#------------------------------------------------------------------------------ #$Date: 2012-02-03 17:16:24 +0000 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/15/2011565.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_2011565 loop_ _publ_author_name 'Kruger, Paul E.' 'Mackie, Philip R.' 'Nieuwenhuyzen, Mark' _publ_section_title ; Redetermination of 1,3,5-trichloro-2,4-dinitrobenzene ; _journal_issue 11 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first e532 _journal_page_last e532 _journal_volume 56 _journal_year 2000 _chemical_formula_moiety 'C6 H1 Cl3 N2 O4 ' _chemical_formula_sum 'C6 H Cl3 N2 O4' _chemical_formula_weight 271.44 _chemical_name_common 1,3,5-Trichloro-2,4-dinitrobenzene _chemical_name_systematic 1,3,5-Trichloro-2,4-dinitrobenzene _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' _cell_angle_alpha 90.00 _cell_angle_beta 91.76(4) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 7.933(7) _cell_length_b 9.328(6) _cell_length_c 12.814(9) _cell_measurement_reflns_used 999 _cell_measurement_temperature 153(2) _cell_measurement_theta_max 25 _cell_measurement_theta_min 2 _cell_volume 947.8(12) _computing_cell_refinement SMART _computing_data_collection 'SMART (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999)' _computing_structure_refinement SHELXTL _computing_structure_solution 'SHELXTL (Bruker, 1998)' _diffrn_ambient_temperature 153(2) _diffrn_measured_fraction_theta_full .994 _diffrn_measured_fraction_theta_max .994 _diffrn_measurement_device_type 'Bruker AXS SMART' _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 .71073 _diffrn_reflns_av_R_equivalents .074 _diffrn_reflns_av_sigmaI/netI .0766 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 5687 _diffrn_reflns_theta_full 26.46 _diffrn_reflns_theta_max 26.46 _diffrn_reflns_theta_min 2.57 _diffrn_standards_decay_% none _exptl_absorpt_coefficient_mu .96 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.902 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 732 _exptl_crystal_size_max .36 _exptl_crystal_size_mid .28 _exptl_crystal_size_min .26 _refine_diff_density_max .768 _refine_diff_density_min -.486 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref .889 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 136 _refine_ls_number_reflns 1942 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all .889 _refine_ls_R_factor_all .082 _refine_ls_R_factor_gt .054 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0729P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .154 _reflns_number_gt 1315 _reflns_number_total 1942 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file qd0039.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/c' _[local]_cod_chemical_formula_sum_orig 'C6 H1 Cl3 N2 O4' _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: '_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 2011565 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -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_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Cl1 .49373(14) .23165(12) .09129(8) .0378(3) Uani d . 1 . . Cl C1 .7276(5) .0237(4) .0908(3) .0259(9) Uani d . 1 . . C H1 .7173 .0267 .0167 .031 Uiso calc R 1 . . H Cl2 .95696(14) -.18278(12) .06791(9) .0364(3) Uani d . 1 . . Cl C2 .8371(5) -.0705(4) .1404(3) .0253(9) Uani d . 1 . . C Cl3 .77463(13) .01355(11) .44296(7) .0296(3) Uani d . 1 . . Cl C3 .8524(5) -.0747(4) .2492(3) .0230(8) Uani d . 1 . . C C4 .7576(5) .0175(4) .3092(3) .0237(9) Uani d . 1 . . C C5 .6486(5) .1104(4) .2583(3) .0244(9) Uani d . 1 . . C C6 .6325(5) .1143(4) .1518(3) .0253(9) Uani d . 1 . . C N11 .9690(5) -.1741(4) .3008(3) .0351(9) Uani d . 1 . . N O11 1.0971(4) -.1258(4) .3409(3) .0535(10) Uani d . 1 . . O O12 .9280(5) -.3001(4) .3011(3) .0535(10) Uani d . 1 . . O O21 .6000(5) .3267(3) .3372(3) .0492(9) Uani d . 1 . . O N22 .5451(4) .2070(4) .3213(3) .0296(8) Uani d . 1 . . N O22 .4143(4) .1598(4) .3533(3) .0428(9) Uani d . 1 . . O 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 Cl1 .0428(7) .0377(7) .0326(6) .0123(5) -.0060(5) .0087(5) C1 .028(2) .028(2) .021(2) -.0068(17) -.0009(17) .0016(17) Cl2 .0401(7) .0344(6) .0351(6) .0060(5) .0056(5) -.0103(5) C2 .028(2) .017(2) .030(2) -.0019(16) .0019(17) -.0060(17) Cl3 .0373(6) .0285(6) .0228(5) .0044(4) -.0043(4) -.0006(4) C3 .026(2) .0158(19) .027(2) .0009(15) -.0060(16) -.0012(16) C4 .027(2) .023(2) .0214(19) -.0018(16) -.0037(16) .0020(16) C5 .025(2) .018(2) .030(2) .0018(16) -.0011(17) -.0020(16) C6 .025(2) .023(2) .028(2) -.0008(16) -.0069(16) .0053(17) N11 .041(2) .031(2) .033(2) .0121(17) -.0020(18) -.0061(16) O11 .042(2) .056(2) .061(2) .0120(18) -.0219(18) -.0105(19) O12 .064(2) .0270(18) .068(3) .0134(17) -.009(2) .0046(17) O21 .067(2) .0243(18) .057(2) .0037(16) .0147(19) -.0063(16) N22 .034(2) .031(2) .0242(18) .0077(16) -.0030(15) .0002(15) O22 .0324(18) .054(2) .0422(19) .0031(15) .0072(15) -.0058(16) 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 Cl1 C6 . 1.720(4) ? C1 C2 . 1.378(6) ? C1 C6 . 1.389(5) ? Cl2 C2 . 1.708(4) ? C2 C3 . 1.396(6) ? Cl3 C4 . 1.716(4) ? C3 C4 . 1.390(5) ? C3 N11 . 1.455(5) ? C4 C5 . 1.374(5) ? C5 C6 . 1.367(6) ? C5 N22 . 1.476(5) ? N11 O11 . 1.211(5) ? N11 O12 . 1.220(5) ? O21 N22 . 1.214(5) ? N22 O22 . 1.210(5) ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl .1484 .1585 '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 C2 C1 C6 118.3(4) C1 C2 C3 120.8(4) C1 C2 Cl2 119.6(3) C3 C2 Cl2 119.5(3) C4 C3 C2 120.2(4) C4 C3 N11 119.3(3) C2 C3 N11 120.4(3) C5 C4 C3 118.1(4) C5 C4 Cl3 121.1(3) C3 C4 Cl3 120.8(3) C6 C5 C4 121.9(4) C6 C5 N22 119.5(3) C4 C5 N22 118.5(3) C5 C6 C1 120.7(4) C5 C6 Cl1 120.4(3) C1 C6 Cl1 119.0(3) O11 N11 O12 125.3(4) O11 N11 C3 118.0(4) O12 N11 C3 116.7(4) O22 N22 O21 125.8(3) O22 N22 C5 117.5(3) O21 N22 C5 116.8(3)