#------------------------------------------------------------------------------ #$Date: 2012-02-03 19:16:24 +0200 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/20/00/2200015.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_2200015 loop_ _publ_author_name 'Yokochi, Alex F. T.' 'White, James D.' 'Sturtz, George' _publ_section_title ; Vulgarone B ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o99 _journal_page_last o101 _journal_volume 57 _journal_year 2001 _chemical_formula_sum 'C15 H22 O' _chemical_formula_weight 218.33 _space_group_IT_number 19 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 6.6280(10) _cell_length_b 10.2180(10) _cell_length_c 19.8890(10) _cell_measurement_reflns_used 99 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.28 _cell_measurement_theta_min 8.02 _cell_volume 1347.0(3) _computing_cell_refinement XSCANS _computing_data_collection 'XSCANS (Siemens, 1996)' _computing_data_reduction XSCANS _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_device_type 'Serial diffractometer' _diffrn_measurement_method \w/2\q _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents .041 _diffrn_reflns_av_sigmaI/netI .0403 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 2270 _diffrn_reflns_theta_max 67.58 _diffrn_reflns_theta_min 4.45 _diffrn_standards_decay_% 1 _diffrn_standards_interval_count 97 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu .495 _exptl_absorpt_correction_T_max .8657 _exptl_absorpt_correction_T_min .8266 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ; via \y scans ((North et al., 1968) using XEMP (Siemens, 1990) ; _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 1.077 _exptl_crystal_density_meas 'Not measured' _exptl_crystal_density_method 'Not measured' _exptl_crystal_description Block _exptl_crystal_F_000 480 _exptl_crystal_size_max .4 _exptl_crystal_size_mid .4 _exptl_crystal_size_min .3 _refine_diff_density_max .122 _refine_diff_density_min -.135 _refine_ls_abs_structure_details 'Flack (1983)' _refine_ls_abs_structure_Flack 'not reliably determined [-0.7(6)]' _refine_ls_extinction_coef .0052(12) _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 176 _refine_ls_number_reflns 1911 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.069 _refine_ls_R_factor_all .056 _refine_ls_R_factor_gt .050 _refine_ls_shift/su_max .001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0858P)^2^+0.0511P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .132 _reflns_number_gt 1666 _reflns_number_total 1911 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file bt6000.cif _[local]_cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2200015 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol O1 .7435(3) .5483(2) .46305(11) .1032(7) Uani d . 1 . . O C1 .5760(3) .5489(2) .43741(11) .0706(6) Uani d . 1 . . C C2 .4529(4) .6664(2) .43026(12) .0739(6) Uani d . 1 . . C H2 .5013 .7476 .4439 .095(3) Uiso calc R 1 . . H C3 .2689(4) .6543(2) .40359(10) .0685(6) Uani d . 1 . . C C31 .1219(5) .7633(3) .39466(13) .0932(8) Uani d . 1 . . C H31A .0104 .7514 .4249 .141(4) Uiso calc R 1 . . H H31B .0735 .7637 .3492 .141(4) Uiso calc R 1 . . H H31C .1871 .8452 .4042 .141(4) Uiso calc R 1 . . H C4 .2094(3) .5195(2) .38143(10) .0654(6) Uani d . 1 A . C H4 .0766 .5116 .3602 .095(3) Uiso calc R 1 . . H C5 .3913(3) .4655(2) .34020(10) .0644(6) Uani d . 1 A . C H5 .4690 .5392 .3223 .095(3) Uiso calc R 1 . . H C6 .3674(4) .3624(2) .28532(13) .0837(7) Uani d . 1 . . C C61 .2627(7) .4305(4) .22528(16) .1334(14) Uani d . 1 A . C H61A .2533 .3705 .1883 .141(4) Uiso calc R 1 . . H H61B .3401 .5056 .2119 .141(4) Uiso calc R 1 . . H H61C .1298 .4578 .2384 .141(4) Uiso calc R 1 . . H C62 .5757(6) .3206(4) .26353(18) .1190(12) Uani d . 1 A . C H62A .5649 .2598 .2269 .141(4) Uiso calc R 1 . . H H62B .6437 .2794 .3005 .141(4) Uiso calc R 1 . . H H62C .6510 .3959 .2493 .141(4) Uiso calc R 1 . . H C71 .2145(19) .2555(10) .2987(6) .098(3) Uani d P .565(14) A 1 C H71A .0800 .2919 .2945 .095(3) Uiso calc PR .565(14) A 1 H H71B .2291 .1881 .2647 .095(3) Uiso calc PR .565(14) A 1 H C81 .2355(19) .1934(7) .3674(4) .105(3) Uani d P .565(14) A 1 C H81A .1565 .1136 .3690 .095(3) Uiso calc PR .565(14) A 1 H H81B .3757 .1706 .3752 .095(3) Uiso calc PR .565(14) A 1 H C91 .167(2) .2825(15) .4200(8) .094(5) Uani d P .565(14) A 1 C H91A .1715 .2321 .4613 .095(3) Uiso calc PR .565(14) A 1 H H91B .0255 .2982 .4108 .095(3) Uiso calc PR .565(14) A 1 H C72 .295(3) .2293(16) .3175(8) .106(4) Uani d P .435(14) A 2 C H72A .2717 .1662 .2819 .095(3) Uiso calc PR .435(14) A 2 H H72B .4011 .1954 .3461 .095(3) Uiso calc PR .435(14) A 2 H C82 .1036(19) .2432(10) .3587(5) .096(4) Uani d P .435(14) A 2 C H82A .0323 .1603 .3586 .095(3) Uiso calc PR .435(14) A 2 H H82B .0170 .3078 .3376 .095(3) Uiso calc PR .435(14) A 2 H C92 .146(3) .2866(13) .4358(11) .075(4) Uani d P .435(14) A 2 C H92A .0186 .2941 .4596 .095(3) Uiso calc PR .435(14) A 2 H H92B .2262 .2202 .4580 .095(3) Uiso calc PR .435(14) A 2 H C10 .2574(3) .4183(2) .43794(11) .0682(6) Uani d . 1 . . C C101 .2191(4) .4569(3) .51137(11) .0833(7) Uani d . 1 A . C H10A .0786 .4764 .5174 .141(4) Uiso calc R 1 . . H H10B .2981 .5327 .5223 .141(4) Uiso calc R 1 . . H H10C .2567 .3857 .5403 .141(4) Uiso calc R 1 . . H C11 .4774(3) .4276(2) .41107(11) .0665(6) Uani d . 1 A . C H11 .5576 .3472 .4132 .095(3) Uiso calc R 1 . . H 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 .0654(11) .1316(16) .1126(14) -.0036(11) -.0180(10) -.0206(12) C1 .0560(12) .0910(15) .0649(11) -.0036(11) -.0026(10) -.0031(11) C2 .0859(17) .0690(13) .0668(12) -.0056(12) -.0046(13) -.0065(10) C3 .0822(17) .0703(12) .0530(9) .0134(12) .0073(12) .0036(9) C31 .115(2) .0872(16) .0778(14) .0329(16) .0104(15) .0097(13) C4 .0529(11) .0794(13) .0638(11) -.0003(10) -.0059(10) .0037(10) C5 .0616(12) .0661(11) .0655(11) -.0043(11) -.0018(10) -.0037(9) C6 .0855(16) .0822(15) .0833(15) -.0123(14) .0031(14) -.0230(12) C61 .165(4) .144(3) .0909(19) -.007(3) -.036(2) -.037(2) C62 .120(3) .127(2) .109(2) .008(2) .021(2) -.046(2) C71 .116(8) .077(4) .101(6) -.025(4) -.025(5) -.013(4) C81 .120(6) .070(3) .125(6) -.017(4) -.007(5) .013(3) C91 .067(5) .125(8) .091(10) -.014(4) .015(5) .028(5) C72 .110(11) .103(9) .105(9) -.024(7) .000(6) -.036(7) C82 .089(6) .075(4) .123(7) -.020(4) .002(5) -.014(4) C92 .099(9) .059(5) .068(7) -.015(4) .025(4) .010(3) C10 .0576(12) .0760(13) .0709(12) .0017(11) .0026(11) .0119(10) C101 .0750(14) .1046(17) .0703(13) .0082(15) .0099(11) .0212(12) C11 .0563(12) .0705(12) .0727(12) .0053(10) -.0030(10) .0022(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 O1 C1 . 1.222(3) ? C1 C2 . 1.458(3) ? C1 C11 . 1.496(3) ? C2 C3 . 1.336(4) ? C3 C31 . 1.491(3) ? C3 C4 . 1.498(3) ? C4 C5 . 1.559(3) ? C4 C10 . 1.560(3) ? C5 C6 . 1.525(3) ? C5 C11 . 1.569(3) ? C6 C62 . 1.509(5) ? C6 C71 . 1.514(12) ? C6 C61 . 1.546(5) ? C6 C72 . 1.579(17) ? C71 C81 . 1.512(16) ? C81 C91 . 1.459(17) ? C91 C10 . 1.553(15) ? C72 C82 . 1.52(2) ? C82 C92 . 1.62(2) ? C92 C10 . 1.537(15) ? C10 C101 . 1.534(3) ? C10 C11 . 1.556(3) ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0181 .0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0492 .0322 '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_publ_flag O1 C1 C2 123.6(2) ? O1 C1 C11 122.6(2) ? C2 C1 C11 113.78(19) ? C3 C2 C1 118.2(2) ? C2 C3 C31 125.1(2) ? C2 C3 C4 116.2(2) ? C31 C3 C4 118.7(2) ? C3 C4 C5 106.07(18) ? C3 C4 C10 110.09(16) ? C5 C4 C10 89.24(16) y C6 C5 C4 122.73(19) ? C6 C5 C11 120.70(19) ? C4 C5 C11 84.03(15) y C62 C6 C71 117.3(5) ? C62 C6 C5 107.8(2) ? C71 C6 C5 116.2(5) ? C62 C6 C61 108.4(3) ? C71 C6 C61 99.2(5) ? C5 C6 C61 106.8(2) ? C62 C6 C72 98.7(7) ? C71 C6 C72 26.2(5) ? C5 C6 C72 109.6(5) ? C61 C6 C72 124.4(7) ? C81 C71 C6 113.6(8) ? C91 C81 C71 111.0(10) ? C81 C91 C10 127.1(11) ? C82 C72 C6 113.2(13) ? C72 C82 C92 113.1(12) ? C10 C92 C82 110.5(12) ? C101 C10 C92 99.9(8) ? C101 C10 C91 112.6(6) ? C92 C10 C91 12.9(13) ? C101 C10 C11 117.80(19) ? C92 C10 C11 119.7(8) ? C91 C10 C11 109.7(6) ? C101 C10 C4 118.83(19) ? C92 C10 C4 117.5(8) ? C91 C10 C4 110.4(6) ? C11 C10 C4 84.44(15) y C1 C11 C10 109.86(19) ? C1 C11 C5 105.62(18) ? C10 C11 C5 89.02(15) y