#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2007135.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_2007135 loop_ _publ_author_name 'L\/oiten, M. S.' 'Dalhus, B.' 'Fjærtoft, B.' 'Klaveness, J.' _publ_section_title ; trans-2,3-Diiodo-2-butene-1,4-diol ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 555 _journal_page_last 557 _journal_volume 54 _journal_year 1998 _chemical_formula_sum 'C4 H6 I2 O2' _chemical_formula_weight 339.89 _chemical_name_systematic ; 2,3-diiodo-2-buten-1,4-diol ; _space_group_IT_number 88 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall '-I 4ad' _symmetry_space_group_name_H-M 'I 41/a :2' _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 13.7270(10) _cell_length_b 13.7270(10) _cell_length_c 8.1300(10) _cell_measurement_reflns_used 8192 _cell_measurement_temperature 150(2) _cell_volume 1531.9(2) _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_collection 'SMART (Siemens, 1995)' _computing_data_reduction SAINT _computing_publication_material 'XPREP (Siemens, 1996)' _computing_structure_refinement SHELXTL _computing_structure_solution 'SHELXTL (Sheldrick, 1994)' _diffrn_ambient_temperature 150(2) _diffrn_measurement_device 'Siemens SMART CCD Area Detector' _diffrn_measurement_method '\w scan' _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 0.0228 _diffrn_reflns_av_sigmaI/netI 0.0178 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 17735 _diffrn_reflns_theta_max 44.93 _diffrn_reflns_theta_min 2.91 _exptl_absorpt_coefficient_mu 8.133 _exptl_absorpt_correction_T_max 0.428 _exptl_absorpt_correction_T_min 0.140 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; XPREP (Siemens, 1996), followed by an empirical correction of intensities due to absorption by the glass fibre and glue (SADABS; Sheldrick, 1996) ; _exptl_crystal_colour Colourless _exptl_crystal_density_diffrn 2.947 _exptl_crystal_density_meas 'not measured' _exptl_crystal_description Block _exptl_crystal_F_000 1216 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _refine_diff_density_max 1.103 _refine_diff_density_min -0.711 _refine_ls_extinction_coef 0.0049(2) _refine_ls_extinction_method SHELXTL_(Sheldrick,_1994) _refine_ls_goodness_of_fit_all 2.239 _refine_ls_goodness_of_fit_obs 2.299 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 39 _refine_ls_number_reflns 2891 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 2.239 _refine_ls_restrained_S_obs 2.299 _refine_ls_R_factor_all 0.0315 _refine_ls_R_factor_obs 0.0271 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w = 1/[\s^2^(Fo^2^)+(0.0086P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_all 0.0531 _refine_ls_wR_factor_obs 0.0522 _reflns_number_observed 2646 _reflns_number_total 2891 _reflns_observed_criterion >2sigma(I) _[local]_cod_data_source_file ab1505.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'I 41/a (second setting)' _cod_original_cell_volume 1531.90(10) _cod_database_code 2007135 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' 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 I1 0.02517(4) 0.01951(4) 0.01827(4) -0.00496(3) 0.00747(3) -0.00002(3) O1 0.0217(4) 0.0151(3) 0.0154(3) 0.0016(3) -0.0033(3) -0.0036(3) C1 0.0134(3) 0.0122(3) 0.0153(4) -0.0010(3) 0.0014(3) -0.0008(3) C2 0.0150(4) 0.0174(4) 0.0187(5) -0.0012(3) -0.0004(3) -0.0047(3) 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 I1 0.654070(8) 0.687482(7) -0.006829(11) 0.02098(3) Uani d . 1 I O1 0.75744(8) 0.90831(7) -0.00683(12) 0.01740(14) Uani d . 1 O H1 0.7224(18) 0.9352(16) -0.0783(8) 0.026 Uiso calc R 1 H C1 0.75028(8) 0.76063(8) -0.16952(15) 0.01362(15) Uani d . 1 C C2 0.81343(9) 0.83352(10) -0.0813(2) 0.0171(2) Uani d . 1 C H3 0.85193(9) 0.79960(10) 0.0042(2) 0.020 Uiso calc R 1 H H2 0.85959(9) 0.86294(10) -0.1606(2) 0.020 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' I I -0.4742 1.8119 '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_site_symmetry_1 _geom_angle _geom_angle_publ_flag C2 O1 H1 . 109.50(10) ? C1 C1 C2 13_664 127.80(10) yes C1 C1 I1 13_664 120.10(10) yes C2 C1 I1 . 112.10(10) yes O1 C2 C1 . 111.90(10) yes O1 C2 H3 . 109.20(10) ? C1 C2 H3 . 109.20(10) ? O1 C2 H2 . 109.20(10) ? C1 C2 H2 . 109.20(10) ? H3 C2 H2 . 107.9 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag I1 C1 . 2.1220(10) yes O1 C2 . 1.418(2) yes O1 H1 . 0.84 ? C1 C1 13_664 1.341(2) yes C1 C2 . 1.505(2) yes C2 H3 . 0.99 ? C2 H2 . 0.99 ? 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_site_symmetry_1 _geom_torsion _geom_torsion_publ_flag C1 C1 C2 O1 13_664 117.9(2) yes I1 C1 C2 O1 . -62.20(10) yes