#------------------------------------------------------------------------------ #$Date: 2015-01-23 12:30:19 +0000 (Fri, 23 Jan 2015) $ #$Revision: 130086 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/74/2007470.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_2007470 loop_ _publ_author_name 'Bromley, Mark K.' 'Looney, Mark G.' 'Solomon, David H.' 'Gable, Robert W.' 'Helliwell, Madeleine' 'Hodge, Philip' _publ_section_title ; 1,5,7,11-Tetraoxaspiro[5.5]undecane, 3,9-Dimethylidene-1,5,7,11-tetraoxaspiro[5.5]undecane and 1,5-Dioxa-7,11-dithiaspiro[5.5]undecane ; _journal_issue 7 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1019 _journal_page_last 1023 _journal_paper_doi 10.1107/S0108270198000274 _journal_volume 54 _journal_year 1998 _chemical_formula_sum 'C7 H12 O4' _chemical_formula_weight 160.17 _chemical_name_systematic ; ? ; _space_group_IT_number 60 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2n 2ab' _symmetry_space_group_name_H-M 'P b c n' _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 7.7068(11) _cell_length_b 10.1645(12) _cell_length_c 9.691(2) _cell_measurement_reflns_used 16 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 15.8 _cell_measurement_theta_min 12.0 _cell_volume 759.2(2) _computing_cell_refinement 'MSC/AFC Diffractometer Control Software' _computing_data_collection ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1994) ; _computing_data_reduction 'TEXSAN (Molecular Structure Corporation, 1995)' _computing_molecular_graphics TEXSAN _computing_publication_material TEXSAN _computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measurement_device 'Rigaku AFC-5R' _diffrn_measurement_method \w-2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_av_sigmaI/netI 0.019 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 672 _diffrn_reflns_theta_max 25.04 _diffrn_reflns_theta_min 3.32 _diffrn_standards_decay_% 0.71 _diffrn_standards_interval_count 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.116 _exptl_absorpt_correction_T_max 0.988 _exptl_absorpt_correction_T_min 0.969 _exptl_absorpt_correction_type '\y scans (North et al., 1968)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.437 _exptl_crystal_density_meas ? _exptl_crystal_description tabular _exptl_crystal_F_000 360 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.156 _refine_diff_density_min -0.131 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.147 _refine_ls_goodness_of_fit_obs 1.193 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 75 _refine_ls_number_reflns 671 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.155 _refine_ls_restrained_S_obs 1.193 _refine_ls_R_factor_all 0.048 _refine_ls_R_factor_obs .035 _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^)+(0.0406P)^2^+0.0735P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_all 0.088 _refine_ls_wR_factor_obs .079 _reflns_number_observed 533 _reflns_number_total 672 _reflns_observed_criterion I>2\s(I) _[local]_cod_data_source_file os1000.cif _[local]_cod_data_source_block s476 _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas ; _cod_database_code 2007470 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, 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 O1 .0531(7) .0402(6) .0502(6) .0068(5) .0038(5) -.0079(5) O2 .0404(6) .0458(6) .0375(6) -.0089(5) -.0038(5) .0019(5) C1 .0391(11) .0325(10) .0370(10) .000 -.0022(9) .000 C2 .0538(11) .0690(12) .0426(9) .0110(9) .0058(8) -.0073(9) C3 .0461(10) .0867(14) .0512(10) -.0047(11) .0072(9) .0077(10) C4 .0489(10) .0558(10) .0524(11) -.0161(9) .0001(9) .0085(8) 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_disorder_group _atom_site_type_symbol O1 .06720(14) .24644(10) .15113(11) .0478(4) Uani d . 1 . O O2 .12579(13) .40598(9) .31408(9) .0412(3) Uani d . 1 . O C1 0 .3285(2) .2500 .0362(5) Uani d S 1 . C C2 .1639(2) .3154(2) .0461(2) .0551(5) Uani d . 1 . C C3 .3015(2) .3983(2) .1104(2) .0613(5) Uani d . 1 . C C4 .2230(2) .4846(2) .2183(2) .0523(5) Uani d . 1 . C H2A .082(2) .3715(17) -.0063(16) .053(5) Uiso d . 1 . H H2B .208(3) .245(2) -.011(2) .070(6) Uiso d . 1 . H H3A .388(3) .3428(18) .1551(19) .070(6) Uiso d . 1 . H H3B .356(3) .4555(19) .041(2) .084(7) Uiso d . 1 . H H4A .145(2) .5515(17) .1790(18) .062(5) Uiso d . 1 . H H4B .308(2) .5324(17) .2744(18) .060(5) Uiso d . 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' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 -3 -2 -2 -2 -2 -3 -2 -1 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_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 O1 C2 . . 113.10(11) y C1 O2 C4 . . 112.91(10) y O1 C1 O1 4 . 105.10(15) y O1 C1 O2 4 4 113.07(6) ? O1 C1 O2 . 4 107.14(6) y O1 C1 O2 4 . 107.14(6) ? O1 C1 O2 . . 113.07(6) y O2 C1 O2 4 . 111.26(15) y O1 C2 C3 . . 110.32(14) y O1 C2 H2A . . 108.3(9) ? C3 C2 H2A . . 109.9(10) ? O1 C2 H2B . . 103.1(11) ? C3 C2 H2B . . 114.0(12) ? H2A C2 H2B . . 110.8(14) ? C2 C3 C4 . . 109.67(15) ? C2 C3 H3A . . 110.1(11) y C4 C3 H3A . . 107.8(11) ? C2 C3 H3B . . 110.7(12) ? C4 C3 H3B . . 107.7(12) ? H3A C3 H3B . . 110.7(16) ? O2 C4 C3 . . 109.68(15) y O2 C4 H4A . . 108.6(10) ? C3 C4 H4A . . 112.4(10) ? O2 C4 H4B . . 105.5(10) ? C3 C4 H4B . . 114.0(10) ? H4A C4 H4B . . 106.3(13) ? 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 O1 C1 . 1.3720(15) y O1 C2 . 1.443(2) y O2 C1 . 1.3948(14) y O2 C4 . 1.436(2) y C1 O1 4 1.3719(15) ? C1 O2 4 1.3948(14) ? C2 C3 . 1.491(3) y C2 H2A . .99(2) ? C2 H2B . .97(2) ? C3 C4 . 1.493(3) y C3 H3A . .97(2) ? C3 H3B . .98(2) ? C4 H4A . .98(2) ? C4 H4B . .98(2) ? 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_4 _geom_torsion C2 O1 C1 O1 4 -172.56(13) C2 O1 C1 O2 4 66.92(14) C2 O1 C1 O2 . -56.02(15) C4 O2 C1 O1 4 172.25(12) C4 O2 C1 O1 . 56.9(2) C4 O2 C1 O2 4 -63.69(10) C1 O1 C2 C3 . 54.3(2) O1 C2 C3 C4 . -52.7(2) C1 O2 C4 C3 . -55.4(2) C2 C3 C4 O2 . 53.4(2)