#------------------------------------------------------------------------------ #$Date: 2010-05-13 20:58:46 +0300 (Thu, 13 May 2010) $ #$Revision: 1167 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/7200842.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_7200842 loop_ _publ_author_name 'Olejniczak, Anna' 'Katrusiak, Andrzej' 'Vij, Ashwani' _publ_section_title ; Halogen⋯oxygen aggregation and disorder modes in pressure frozen XCF2CF2X : 1,4-dioxane (X = Br,I) complexes ; _journal_issue 7 _journal_name_full CrystEngComm _journal_page_first 1240 _journal_volume 11 _journal_year 2009 _chemical_formula_moiety 'C4 H8 O2' _chemical_formula_sum 'C4 H8 O2' _chemical_formula_weight 88.10 _chemical_melting_point 285 _chemical_name_common 1,4-dioxane _chemical_name_systematic ; 1,4-dioxane ; _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 98.36(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 5.6590(10) _cell_length_b 6.4100(10) _cell_length_c 5.8920(10) _cell_measurement_pressure 420000 _cell_measurement_reflns_used 180 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 29.59 _cell_measurement_theta_min 4.83 _cell_volume 211.46(6) _computing_cell_refinement 'CrysAlis (Oxford Diffraction, 2002)' _computing_data_collection 'CrysAlis (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlis (Oxford Diffraction, 2002)' _computing_molecular_graphics ;X-Seed (Barbour, 2001) and POV-Ray (Persistence of Vision, 2004) ; _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 296(2) _diffrn_detector_area_resol_mean 16.4 _diffrn_measured_fraction_theta_full 0.304 _diffrn_measured_fraction_theta_max 0.304 _diffrn_measurement_device_type 'Kuma KM4CCD \k geometry' _diffrn_measurement_method ;HP omega scans - for more details see: A. Budzianowski, A. Katrusiak in High-Pressure Crystallography (Eds.: A. Katrusiak, P. F. McMillan), Dordrecht: Kluwer Acad. Publ., 2004 pp.157-168 ; _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 0.1265 _diffrn_reflns_av_sigmaI/netI 0.1116 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_limit_l_min -4 _diffrn_reflns_number 1696 _diffrn_reflns_theta_full 29.59 _diffrn_reflns_theta_max 29.59 _diffrn_reflns_theta_min 4.83 _exptl_absorpt_coefficient_mu 0.110 _exptl_absorpt_correction_T_max 0.91 _exptl_absorpt_correction_T_min 0.50 _exptl_absorpt_correction_type integration _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 1.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 96 _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.07 _refine_diff_density_max 0.180 _refine_diff_density_min -0.264 _refine_diff_density_rms 0.060 _refine_ls_extinction_coef 1.7(6) _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 1.416 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 29 _refine_ls_number_reflns 180 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.416 _refine_ls_R_factor_all 0.2073 _refine_ls_R_factor_gt 0.1784 _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^)+(0.0757P)^2^+1.1475P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3250 _refine_ls_wR_factor_ref 0.3400 _reflns_number_gt 149 _reflns_number_total 180 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file b822832a.txt _[local]_cod_data_source_block C4H8O2 _[local]_cod_cif_authors_sg_H-M 'P 2(1)/n' _cod_database_code 7200842 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_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 _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.7141(19) 0.6145(11) 0.521(3) 0.091(15) Uani 1 1 d . . . C1 C 0.504(3) 0.7049(18) 0.572(5) 0.06(3) Uani 1 1 d . . . H1 H 0.4232 0.7746 0.4361 0.072 Uiso 1 1 calc R . . H2 H 0.5429 0.8089 0.6908 0.072 Uiso 1 1 calc R . . C2 C 0.663(4) 0.4587(18) 0.348(5) 0.06(2) Uani 1 1 d . . . H3 H 0.8097 0.3928 0.3193 0.069 Uiso 1 1 calc R . . H4 H 0.5873 0.5222 0.2065 0.069 Uiso 1 1 calc R . . 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 0.066(12) 0.030(5) 0.15(3) -0.015(7) -0.072(17) 0.001(5) C1 0.066(17) 0.025(5) 0.08(6) 0.009(10) -0.02(3) -0.016(7) C2 0.075(19) 0.042(7) 0.05(5) -0.023(11) -0.01(3) 0.008(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' 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 C1 O1 C2 110.6(12) . . ? O1 C1 C2 111.4(11) . 3_666 ? O1 C1 H1 109.3 . . ? C2 C1 H1 109.3 3_666 . ? O1 C1 H2 109.3 . . ? C2 C1 H2 109.3 3_666 . ? H1 C1 H2 108.0 . . ? O1 C2 C1 109(3) . 3_666 ? O1 C2 H3 109.8 . . ? C1 C2 H3 109.8 3_666 . ? O1 C2 H4 109.8 . . ? C1 C2 H4 109.8 3_666 . ? H3 C2 H4 108.3 . . ? 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 C1 1.39(3) . ? O1 C2 1.43(2) . ? C1 C2 1.53(4) 3_666 ? C1 H1 0.9700 . ? C1 H2 0.9700 . ? C2 C1 1.53(4) 3_666 ? C2 H3 0.9700 . ? C2 H4 0.9700 . ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 O1 C1 C2 58(3) . . . 3_666 ? C1 O1 C2 C1 -57.0(16) . . . 3_666 ?