#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2200015.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_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_ _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 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance 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)