#------------------------------------------------------------------------------ #$Date: 2011-09-17 22:27:16 +0200 (Sat, 17 Sep 2011) $ #$Revision: 26029 $ #$URL: svn://www.crystallography.net/cod/cif/2/2100663.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_2100663 loop_ _publ_author_name 'Marcin Podsiad{\l}o' 'Andrzej Katrusiak' _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 _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 _cell_angle_alpha 90.00 _cell_angle_beta 96.13(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 5.1285(10) _cell_length_b 11.377(2) _cell_length_c 9.859(2) _cell_measurement_reflns_used 3388 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 29 _cell_measurement_theta_min 4 _cell_volume 572.0(2) _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 0.333 _diffrn_measured_fraction_theta_max 0.333 _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 0.1124 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 4612 _diffrn_reflns_theta_full 29.66 _diffrn_reflns_theta_max 29.66 _diffrn_reflns_theta_min 4.16 _exptl_absorpt_coefficient_mu 1.449 _exptl_absorpt_correction_T_max 0.69 _exptl_absorpt_correction_T_min 0.27 _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 1.712 _exptl_crystal_density_method 'not measured' _exptl_crystal_description cylinder _exptl_crystal_F_000 296 _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.18 _refine_diff_density_max 0.284 _refine_diff_density_min -0.253 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 77 _refine_ls_number_reflns 538 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.021 _refine_ls_R_factor_all 0.0718 _refine_ls_R_factor_gt 0.0607 _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^)+(0.1230P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1510 _refine_ls_wR_factor_ref 0.1616 _reflns_number_gt 438 _reflns_number_total 538 _reflns_threshold_expression >4sigma(I) _[local]_cod_data_source_file av5065.cif _[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_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 2100663 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 0.2569(2) 0.0380(3) 0.85765(13) 0.061(3) Uani d 1 Cl Cl1 -0.2556(2) 0.1043(3) 0.52835(11) 0.063(3) Uani d 1 Cl Cl2 -0.2749(2) 0.3236(4) 0.74693(11) 0.057(2) Uani d 1 C C2 -0.0030(7) 0.2309(11) 0.7396(4) 0.041(7) Uani d 1 H H2A 0.180(5) 0.275(7) 0.771(3) 0.003(6) Uiso d 1 C C3 -0.0268(8) 0.1287(11) 0.8420(4) 0.044(7) Uani d 1 H H3A -0.213(11) 0.049(11) 0.846(5) 0.067(19) Uiso d 1 H H3B -0.047(8) 0.137(13) 0.931(5) 0.053(13) Uiso d 1 C C1 0.0229(9) 0.1851(13) 0.5959(5) 0.044(6) Uani d 1 H H1A 0.189(11) 0.126(11) 0.577(5) 0.051(13) Uiso d 1 H H1B 0.042(11) 0.242(17) 0.547(7) 0.07(2) 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 0.0506(7) 0.057(8) 0.0751(8) 0.0153(12) -0.0023(5) 0.0107(12) Cl1 0.0614(7) 0.070(8) 0.0539(7) 0.0031(13) -0.0066(5) -0.0111(10) Cl2 0.0554(7) 0.049(7) 0.0671(8) 0.0088(12) 0.0101(5) -0.0048(11) C2 0.0362(18) 0.04(2) 0.050(2) -0.003(4) 0.0021(14) 0.000(4) C3 0.051(2) 0.04(2) 0.047(2) -0.001(4) 0.0092(15) 0.005(4) C1 0.050(2) 0.03(2) 0.049(2) 0.001(4) 0.0098(17) 0.003(4) 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 C1 C2 C3 111.5(10) C1 C2 Cl2 113.0(4) C3 C2 Cl2 107.8(3) C1 C2 H2A 105.5(17) C3 C2 H2A 107(3) Cl2 C2 H2A 112(4) C2 C3 Cl3 111.8(3) C2 C3 H3A 130(3) Cl3 C3 H3A 101(4) C2 C3 H3B 126(9) Cl3 C3 H3B 99(5) H3A C3 H3B 83(7) C2 C1 Cl1 112.3(4) C2 C1 H1A 120(2) Cl1 C1 H1A 103(4) C2 C1 H1B 108(10) Cl1 C1 H1B 109(6) H1A C1 H1B 104(9) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Cl3 C3 1.776(9) Cl1 C1 1.768(9) Cl2 C2 1.756(9) C2 C1 1.529(9) C2 C3 1.554(14) C2 H2A 1.08(4) C3 H3A 1.32(10) C3 H3B 0.90(5) C1 H1A 1.12(9) C1 H1B 0.82(16) 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 62.0(5) Cl2 C2 C3 Cl3 -173.4(4) C3 C2 C1 Cl1 62.3(7) Cl2 C2 C1 Cl1 -59.4(11)