#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2006291.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_2006291 loop_ _publ_author_name 'Griesbaum, K.' 'McCullough, K. J.' 'Perner, I.' 'Quinkert, R.-O.' 'Rosair, G. M.' _publ_section_title ; (E)-3,5-Dichloro-3,5-bis(chloromethyl)-1,2,4-trioxolane ; _journal_issue 7 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 911 _journal_page_last 913 _journal_volume 53 _journal_year 1997 _chemical_formula_moiety 'C4 H4 Cl4 O3' _chemical_formula_sum 'C4 H4 Cl4 O3' _chemical_formula_weight 241.87 _chemical_melting_point 314 _chemical_name_systematic ; E-3,5-Dichloro-3,5-bis(chloromethyl)-1,2,4-trioxolane ; _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' _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 115.810(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 10.732(2) _cell_length_b 8.9450(10) _cell_length_c 10.1450(10) _cell_measurement_reflns_used 11 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 12.49 _cell_measurement_theta_min 12.15 _cell_volume 876.7(2) _computing_cell_refinement XSCANS _computing_data_collection 'XSCANS (Siemens, 1994)' _computing_data_reduction XSCANS _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXTL/PC _computing_structure_refinement SHELXTL/PC _computing_structure_solution 'SHELXTL/PC (Sheldrick, 1994)' _diffrn_ambient_temperature 293(2) _diffrn_measurement_device 'Siemens P4' _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 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0302 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_number 2884 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_min 2.11 _diffrn_standards_decay_% 8.4 _diffrn_standards_interval_count 97 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.304 _exptl_absorpt_correction_T_max 0.634 _exptl_absorpt_correction_T_min 0.570 _exptl_absorpt_correction_type 'empirical via \y scans (XSCANS: Siemens, 1994)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.832 _exptl_crystal_density_method none _exptl_crystal_description block _exptl_crystal_F_000 480 _exptl_crystal_size_max 0.57 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.35 _refine_diff_density_max 0.268 _refine_diff_density_min -0.240 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.061 _refine_ls_goodness_of_fit_obs 1.096 _refine_ls_hydrogen_treatment 'H atoms riding (see text)' _refine_ls_matrix_type full _refine_ls_number_parameters 100 _refine_ls_number_reflns 1235 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.061 _refine_ls_restrained_S_obs 1.096 _refine_ls_R_factor_all 0.0487 _refine_ls_R_factor_obs 0.0362 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w = 1/[\s^2^(Fo^2^)+(0.0455P)^2^+0.4456P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_all 0.0950 _refine_ls_wR_factor_obs 0.0873 _reflns_number_observed 995 _reflns_number_total 1235 _reflns_observed_criterion >2sigma(I) _[local]_cod_data_source_file cf1150.cif _[local]_cod_data_source_block ip2ab _[local]_cod_cif_authors_sg_H-M P21/c _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_database_code 2006291 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_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 0.0554(5) 0.0532(4) 0.0634(8) -0.0030(3) 0.0397(5) 0.0022(5) Cl2 0.0509(4) 0.0747(6) 0.0733(9) 0.0015(4) 0.0385(5) -0.0061(6) Cl3 0.0833(6) 0.0497(5) 0.1299(13) -0.0150(4) 0.0692(7) 0.0034(6) Cl4 0.0848(6) 0.0506(5) 0.0720(9) -0.0009(4) 0.0341(6) 0.0155(5) O1 0.0450(11) 0.0443(11) 0.042(2) -0.0002(9) 0.0158(11) -0.0055(11) O2 0.0475(11) 0.0466(11) 0.041(2) 0.0070(9) 0.0214(12) 0.0090(11) O3 0.0409(10) 0.0371(10) 0.036(2) 0.0017(8) 0.0147(10) -0.0031(10) C1 0.0404(14) 0.0390(14) 0.036(3) 0.0000(12) 0.021(2) 0.003(2) C2 0.0420(14) 0.045(2) 0.036(2) 0.0008(13) 0.020(2) -0.001(2) C3 0.057(2) 0.037(2) 0.070(3) 0.0007(13) 0.037(2) 0.005(2) C4 0.059(2) 0.042(2) 0.060(3) 0.0099(14) 0.019(2) -0.001(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_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol Cl1 0.04013(8) 0.12393(9) 0.40401(12) 0.0524(3) Uani d . 1 Cl Cl2 0.41882(8) 0.02013(11) 0.25996(13) 0.0622(4) Uani d . 1 Cl Cl3 0.32703(11) 0.39763(10) 0.3223(2) 0.0795(5) Uani d . 1 Cl Cl4 0.21114(10) -0.23670(10) 0.46382(13) 0.0692(4) Uani d . 1 Cl O1 0.1573(2) -0.0245(2) 0.2027(3) 0.0449(7) Uani d . 1 O O2 0.1231(2) 0.1349(2) 0.1953(3) 0.0441(7) Uani d . 1 O O3 0.2870(2) 0.0830(2) 0.4174(2) 0.0385(6) Uani d . 1 O C1 0.1692(3) 0.1703(3) 0.3425(4) 0.0368(9) Uani d . 1 C C2 0.2880(3) -0.0265(3) 0.3203(4) 0.0397(10) Uani d . 1 C C3 0.1940(3) 0.3363(3) 0.3666(5) 0.0513(11) Uani d . 1 C H3A 0.2186(3) 0.3596(3) 0.4683(5) 0.077 Uiso calc R 1 H H3B 0.1093(3) 0.3895(3) 0.3066(5) 0.077 Uiso calc R 1 H C4 0.3214(3) -0.1823(4) 0.3858(5) 0.0562(12) Uani d . 1 C H4B 0.4165(3) -0.1846(4) 0.4603(5) 0.084 Uiso calc R 1 H H4A 0.3130(3) -0.2530(4) 0.3099(5) 0.084 Uiso calc R 1 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' O O 0.0106 0.0060 '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 _geom_angle_publ_flag C2 O1 O2 101.1(2) y C1 O2 O1 101.7(2) y C2 O3 C1 107.0(2) y O2 C1 O3 105.8(3) y O2 C1 C3 110.7(3) y O3 C1 C3 114.1(2) y O2 C1 Cl1 110.6(2) y O3 C1 Cl1 109.5(2) y C3 C1 Cl1 106.2(3) y O1 C2 O3 106.4(2) y O1 C2 C4 110.2(3) y O3 C2 C4 114.1(3) y O1 C2 Cl2 110.4(3) y O3 C2 Cl2 108.9(2) y C4 C2 Cl2 106.8(2) y C1 C3 Cl3 111.8(3) y C2 C4 Cl4 112.0(3) y loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Cl1 C1 1.798(3) y Cl2 C2 1.807(4) y Cl3 C3 1.760(4) y Cl4 C4 1.755(4) y O1 C2 1.391(4) y O1 O2 1.465(3) y O2 C1 1.390(4) y O3 C2 1.392(4) y O3 C1 1.396(3) y C1 C3 1.510(4) y C2 C4 1.518(4) y 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 _geom_torsion_publ_flag C2 O1 O2 C1 -42.2(3) n O1 O2 C1 O3 34.8(3) n O1 O2 C1 C3 158.8(2) n O1 O2 C1 Cl1 -83.7(2) n C2 O3 C1 O2 -14.4(3) n C2 O3 C1 C3 -136.3(3) n C2 O3 C1 Cl1 104.8(3) n O2 O1 C2 O3 34.0(3) n O2 O1 C2 C4 158.2(3) n O2 O1 C2 Cl2 -84.0(2) n C1 O3 C2 O1 -13.4(3) n C1 O3 C2 C4 -135.1(3) n C1 O3 C2 Cl2 105.6(2) n O2 C1 C3 Cl3 -63.7(3) n O3 C1 C3 Cl3 55.5(4) n Cl1 C1 C3 Cl3 176.2(2) y O1 C2 C4 Cl4 -65.2(4) n O3 C2 C4 Cl4 54.4(3) n Cl2 C2 C4 Cl4 174.9(2) y