#------------------------------------------------------------------------------ #$Date: 2011-09-10 05:16:28 +0200 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2100662.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_2100662 loop_ _publ_author_name 'Podsiad\/lo, Marcin' 'Katrusiak, Andrzej' _publ_section_title ; Pressure-frozen 1,2,3-trichloropropane ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 1071 _journal_page_last 1077 _journal_volume 62 _journal_year 2006 _chemical_formula_moiety C3H5Cl3 _chemical_formula_sum 'C3 H5 Cl3' _chemical_formula_weight 147.42 _chemical_melting_point 259 _chemical_name_common 1,2,3-trichloropropane _chemical_name_systematic ; 1,2,3-trichloropropane ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 96.21(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 5.1404(10) _cell_length_b 11.363(2) _cell_length_c 9.885(2) _cell_measurement_reflns_used 3519 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 30 _cell_measurement_theta_min 3 _cell_volume 574.00(19) _computing_cell_refinement 'CrysAlis (Oxford Diffraction, 2004)' _computing_data_collection 'CrysAlis (Oxford Diffraction, 2004)' _computing_data_reduction 'CrysAlis (Oxford Diffraction, 2004)' _computing_molecular_graphics 'XP (Siemens, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.402 _diffrn_measured_fraction_theta_max 0.402 _diffrn_measurement_device_type 'Kuma KM4CCD \k geometry' _diffrn_measurement_method '\w scans' _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 0.0823 _diffrn_reflns_av_sigmaI/netI 0.0386 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 4431 _diffrn_reflns_theta_full 30.11 _diffrn_reflns_theta_max 30.11 _diffrn_reflns_theta_min 2.74 _exptl_absorpt_coefficient_mu 1.444 _exptl_absorpt_correction_T_max 0.61 _exptl_absorpt_correction_T_min 0.20 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; Katrusiak, A. (2003). REDSHADE - Program for correcting reflections intensities for DAC absorption, gasket shadowing and sample crystal absorption. Adam Mickiewicz University, Pozna\'n. Katrusiak, A. (2004). Z. Kristallogr. 219, 461-467 ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.706 _exptl_crystal_density_method 'not measured' _exptl_crystal_description cylinder _exptl_crystal_F_000 296 _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.26 _refine_diff_density_max 0.322 _refine_diff_density_min -0.340 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 77 _refine_ls_number_reflns 679 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.033 _refine_ls_R_factor_all 0.0798 _refine_ls_R_factor_gt 0.0625 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1174P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1508 _refine_ls_wR_factor_ref 0.1668 _reflns_number_gt 520 _reflns_number_total 679 _reflns_threshold_expression >4sigma(I) _[local]_cod_data_source_file av5065.cif _[local]_cod_data_source_block 1tcp _[local]_cod_cif_authors_sg_H-M 'P 2(1) / n' _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_original_cell_volume 574.0(2) _cod_database_code 2100662 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_type_symbol _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_occupancy Cl Cl3 0.25665(19) 0.0386(2) 0.85740(13) 0.0608(14) Uani d 1 Cl Cl1 -0.2553(2) 0.1045(2) 0.52854(10) 0.0575(13) Uani d 1 Cl Cl2 -0.27487(19) 0.3235(3) 0.74680(10) 0.0518(14) Uani d 1 C C2 0.0000(7) 0.2277(9) 0.7403(4) 0.033(4) Uani d 1 H H2A 0.159(6) 0.253(7) 0.769(3) 0.020(8) Uiso d 1 C C3 -0.0271(8) 0.1301(9) 0.8416(4) 0.048(4) Uani d 1 H H3A -0.176(11) 0.052(9) 0.823(5) 0.066(16) Uiso d 1 H H3B -0.032(7) 0.179(8) 0.924(4) 0.039(11) Uiso d 1 C C1 0.0201(8) 0.1870(10) 0.5959(4) 0.048(4) Uani d 1 H H1A 0.167(10) 0.139(10) 0.586(4) 0.054(14) Uiso d 1 H H1B 0.039(9) 0.260(11) 0.539(5) 0.057(16) Uiso d 1 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 Cl3 0.0493(6) 0.053(5) 0.0782(9) 0.0134(10) -0.0036(5) 0.0111(10) Cl1 0.0621(7) 0.054(4) 0.0535(7) 0.0042(10) -0.0076(4) -0.0087(8) Cl2 0.0564(7) 0.034(4) 0.0655(7) 0.0119(9) 0.0095(5) -0.0011(7) C2 0.0378(17) 0.006(13) 0.055(2) -0.005(3) 0.0010(14) 0.000(3) C3 0.050(2) 0.053(14) 0.042(2) 0.004(4) 0.0067(15) 0.006(3) C1 0.046(2) 0.051(13) 0.048(2) -0.010(4) 0.0079(15) -0.001(3) 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' Cl Cl 0.1484 0.1585 '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 C3 C2 C1 114.9(8) C3 C2 Cl2 107.1(3) C1 C2 Cl2 110.7(4) C3 C2 H2A 100(4) C1 C2 H2A 104(2) Cl2 C2 H2A 120(4) C2 C3 Cl3 110.7(3) C2 C3 H3A 124(3) Cl3 C3 H3A 95(4) C2 C3 H3B 99(5) Cl3 C3 H3B 110(3) H3A C3 H3B 119(5) C2 C1 Cl1 112.6(3) C2 C1 H1A 114(3) Cl1 C1 H1A 106(5) C2 C1 H1B 107(5) Cl1 C1 H1B 110(3) H1A C1 H1B 107(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Cl3 C3 1.784(7) Cl1 C1 1.766(7) Cl2 C2 1.791(7) C2 C3 1.510(10) C2 C1 1.515(7) C2 H2A 0.88(4) C3 H3A 1.17(8) C3 H3B 0.99(6) C1 H1A 0.95(8) C1 H1B 1.01(10) 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 C1 C2 C3 Cl3 63.2(5) Cl2 C2 C3 Cl3 -173.4(3) C3 C2 C1 Cl1 59.2(6) Cl2 C2 C1 Cl1 -62.2(8)