#------------------------------------------------------------------------------ #$Date: 2014-07-12 07:06:18 +0300 (Sat, 12 Jul 2014) $ #$Revision: 120112 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/20/74/7207491.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7207491 loop_ _publ_author_name 'Yufit, D. S.' 'Howard, J. A. K.' _publ_section_title ; Low melting molecular complexes. The structures of molecular complexes of tri- and di-chloromethanes with small ketones and 1,4-dioxane ; _journal_issue 6 _journal_name_full CrystEngComm _journal_page_first 2003 _journal_volume 14 _journal_year 2012 _chemical_formula_moiety 'C4 H8 O2, 2 C H2 Cl2' _chemical_formula_sum 'C6 H12 Cl4 O2' _chemical_formula_weight 257.96 _chemical_melting_point 205.5(5) _chemical_name_common 'dichloromethane dioxane co-crystal' _chemical_name_systematic ; dichloromethane 1,4-dioxane clathrate (2:1) ; _space_group_IT_number 61 _symmetry_cell_setting orthorhombic _symmetry_Int_Tables_number 61 _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_space_group_name_H-M 'P b c a' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method ; manual editing of the CIF file created by SHELXTL Ver. 6.14 and processed with modiCIfer-09152005. ; _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 7.8287(13) _cell_length_b 10.025(2) _cell_length_c 14.764(3) _cell_measurement_reflns_used 1108 _cell_measurement_temperature 195.0(2) _cell_measurement_theta_max 25.84 _cell_measurement_theta_min 2.76 _cell_volume 1158.7(4) _computing_cell_refinement 'SAINT Ver. 6.45 (Bruker-AXS, 2003)' _computing_data_collection 'SMART Ver. 5.630 (Bruker-AXS, 2003)' _computing_data_reduction 'SAINT Ver. 6.45' _computing_molecular_graphics 'SHELXTL Ver. 6.14' _computing_publication_material 'SHELXTL Ver. 6.14' _computing_structure_refinement 'SHELXTL Ver. 6.14' _computing_structure_solution 'SHELXTL Ver. 6.14 (Bruker-AXS, 2003)' _diffrn_ambient_temperature 195.0(2) _diffrn_measured_fraction_theta_full 0.948 _diffrn_measured_fraction_theta_max 0.948 _diffrn_measurement_device_type 'Bruker SMART CCD 6000' _diffrn_measurement_method '0.30\% \w scans' _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 0.0316 _diffrn_reflns_av_sigmaI/netI 0.0212 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 8652 _diffrn_reflns_theta_full 29.00 _diffrn_reflns_theta_max 29.00 _diffrn_reflns_theta_min 2.76 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.985 _exptl_absorpt_correction_T_max 0.7565 _exptl_absorpt_correction_T_min 0.6940 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS (Bruker-AXS, 2003) ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.479 _exptl_crystal_density_method 'not measured' _exptl_crystal_description cylinder _exptl_crystal_F_000 528 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _refine_diff_density_max 0.247 _refine_diff_density_min -0.349 _refine_diff_density_rms 0.044 _refine_ls_extinction_coef 0.0076(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 80 _refine_ls_number_reflns 1462 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.032 _refine_ls_R_factor_all 0.0512 _refine_ls_R_factor_gt 0.0326 _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^)+(0.0300P)^2^+0.5000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0753 _refine_ls_wR_factor_ref 0.0848 _reflns_number_gt 1074 _reflns_number_total 1462 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file c2ce06526f.txt _[local]_cod_data_source_block 9_dd1 _[local]_cod_cif_authors_sg_H-M 'P b c a ' _[local]_cod_cif_authors_sg_Hall '-P 2ac 2ab ' _cod_depositor_comments ; The following automatic conversions were performed: '_chemical_melting_point' value '205-206' was changed to '205.5(5)' - the average value was taken and precision was estimated. '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' 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 1158.8(4) _cod_database_code 7207491 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' '-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_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag O1 O 0.04928(17) 0.48374(13) 0.09089(8) 0.0495(3) Uani 1 1 d C1 C 0.0434(3) 0.37376(19) 0.02970(14) 0.0518(5) Uani 1 1 d C2 C 0.0868(3) 0.60305(19) 0.04245(13) 0.0481(4) Uani 1 1 d H11 H 0.010(3) 0.296(2) 0.0651(14) 0.063(6) Uiso 1 1 d H12 H 0.153(3) 0.361(2) 0.0012(14) 0.062(6) Uiso 1 1 d H21 H 0.197(3) 0.596(2) 0.0165(13) 0.050(5) Uiso 1 1 d H22 H 0.088(3) 0.675(2) 0.0884(14) 0.066(6) Uiso 1 1 d Cl1 Cl 0.01586(7) 0.47681(5) 0.37443(4) 0.06028(19) Uani 1 1 d Cl2 Cl 0.18800(10) 0.26370(6) 0.27788(5) 0.0844(3) Uani 1 1 d C1S C 0.1773(3) 0.43601(19) 0.29593(13) 0.0462(4) Uani 1 1 d H1S H 0.149(3) 0.475(2) 0.2404(15) 0.053(5) Uiso 1 1 d H2S H 0.281(3) 0.465(2) 0.3240(14) 0.062(6) Uiso 1 1 d loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0590(8) 0.0540(7) 0.0354(6) 0.0037(5) -0.0022(6) 0.0023(6) C1 0.0631(13) 0.0411(9) 0.0512(10) 0.0060(8) 0.0052(9) 0.0083(9) C2 0.0501(12) 0.0468(9) 0.0474(10) -0.0057(8) 0.0064(9) -0.0058(8) Cl1 0.0573(4) 0.0632(3) 0.0604(3) -0.0054(2) 0.0075(2) 0.0054(2) Cl2 0.0963(5) 0.0491(3) 0.1078(5) 0.0019(3) 0.0394(4) 0.0094(3) C1S 0.0488(12) 0.0492(10) 0.0407(9) 0.0042(7) -0.0006(8) -0.0024(8) 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' O O 0.0106 0.0060 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 O1 C1 109.75(14) . . yes O1 C1 C2 110.73(15) . 5_565 yes O1 C1 H11 106.6(12) . . ? C2 C1 H11 109.1(13) 5_565 . ? O1 C1 H12 110.4(13) . . ? C2 C1 H12 108.5(13) 5_565 . ? H11 C1 H12 111.5(18) . . ? O1 C2 C1 110.40(16) . 5_565 yes O1 C2 H21 109.1(12) . . ? C1 C2 H21 110.2(12) 5_565 . ? O1 C2 H22 105.5(12) . . ? C1 C2 H22 112.5(13) 5_565 . ? H21 C2 H22 108.9(18) . . ? Cl2 C1S Cl1 111.32(11) . . yes Cl2 C1S H1S 107.0(12) . . ? Cl1 C1S H1S 108.1(13) . . ? Cl2 C1S H2S 109.0(13) . . ? Cl1 C1S H2S 104.7(13) . . ? H1S C1S H2S 116.7(19) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C2 1.424(2) . yes O1 C1 1.426(2) . yes C1 C2 1.492(3) 5_565 yes C1 H11 0.97(2) . ? C1 H12 0.97(2) . ? C2 C1 1.492(3) 5_565 yes C2 H21 0.95(2) . ? C2 H22 0.99(2) . ? Cl1 C1S 1.763(2) . yes Cl2 C1S 1.750(2) . yes C1S H1S 0.93(2) . ? C1S H2S 0.96(2) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C1S H1S O1 0.93(2) 2.34(2) 3.225(2) 156.8(17) . C1S H2S O1 0.96(2) 2.45(2) 3.391(3) 166.1(18) 6_656 _journal_paper_doi 10.1039/c2ce06526f