#------------------------------------------------------------------------------ #$Date: 2016-02-19 14:29:56 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176759 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/85/2008504.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_2008504 loop_ _publ_author_name 'Umehara, Misao' 'Hosomi, Hiroyuki' 'Ohba, Shigeru' _publ_section_title ; cis-4,4-Dimethyltricyclo[6.3.0.0^1,7^]undecane-2,6-dione ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first IUC9900039 _journal_paper_doi 10.1107/S0108270199099412 _journal_volume 55 _journal_year 1999 _chemical_formula_moiety 'C13 H18 O2' _chemical_formula_sum 'C13 H18 O2' _chemical_formula_weight 206.29 _chemical_name_systematic ; 4,4-Dimethyltricyclo[6.3.0.0^1,7^]undecane-2,6-dione ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yab' _symmetry_space_group_name_H-M 'P 1 21/a 1' _atom_type_scat_source IntTabIV _cell_angle_alpha 90.00000 _cell_angle_beta 117.150(10) _cell_angle_gamma 90.00000 _cell_formula_units_Z 4 _cell_length_a 11.337(2) _cell_length_b 9.960(2) _cell_length_c 11.423(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 297 _cell_measurement_theta_max 14.2 _cell_measurement_theta_min 10.5 _cell_volume 1147.7(4) _computing_cell_refinement 'AFC/MSC Diffractometer Control System' _computing_data_collection 'AFC/MSC Diffractometer Control System (Rigaku Corporation, 1993)' _computing_data_reduction 'local programs' _computing_molecular_graphics CRYSTAN-GM _computing_publication_material CRYSTAN-GM _computing_structure_refinement CRYSTAN-GM _computing_structure_solution 'CRYSTAN-GM (Edwards et al., 1996)' _diffrn_measurement_device_type 'Rigaku AFC-5' _diffrn_measurement_method \q-2\q _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.018 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 2370 _diffrn_reflns_theta_max 26.0 _diffrn_standards_decay_% 3.6 _diffrn_standards_interval_count 100 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.079 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.194 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 448 _exptl_crystal_size_max 0.7 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.26 _refine_diff_density_min -0.33 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.09 _refine_ls_hydrogen_treatment constr _refine_ls_number_parameters 136 _refine_ls_number_reflns 1788 _refine_ls_R_factor_gt 0.065 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.0005 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0009F^2^]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.076 _reflns_number_gt 1063 _reflns_number_total 2249 _reflns_threshold_expression I>2\s(I) _cod_data_source_file qb0094.cif _cod_data_source_block QB0094 _cod_depositor_comments ; The following automatic conversions were performed: '_atom_site_thermal_displace_type' tag value 'Uij' was replaced with 'Uani' value 15 times. Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana ; _cod_original_sg_symbol_H-M 'P 21/a' _cod_database_code 2008504 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z -x+1/2,+y+1/2,-z +x+1/2,-y+1/2,+z 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 .111(2) .086(2) .0470(10) -.0170(10) .0090(10) -.0050(10) O2 .097(2) .100(2) .089(2) .0180(10) .0680(10) .0220(10) C3 .065(2) .064(2) .040(2) -.022(2) .0180(10) .001(2) C4 .074(2) .056(2) .051(2) -.011(2) .034(2) -.010(2) C5 .052(2) .055(2) .051(2) -.0070(10) .0250(10) .0000(10) C6 .052(2) .065(2) .047(2) .001(2) .0220(10) .005(2) C7 .058(2) .070(2) .0460(10) -.002(2) .0300(10) -.002(2) C8 .050(2) .063(2) .056(2) .008(2) .0270(10) .000(2) C9 .048(2) .054(2) .054(2) .0010(10) .0210(10) -.0010(10) C10 .071(2) .062(2) .074(2) -.004(2) .033(2) -.001(2) C11 .081(2) .068(2) .095(3) .018(2) .046(2) .025(2) C12 .050(2) .086(2) .070(2) .003(2) .0200(10) .019(2) C13 .0400(10) .060(2) .045(2) -.0050(10) .0140(10) .003(2) C14 .072(2) .074(2) .068(2) -.028(2) .025(2) -.001(2) C15 .086(2) .058(2) .082(2) .005(2) .047(2) .005(2) 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_occupancy O1 -.1042(2) .7161(2) .4954(2) .0970(10) Uani 1.000 O2 -.0770(2) .7297(2) .9423(2) .1030(10) Uani 1.000 C3 -.0234(3) .7354(3) .6094(3) .0650(10) Uani 1.000 C4 .0825(3) .6323(3) .6806(3) .0750(10) Uani 1.000 C5 .0698(3) .5514(3) .7896(3) .0620(10) Uani 1.000 C6 .0988(3) .6394(3) .9107(3) .0610(10) Uani 1.000 C7 -.0040(3) .7438(3) .8913(2) .0680(10) Uani 1.000 C8 -.0194(3) .8646(3) .8126(3) .0660(10) Uani 1.000 C9 .0881(3) .9260(3) .7859(3) .0620(10) Uani 1.000 C10 .0805(3) 1.0749(3) .7648(3) .082(2) Uani 1.000 C11 -.0622(3) 1.1045(3) .6664(3) .087(2) Uani 1.000 C12 -.1157(3) .9752(3) .5867(3) .072(2) Uani 1.000 C13 -.0291(2) .8622(3) .6732(2) .0550(10) Uani 1.000 C14 -.0695(3) .4896(3) .7354(3) .084(2) Uani 1.000 C15 .1736(3) .4391(3) .8353(3) .088(2) Uani 1.000 H4A .08310 .57010 .61670 .07 Uiso 1.000 H4B .16580 .67880 .72050 .07 Uiso 1.000 H6A .10880 .58220 .98240 .07 Uiso 1.000 H6B .18080 .68570 .93410 .07 Uiso 1.000 H8 -.07450 .93210 .82280 .07 Uiso 1.000 H9 .17260 .88170 .82160 .07 Uiso 1.000 H10A .10430 1.12130 .84610 .07 Uiso 1.000 H10B .13890 1.10260 .72940 .07 Uiso 1.000 H11A -.11290 1.12550 .71210 .07 Uiso 1.000 H11B -.06830 1.17810 .60960 .07 Uiso 1.000 H12A -.20700 .96010 .56510 .07 Uiso 1.000 H12B -.10740 .97950 .50680 .07 Uiso 1.000 H14A -.07920 .43980 .80250 .10 Uiso 1.000 H14B -.13440 .56000 .70370 .10 Uiso 1.000 H14C -.08330 .43070 .66370 .10 Uiso 1.000 H15A .16390 .38930 .90230 .10 Uiso 1.000 H15B .15980 .38120 .76290 .10 Uiso 1.000 H15C .26100 .47690 .87020 .10 Uiso 1.000 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag O1 C3 C4 119.7(3) no O1 C3 C13 118.9(3) no C4 C3 C13 121.4(3) no C3 C4 C5 116.5(3) no C4 C5 C6 111.5(3) no C4 C5 C14 109.9(3) no C4 C5 C15 108.4(3) no C6 C5 C14 110.4(3) no C6 C5 C15 107.1(3) no C14 C5 C15 109.5(3) no C5 C6 C7 115.4(3) no O2 C7 C6 120.0(3) no O2 C7 C8 118.1(3) no C6 C7 C8 121.8(3) no C7 C8 C9 125.1(3) no C7 C8 C13 123.5(3) no C9 C8 C13 58.9(2) yes C8 C9 C10 116.1(3) no C8 C9 C13 61.6(2) yes C10 C9 C13 108.5(3) no C9 C10 C11 105.9(3) no C10 C11 C12 106.0(3) no C11 C12 C13 105.8(3) no C3 C13 C8 121.6(3) no C3 C13 C9 124.3(3) no C3 C13 C12 118.2(3) no C8 C13 C9 59.5(2) yes C8 C13 C12 112.2(3) no C9 C13 C12 107.4(3) no C3 C4 H4A 108.1 no C3 C4 H4B 107.3 no C5 C4 H4A 108.2 no C5 C4 H4B 107.6 no H4A C4 H4B 109.0 no C5 C6 H6A 108.8 no C5 C6 H6B 107.8 no C7 C6 H6A 108.6 no C7 C6 H6B 107.2 no H6A C6 H6B 109.0 no C7 C8 H8 113.8 no C9 C8 H8 111.7 no C13 C8 H8 113.0 no C8 C9 H9 117.9 no C10 C9 H9 119.7 no C13 C9 H9 119.3 no C9 C10 H10A 110.5 no C9 C10 H10B 110.6 no C11 C10 H10A 110.9 no C11 C10 H10B 109.8 no H10A C10 H10B 109.0 no C10 C11 H11A 109.9 no C10 C11 H11B 111.8 no C12 C11 H11A 109.5 no C12 C11 H11B 110.7 no H11A C11 H11B 109.0 no C11 C12 H12A 111.8 no C11 C12 H12B 110.1 no C13 C12 H12A 110.6 no C13 C12 H12B 109.6 no H12A C12 H12B 108.9 no C5 C14 H14A 110.9 no C5 C14 H14B 109.2 no C5 C14 H14C 109.0 no H14A C14 H14B 109.3 no H14A C14 H14C 109.4 no H14B C14 H14C 109.0 no C5 C15 H15A 107.4 no C5 C15 H15B 110.3 no C5 C15 H15C 110.0 no H15A C15 H15B 110.1 no H15A C15 H15C 110.1 no H15B C15 H15C 108.9 no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1 C3 . . 1.218(4) yes O2 C7 . . 1.218(4) yes C3 C4 . . 1.505(5) yes C3 C13 . . 1.474(5) yes C4 C5 . . 1.544(5) yes C5 C6 . . 1.541(5) yes C5 C14 . . 1.537(5) yes C5 C15 . . 1.532(5) yes C6 C7 . . 1.501(5) yes C7 C8 . . 1.464(5) yes C8 C9 . . 1.514(5) yes C8 C13 . . 1.545(4) yes C9 C10 . . 1.499(5) yes C9 C13 . . 1.505(4) yes C10 C11 . . 1.519(5) yes C11 C12 . . 1.533(5) yes C12 C13 . . 1.524(4) yes C4 H4A . . .960 no C4 H4B . . .960 no C6 H6A . . .961 no C6 H6B . . .960 no C8 H8 . . .960 no C9 H9 . . .960 no C10 H10A . . .959 no C10 H10B . . .960 no C11 H11A . . .959 no C11 H11B . . .960 no C12 H12A . . .960 no C12 H12B . . .960 no C14 H14A . . .960 no C14 H14B . . .960 no C14 H14C . . .960 no C15 H15A . . .960 no C15 H15B . . .961 no C15 H15C . . .960 no