# Electronic Supplementary Material for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_author_address ;Faculty of Crystal Chemistry, Adam Mickiewicz University, Grunwaldzka 6, 60-780 Poznan Poland ; loop_ _publ_author_footnote ; Faculty of Crystal Chemistry, Adam Mickiewicz University, Grunwaldzka 6, 60-780 Poznan Poland ; _publ_contact_author_address ;Faculty of Crystal Chemistry, Adam Mickiewicz University, Grunwaldzka 6, 60-780 Poznan Poland ; _publ_contact_author_email katran@amu.edu.pl _publ_contact_author_fax +48(61)8658008 _publ_contact_author_phone +48(61)8291443 _publ_contact_author_name 'Andrzej Katrusiak' _publ_section_title ; Halogen...oxygen interactions and disorder modes in pressure frozen complexes of 1,2-dihaloperfuoroethanes with with 1,4-dioxane ; loop_ _publ_author_name A.Katrusiak A.Olejniczak A.Vij data_BrCF2CF2I_C4H8O2 _database_code_depnum_ccdc_archive 'CCDC 656092' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1-bromo-2-iodo-1,1,2,2-tetrafluoroethane:1,4-dioxane ; _chemical_name_common 1-bromo-2-iodo-1,1,2,2-tetrafluoroethane:1,4-dioxane _chemical_formula_moiety 'C6 H8 Br F4 I O2' _chemical_formula_sum 'C6 H8 Br F4 I O2' _chemical_formula_weight 394.93 _chemical_melting_point ? _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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' _cell_length_a 9.5983(19) _cell_length_b 5.9716(12) _cell_length_c 9.784(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.41(3) _cell_angle_gamma 90.00 _cell_volume 535.13(19) _cell_formula_units_Z 2 _cell_measurement_reflns_used 3961 _cell_measurement_theta_min 4.05 _cell_measurement_theta_max 29.31 _cell_measurement_temperature 296(2) _cell_measurement_pressure 620000 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.47 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.451 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 368 _exptl_absorpt_coefficient_mu 6.755 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details ; Katrusiak, A. (2003). REDSHABS - 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_absorpt_correction_T_min 0.15 _exptl_absorpt_correction_T_max 0.30 _exptl_special_details ; high-pressure measurement of 1-bromo-2-iodotetrafluoroethane with 1,4-dioxane at 0.62(5) GPa ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _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_detector_area_resol_mean 16.4 _diffrn_reflns_number 3961 _diffrn_reflns_av_R_equivalents 0.0663 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_theta_min 4.05 _diffrn_reflns_theta_max 29.31 _diffrn_reflns_theta_full 29.31 _diffrn_measured_fraction_theta_max 0.310 _diffrn_measured_fraction_theta_full 0.310 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _reflns_number_total 455 _reflns_number_gt 400 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0814 _refine_ls_R_factor_gt 0.0700 _refine_ls_wR_factor_ref 0.1651 _refine_ls_wR_factor_gt 0.1584 _refine_ls_goodness_of_fit_ref 1.196 _refine_ls_restrained_S_all 1.196 _refine_ls_number_reflns 455 _refine_ls_number_parameters 64 _refine_ls_number_restraints 0 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0643P)^2^+4.1936P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.504 _refine_diff_density_min -0.357 _refine_diff_density_rms 0.101 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection 'CrysAlis (Oxford Diffraction, 2002)' _computing_cell_refinement 'CrysAlis (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlis (Oxford Diffraction, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;X-Seed (Barbour, 2001) and POV-Ray (Persistence of Vision, 2004) ; _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' 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 I1 I 0.1960(4) 0.23522(18) 0.5930(2) 0.063(3) Uani 0.50 1 d P . . Br1 Br 0.1960(4) 0.23522(18) 0.5930(2) 0.063(3) Uani 0.50 1 d P . . C2 C 0.010(7) 0.432(4) 0.560(4) 0.17(5) Uani 1 1 d . . . O1 O 0.527(3) 0.4994(13) 0.8635(11) 0.049(15) Uani 1 1 d . . . C12 C 0.532(4) 0.2969(18) 0.9437(17) 0.09(2) Uani 1 1 d . . . H12A H 0.6008 0.1934 0.9233 0.102 Uiso 1 1 calc R . . H12B H 0.4363 0.2265 0.9158 0.102 Uiso 1 1 calc R . . C11 C 0.577(4) 0.349(2) 1.1006(17) 0.05(2) Uani 1 1 d . . . H11A H 0.5830 0.2111 1.1544 0.056 Uiso 1 1 calc R . . H11B H 0.6728 0.4175 1.1281 0.056 Uiso 1 1 calc R . . F3 F -0.099(5) 0.325(3) 0.577(3) 0.16(3) Uani 1 1 d . . . F2 F 0.060(5) 0.595(4) 0.672(2) 0.25(3) Uani 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 I1 0.070(9) 0.0524(8) 0.0631(14) 0.0003(6) 0.017(3) 0.0106(10) Br1 0.070(9) 0.0524(8) 0.0631(14) 0.0003(6) 0.017(3) 0.0106(10) C2 0.34(15) 0.077(13) 0.14(3) 0.027(14) 0.15(6) 0.01(3) O1 0.08(5) 0.043(4) 0.027(7) 0.001(3) 0.027(17) -0.001(7) C12 0.19(8) 0.032(6) 0.036(10) -0.002(5) 0.04(3) -0.003(12) C11 0.05(8) 0.037(6) 0.037(10) 0.006(6) 0.00(3) 0.027(11) F3 0.14(9) 0.137(12) 0.21(3) 0.098(15) 0.07(4) 0.01(2) F2 0.33(11) 0.27(2) 0.109(16) -0.113(15) 0.00(4) 0.12(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 I1 C2 2.08(5) . ? Br1 C2 2.08(5) . ? C2 F3 1.27(6) . ? C2 C2 1.40(5) 3_566 ? C2 F2 1.44(4) . ? O1 C12 1.435(13) . ? O1 C11 1.46(3) 3_667 ? C12 C11 1.50(2) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C11 O1 1.46(3) 3_667 ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? 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 F3 C2 C2 120(7) . 3_566 ? F3 C2 F2 110(3) . . ? C2 C2 F2 100(3) 3_566 . ? F3 C2 Br1 113(2) . . ? C2 C2 Br1 110(5) 3_566 . ? F2 C2 Br1 101(4) . . ? F3 C2 I1 113(2) . . ? C2 C2 I1 110(5) 3_566 . ? F2 C2 I1 101(4) . . ? Br1 C2 I1 0.00(12) . . ? C12 O1 C11 107.7(14) . 3_667 ? O1 C12 C11 109.7(11) . . ? O1 C12 H12A 109.7 . . ? C11 C12 H12A 109.7 . . ? O1 C12 H12B 109.7 . . ? C11 C12 H12B 109.7 . . ? H12A C12 H12B 108.2 . . ? O1 C11 C12 111(2) 3_667 . ? O1 C11 H11A 109.3 3_667 . ? C12 C11 H11A 109.3 . . ? O1 C11 H11B 109.3 3_667 . ? C12 C11 H11B 109.3 . . ? H11A C11 H11B 108.0 . . ? #END # Attachment 'C4H8O2.txt' data_C4H8O2 _database_code_depnum_ccdc_archive 'CCDC 656093' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,4-dioxane ; _chemical_name_common 1,4-dioxane _chemical_formula_moiety 'C4 H8 O2' _chemical_formula_sum 'C4 H8 O2' _chemical_formula_weight 88.10 _chemical_melting_point 285 _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 2(1)/n' _symmetry_space_group_name_Hall '-P 2yn' 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' _cell_length_a 5.6590(10) _cell_length_b 6.4100(10) _cell_length_c 5.8920(10) _cell_angle_alpha 90.00 _cell_angle_beta 98.36(3) _cell_angle_gamma 90.00 _cell_volume 211.46(6) _cell_formula_units_Z 2 _cell_measurement_reflns_used 180 _cell_measurement_theta_min 4.83 _cell_measurement_theta_max 29.59 _cell_measurement_temperature 296(2) _cell_measurement_pressure 420000 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.07 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 96 _exptl_absorpt_coefficient_mu 0.110 _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_absorpt_correction_T_min 0.50 _exptl_absorpt_correction_T_max 0.91 _exptl_special_details ; high-pressure measurement of 1,4-dioxane at 0.42(5) GPa ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _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_detector_area_resol_mean 16.4 _diffrn_reflns_number 1696 _diffrn_reflns_av_R_equivalents 0.1265 _diffrn_reflns_av_sigmaI/netI 0.1116 _diffrn_reflns_theta_min 4.83 _diffrn_reflns_theta_max 29.59 _diffrn_reflns_theta_full 29.59 _diffrn_measured_fraction_theta_max 0.304 _diffrn_measured_fraction_theta_full 0.304 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -4 _diffrn_reflns_limit_l_max 4 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _reflns_number_total 180 _reflns_number_gt 149 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.2073 _refine_ls_R_factor_gt 0.1784 _refine_ls_wR_factor_ref 0.3400 _refine_ls_wR_factor_gt 0.3250 _refine_ls_goodness_of_fit_ref 1.416 _refine_ls_restrained_S_all 1.416 _refine_ls_number_reflns 180 _refine_ls_number_parameters 29 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0757P)^2^+1.1475P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.180 _refine_diff_density_min -0.264 _refine_diff_density_rms 0.060 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 1.7(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection 'CrysAlis (Oxford Diffraction, 2002)' _computing_cell_refinement 'CrysAlis (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlis (Oxford Diffraction, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;X-Seed (Barbour, 2001) and POV-Ray (Persistence of Vision, 2004) ; _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' 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) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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_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_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 ? #END # Attachment 'ICF2CF2I_C4H8O2.txt' data_ICF2CF2I_C4H8O2 _database_code_depnum_ccdc_archive 'CCDC 656094' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,2-diiodo-1,1,2,2-tetrafluoroethane:1,4-dioxane ; _chemical_name_common 1,2-diiodo-1,1,2,2-tetrafluoroethane:1,4-dioxane _chemical_formula_moiety 'C6 H8 F4 I2 O2' _chemical_formula_sum 'C6 H8 F4 I2 O2' _chemical_formula_weight 441.92 _chemical_melting_point ? _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'R -3' _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 8.8380(10) _cell_length_b 8.8380(10) _cell_length_c 13.532(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 915.4(3) _cell_formula_units_Z 3 _cell_measurement_reflns_used 237 _cell_measurement_theta_min 3.06 _cell_measurement_theta_max 29.53 _cell_measurement_temperature 296(2) _cell_measurement_pressure 300000 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 606 _exptl_absorpt_coefficient_mu 5.180 _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_absorpt_correction_T_min 0.43 _exptl_absorpt_correction_T_max 0.62 _exptl_special_details ; high-pressure measurement of 1,2-diiodotetrafluoroethane with 1,4-dioxane at 0.30(5) GPa ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _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_detector_area_resol_mean 16.4 _diffrn_reflns_number 1688 _diffrn_reflns_av_R_equivalents 0.1380 _diffrn_reflns_av_sigmaI/netI 0.0556 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 29.53 _diffrn_reflns_theta_full 29.53 _diffrn_measured_fraction_theta_max 0.407 _diffrn_measured_fraction_theta_full 0.407 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _reflns_number_total 237 _reflns_number_gt 197 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.1451 _refine_ls_R_factor_gt 0.1335 _refine_ls_wR_factor_ref 0.3668 _refine_ls_wR_factor_gt 0.3502 _refine_ls_goodness_of_fit_ref 1.440 _refine_ls_restrained_S_all 1.440 _refine_ls_number_reflns 237 _refine_ls_number_parameters 39 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.380 _refine_diff_density_min -1.017 _refine_diff_density_rms 0.135 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.18(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection 'CrysAlis (Oxford Diffraction, 2002)' _computing_cell_refinement 'CrysAlis (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlis (Oxford Diffraction, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;X-Seed (Barbour, 2001) and POV-Ray (Persistence of Vision, 2004) ; _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' 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 1.0000 1.0000 0.076(3) 0.146(19) Uani 1 3 d S . . C2 C 0.896(3) 1.066(3) 0.023(3) 0.127(19) Uani 0.67 1 d P . . H1 H 0.8116 1.0794 0.0632 0.153 Uiso 0.33 1 d P . . H2 H 0.9613 1.1654 -0.0203 0.153 Uiso 0.33 1 d P . . H3 H 0.8031 0.9818 -0.0196 0.153 Uiso 0.33 1 d P . . H4 H 0.8560 1.1309 0.0633 0.153 Uiso 0.33 1 d P . . F2 F 0.928(7) 0.783(4) 0.506(3) 0.101(14) Uani 0.33 1 d P . . I1 I 1.0000 1.0000 0.6891(6) 0.202(7) Uani 1 3 d S . . C1 C 0.9399(13) 0.9374(12) 0.5402(17) 0.018(3) Uiso 0.33 1 d P . . F1 F 0.818(5) 0.778(3) 0.504(2) 0.092(13) Uani 0.33 1 d P . . 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 0.126(7) 0.126(7) 0.18(6) 0.000 0.000 0.063(4) C2 0.144(19) 0.115(11) 0.10(6) 0.016(14) -0.046(16) 0.050(10) F2 0.124(16) 0.15(2) 0.01(5) -0.002(15) -0.002(14) 0.057(15) I1 0.217(6) 0.217(6) 0.173(19) 0.000 0.000 0.109(3) F1 0.111(17) 0.110(14) 0.01(4) -0.008(11) -0.009(11) 0.025(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 1.50(3) 2_765 ? O1 C2 1.50(3) 3_675 ? O1 C2 1.50(3) . ? O1 C2 1.88(7) 12_655 ? O1 C2 1.88(7) 11_565 ? O1 C2 1.88(7) 10_775 ? C2 C2 1.45(6) 12_655 ? C2 C2 1.45(6) 11_565 ? C2 O1 1.88(7) 10_775 ? C2 H1 0.9778 . ? C2 H2 0.9682 . ? C2 H3 0.9734 . ? C2 H4 0.9764 . ? F2 F1 0.88(2) 12_656 ? F2 F1 0.96(2) . ? F2 C1 1.35(4) 12_656 ? F2 C1 1.39(4) . ? F2 F2 1.70(3) 11_566 ? F2 F2 1.70(3) 12_656 ? F2 C1 1.75(3) 2_765 ? I1 C1 2.09(2) 3_675 ? I1 C1 2.09(2) . ? I1 C1 2.09(2) 2_765 ? C1 C1 0.940(18) 3_675 ? C1 C1 0.940(18) 2_765 ? C1 C1 1.22(4) 11_566 ? C1 C1 1.22(4) 12_656 ? C1 F2 1.35(4) 11_566 ? C1 F1 1.37(2) . ? C1 C1 1.54(3) 10_776 ? C1 F1 1.65(3) 11_566 ? C1 F2 1.75(3) 3_675 ? C1 F1 1.78(2) 12_656 ? F1 F2 0.88(2) 11_566 ? F1 C1 1.65(3) 12_656 ? F1 C1 1.78(2) 11_566 ? 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 C2 99(3) 2_765 3_675 ? C2 O1 C2 99(3) 2_765 . ? C2 O1 C2 99(3) 3_675 . ? C2 O1 C2 49.4(13) 2_765 12_655 ? C2 O1 C2 106(3) 3_675 12_655 ? C2 O1 C2 49.4(13) . 12_655 ? C2 O1 C2 106(3) 2_765 11_565 ? C2 O1 C2 49.4(13) 3_675 11_565 ? C2 O1 C2 49.4(13) . 11_565 ? C2 O1 C2 74.6(19) 12_655 11_565 ? C2 O1 C2 49.4(13) 2_765 10_775 ? C2 O1 C2 49.4(13) 3_675 10_775 ? C2 O1 C2 106(3) . 10_775 ? C2 O1 C2 74.6(19) 12_655 10_775 ? C2 O1 C2 74.6(19) 11_565 10_775 ? C2 C2 C2 103(3) 12_655 11_565 ? C2 C2 O1 79.0(13) 12_655 . ? C2 C2 O1 79.0(13) 11_565 . ? C2 C2 O1 51.6(18) 12_655 10_775 ? C2 C2 O1 51.6(18) 11_565 10_775 ? O1 C2 O1 74(3) . 10_775 ? C2 C2 H1 115.2 12_655 . ? C2 C2 H1 140.6 11_565 . ? O1 C2 H1 115.4 . . ? O1 C2 H1 163.5 10_775 . ? C2 C2 H2 115.6 12_655 . ? C2 C2 H2 37.8 11_565 . ? O1 C2 H2 116.1 . . ? O1 C2 H2 71.9 10_775 . ? H1 C2 H2 111.9 . . ? C2 C2 H3 37.5 12_655 . ? C2 C2 H3 116.4 11_565 . ? O1 C2 H3 115.6 . . ? O1 C2 H3 72.3 10_775 . ? H1 C2 H3 91.2 . . ? H2 C2 H3 103.4 . . ? C2 C2 H4 140.3 12_655 . ? C2 C2 H4 115.5 11_565 . ? O1 C2 H4 115.4 . . ? O1 C2 H4 163.7 10_775 . ? H1 C2 H4 25.2 . . ? H2 C2 H4 91.9 . . ? H3 C2 H4 111.5 . . ? F1 F2 F1 161(4) 12_656 . ? F1 F2 C1 72(2) 12_656 12_656 ? F1 F2 C1 90(3) . 12_656 ? F1 F2 C1 101(3) 12_656 . ? F1 F2 C1 68(2) . . ? C1 F2 C1 53(2) 12_656 . ? F1 F2 F2 141(3) 12_656 11_566 ? F1 F2 F2 22(2) . 11_566 ? C1 F2 F2 69.0(12) 12_656 11_566 ? C1 F2 F2 50.8(10) . 11_566 ? F1 F2 F2 24(2) 12_656 12_656 ? F1 F2 F2 141(2) . 12_656 ? C1 F2 F2 52.7(14) 12_656 12_656 ? C1 F2 F2 78.0(10) . 12_656 ? F2 F2 F2 119.0(10) 11_566 12_656 ? F1 F2 C1 69(2) 12_656 2_765 ? F1 F2 C1 100(3) . 2_765 ? C1 F2 C1 44(2) 12_656 2_765 ? C1 F2 C1 32.3(11) . 2_765 ? F2 F2 C1 80.5(8) 11_566 2_765 ? F2 F2 C1 46.2(9) 12_656 2_765 ? C1 I1 C1 26.0(5) 3_675 . ? C1 I1 C1 26.0(5) 3_675 2_765 ? C1 I1 C1 26.0(5) . 2_765 ? C1 C1 C1 60.000(18) 3_675 2_765 ? C1 C1 C1 67.3(10) 3_675 11_566 ? C1 C1 C1 90.000(9) 2_765 11_566 ? C1 C1 C1 90.000(11) 3_675 12_656 ? C1 C1 C1 67.3(10) 2_765 12_656 ? C1 C1 C1 45.4(19) 11_566 12_656 ? C1 C1 F2 116(2) 3_675 11_566 ? C1 C1 F2 152.2(19) 2_765 11_566 ? C1 C1 F2 65(2) 11_566 11_566 ? C1 C1 F2 86(2) 12_656 11_566 ? C1 C1 F1 151.8(16) 3_675 . ? C1 C1 F1 135(2) 2_765 . ? C1 C1 F1 87.2(19) 11_566 . ? C1 C1 F1 79.4(19) 12_656 . ? F2 C1 F1 37.8(11) 11_566 . ? C1 C1 F2 150(2) 3_675 . ? C1 C1 F2 96(2) 2_765 . ? C1 C1 F2 97(3) 11_566 . ? C1 C1 F2 62(2) 12_656 . ? F2 C1 F2 76.4(9) 11_566 . ? F1 C1 F2 40.6(10) . . ? C1 C1 C1 52.3(11) 3_675 10_776 ? C1 C1 C1 52.3(11) 2_765 10_776 ? C1 C1 C1 37.7(11) 11_566 10_776 ? C1 C1 C1 37.7(11) 12_656 10_776 ? F2 C1 C1 102(3) 11_566 10_776 ? F1 C1 C1 113(2) . 10_776 ? F2 C1 C1 99(3) . 10_776 ? C1 C1 F1 82.0(17) 3_675 11_566 ? C1 C1 F1 136.8(15) 2_765 11_566 ? C1 C1 F1 54.3(10) 11_566 11_566 ? C1 C1 F1 95(2) 12_656 11_566 ? F2 C1 F1 35.4(10) 11_566 11_566 ? F1 C1 F1 73.2(7) . 11_566 ? F2 C1 F1 110.9(16) . 11_566 ? C1 C1 F1 89.1(16) 10_776 11_566 ? C1 C1 F2 52.2(17) 3_675 3_675 ? C1 C1 F2 109.8(17) 2_765 3_675 ? C1 C1 F2 50.5(14) 11_566 3_675 ? C1 C1 F2 96(2) 12_656 3_675 ? F2 C1 F2 64.8(7) 11_566 3_675 ? F1 C1 F2 102.6(14) . 3_675 ? F2 C1 F2 137(3) . 3_675 ? C1 C1 F2 72.8(14) 10_776 3_675 ? F1 C1 F2 29.9(9) 11_566 3_675 ? C1 C1 F1 122.8(17) 3_675 12_656 ? C1 C1 F1 66.6(16) 2_765 12_656 ? C1 C1 F1 94.6(19) 11_566 12_656 ? C1 C1 F1 49.9(10) 12_656 12_656 ? F2 C1 F1 101.5(16) 11_566 12_656 ? F1 C1 F1 68.9(7) . 12_656 ? F2 C1 F1 29.0(10) . 12_656 ? C1 C1 F1 79.7(16) 10_776 12_656 ? F1 C1 F1 132(2) 11_566 12_656 ? F2 C1 F1 145(2) 3_675 12_656 ? C1 C1 I1 77.0(3) 3_675 . ? C1 C1 I1 77.0(3) 2_765 . ? C1 C1 I1 143.7(11) 11_566 . ? C1 C1 I1 143.7(11) 12_656 . ? F2 C1 I1 130(2) 11_566 . ? F1 C1 I1 125.8(15) . . ? F2 C1 I1 117.5(19) . . ? C1 C1 I1 120.0(15) 10_776 . ? F1 C1 I1 116.0(14) 11_566 . ? F2 C1 I1 102.2(17) 3_675 . ? F1 C1 I1 110.2(12) 12_656 . ? F2 F1 F2 135(5) 11_566 . ? F2 F1 C1 70(2) 11_566 . ? F2 F1 C1 71(3) . . ? F2 F1 C1 81(3) 11_566 12_656 ? F2 F1 C1 55(2) . 12_656 ? C1 F1 C1 46.3(17) . 12_656 ? F2 F1 C1 50(3) 11_566 11_566 ? F2 F1 C1 86(2) . 11_566 ? C1 F1 C1 42.9(16) . 11_566 ? C1 F1 C1 31.4(8) 12_656 11_566 ? #END