) _diffrn_measurement_device CAD4 _diffrn_measurement_method \w/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0205 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 964 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_min 3 _diffrn_standards_decay_% 'not significant' _diffrn_standards_interval_count 200 _diffrn_standards_interval_time 120 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.383 _exptl_absorpt_correction_T_max 0.909 _exptl_absorpt_correction_T_min 0.784 _exptl_absorpt_correction_type 'empirical \y scan' _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.387 _exptl_crystal_density_meas 1.365 _exptl_crystal_density_method 'by flotation in benzene-bromoform mixture' _exptl_crystal_description needle-shaped _exptl_crystal_F_000 392 _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _refine_diff_density_max 0.255 _refine_diff_density_min -0.277 _refine_ls_abs_structure_details 'Flack (1983)' _refine_ls_abs_structure_Flack -0.01(16) _refine_ls_extinction_coef 0.027(6) _refine_ls_extinction_method SHELXL93 _refine_ls_goodness_of_fit_all 0.768 _refine_ls_goodness_of_fit_obs 0.747 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 110 _refine_ls_number_reflns 961 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.838 _refine_ls_restrained_S_obs 0.747 _refine_ls_R_factor_all 0.045 _refine_ls_R_factor_obs .035 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1109P)^2^+0.8971P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.127 _refine_ls_wR_factor_obs .106 _reflns_number_observed 853 _reflns_number_total 964 _reflns_observed_criterion >2sigma(I) _[local]_cod_data_source_file vj1074.cif _[local]_cod_data_source_block TOZ _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w = 1/[\s^2^(Fo^2^)+(0.1109P)^2^+0.8971P] 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^)+(0.1109P)^2^+0.8971P] 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 2007201 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_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 Cl .0357(5) .0350(5) .0400(5) -.0093(4) .0019(4) -.0013(4) O1 .0258(13) .0403(14) .058(2) .0048(13) .0099(12) -.0011(14) O2 .054(2) .0315(14) .070(2) .0105(14) .019(2) .0061(14) N .0330(15) .0372(15) .0296(14) .008(2) .0041(12) .0049(12) C1 .048(2) .031(2) .035(2) .009(2) .005(2) .0016(14) C2 .037(2) .039(2) .040(2) .000(2) .012(2) .005(2) C3 .0222(15) .035(2) .040(2) -.003(2) .0013(15) .002(2) C4 .028(2) .0228(15) .035(2) .007(2) .001(2) .0034(13) C5 .027(2) .032(2) .039(2) -.006(2) .0016(15) .000(2) C6 .043(2) .031(2) .039(2) -.005(2) -.004(2) -.005(2) C7 .0198(15) .0290(15) .033(2) .005(2) .0015(14) -.0003(13) C8 .033(2) .031(2) .031(2) .009(2) -.0032(15) -.0053(14) 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_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol Cl .2276(2) .83340(12) .18557(4) .0369(3) Uani d . 1 . Cl O1 .6260(5) .8320(4) .30352(12) .0414(7) Uani d . 1 . O O2 .3804(6) .6195(4) .34412(14) .0517(9) Uani d . 1 . O H4 .4956(6) .5500(4) .33706(14) .062 Uiso calc R 1 . H N .2608(6) 1.0866(4) .30195(12) .0333(7) Uani d . 1 . N H8 .1387(6) 1.1656(4) .30868(12) .040 Uiso calc R 1 . H H9 .2609(6) 1.0549(4) .26420(12) .040 Uiso calc R 1 . H H10 .4036(6) 1.1395(4) .31093(12) .040 Uiso calc R 1 . H C1 .2201(8) 1.0109(5) .5246(2) .0381(9) Uani d . 1 . C H1 .2210(8) 1.0263(5) .5652(2) .046 Uiso calc R 1 . H C2 .0274(7) .9189(5) .4980(2) .0385(9) Uani d . 1 . C H2 -.1022(7) .8739(5) .5204(2) .046 Uiso calc R 1 . H C3 .0281(6) .8940(5) .4374(2) .0323(8) Uani d . 1 . C H3 -.1007(6) .8317(5) .4193(2) .039 Uiso calc R 1 . H C4 .2201(6) .9619(4) .40430(15) .0283(7) Uani d . 1 . C C5 .4112(7) 1.0557(5) .4312(2) .0324(8) Uani d . 1 . C H5 .5400(7) 1.1026(5) .4089(2) .039 Uiso calc R 1 . H C6 .4092(8) 1.0792(5) .4917(2) .0378(9) Uani d . 1 . C H6 .5374(8) 1.1419(5) .5100(2) .045 Uiso calc R 1 . H C7 .2259(6) .9188(5) .33889(14) .0274(7) Uani d . 1 . C H7 .0704(6) .8599(5) .32788(14) .033 Uiso calc R 1 . H C8 .4351(7) .7868(5) .32608(15) .0320(8) Uani d . 1 . C 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' O O 0.0106 0.0060 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 -4 3 1 -4 1 -1 -3 -2 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C8 O2 H4 109.5(2) C7 N H8 109.5(2) C7 N H9 109.5(2) H8 N H9 109.5 C7 N H10 109.5(2) H8 N H10 109.5 H9 N H10 109.5 C6 C1 C2 120.3(3) C6 C1 H1 119.8(2) C2 C1 H1 119.8(2) C1 C2 C3 119.7(3) C1 C2 H2 120.1(2) C3 C2 H2 120.1(2) C4 C3 C2 119.9(3) C4 C3 H3 120.1(2) C2 C3 H3 120.1(2) C5 C4 C3 120.1(3) C5 C4 C7 121.2(3) C3 C4 C7 118.5(3) C6 C5 C4 119.6(3) C6 C5 H5 120.2(2) C4 C5 H5 120.2(2) C1 C6 C5 120.4(4) C1 C6 H6 119.8(2) C5 C6 H6 119.8(2) N C7 C8 108.2(3) N C7 C4 112.7(3) C8 C7 C4 109.5(3) N C7 H7 108.8(2) C8 C7 H7 108.8(2) C4 C7 H7 108.8(2) O1 C8 O2 125.4(4) O1 C8 C7 123.8(3) O2 C8 C7 110.7(3) 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 C8 . 1.203(5) ? O2 C8 . 1.316(5) ? O2 H4 . .82 ? N C7 . 1.492(4) ? N H8 . .89 ? N H9 . .89 ? N H10 . .89 ? C1 C6 . 1.365(6) ? C1 C2 . 1.383(6) ? C1 H1 . .93 ? C2 C3 . 1.390(5) ? C2 H2 . .93 ? C3 C4 . 1.379(5) ? C3 H3 . .93 ? C4 C5 . 1.385(5) ? C4 C7 . 1.522(5) ? C5 C6 . 1.389(5) ? C5 H5 . .93 ? C6 H6 . .93 ? C7 C8 . 1.516(5) ? C7 H7 . .98 ? 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_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA N H9 Cl 1_555 2.41 3.230(3) 152 O2 H4 Cl 4_645 2.23 3.051(3) 172 N H8 Cl 4_555 2.33 3.216(3) 168 N H10 Cl 4_655 2.45 3.321(3) 165 N H9 O1 4_655 2.60 3.053(4) 111 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 C6 C1 C2 C3 0.8(6) C1 C2 C3 C4 -0.3(5) C2 C3 C4 C5 -0.4(5) C2 C3 C4 C7 175.1(3) C3 C4 C5 C6 0.6(5) C7 C4 C5 C6 -174.7(3) C2 C1 C6 C5 -0.6(6) C4 C5 C6 C1 -0.1(6) C5 C4 C7 N -55.4(4) C3 C4 C7 N 129.2(3) C5 C4 C7 C8 65.0(4) C3 C4 C7 C8 -110.4(3) N C7 C8 O1 18.9(5) C4 C7 C8 O1 -104.3(4) N C7 C8 O2 -162.5(3) C4 C7 C8 O2 74.3(4)