#------------------------------------------------------------------------------ #$Date: 2015-04-02 12:22:18 +0100 (Thu, 02 Apr 2015) $ #$Revision: 134621 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/55/2005545.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_2005545 loop_ _publ_author_name 'Chiaroni, A.' 'Riche, C.' 'Benharref, A.' 'Lassaba, E.' 'Baouid, A.' _publ_contact_author ; Dr Claude Riche Institut de Chimie des Substances Naturelles C.N.R.S. 91198 Gif-sur-Yvette CEDEX France ; _publ_section_title ; 2\a,3\a:6\a,7\a-Di\'epoxyhimachalane ; _journal_issue 10 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 2504 _journal_page_last 2507 _journal_paper_doi 10.1107/S0108270196005756 _journal_volume 52 _journal_year 1996 _chemical_formula_moiety 'C15 H24 O2' _chemical_formula_sum 'C15 H24 O2' _chemical_formula_weight 236.35 _chemical_name_systematic ; 2\a ,3\a ,6\a ,7\a-di\'epoxyhimachalane ; _space_group_IT_number 4 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _atom_type_scat_source IntTabIV _cell_angle_alpha 90.00 _cell_angle_beta 104.31(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 8.537(2) _cell_length_b 8.221(2) _cell_length_c 10.364(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293 _cell_measurement_theta_max 24.2 _cell_measurement_theta_min 16.5 _cell_volume 704.8(3) _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_data_reduction 'PHIL (Riche, 1981)' _computing_molecular_graphics 'R3M (Riche, 1983), ORTEP (Johnson, 1965)' _computing_publication_material 'ACTACIF (Riche, 1992)' _computing_structure_refinement 'SHELX76 (Sheldrick, 1976)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1985)' _diffrn_ambient_temperature 293 _diffrn_measurement_device 'Nonius CAD4 diffractometer' _diffrn_measurement_method \q/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_reflns_av_R_equivalents 0.030 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 1864 _diffrn_reflns_theta_max 66.78 _diffrn_reflns_theta_min 4.40 _diffrn_standards_decay_% 3 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.52 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.11 _exptl_crystal_description prism _exptl_crystal_F_000 260.00 _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.24 _refine_diff_density_max 0.35 _refine_diff_density_min -0.43 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 0.59 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 166 _refine_ls_number_reflns 1694 _refine_ls_R_factor_obs 0.059 _refine_ls_shift/esd_max 0.02 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/[\s^2^(F)]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_obs 0.070 _reflns_number_observed 1709 _reflns_number_total 1757 _reflns_observed_criterion refl_observed_if_I_>_3.0_sigma(I) _[local]_cod_data_source_file pa1235.cif _[local]_cod_data_source_block diepohima _[local]_cod_cif_authors_sg_H-M 'P 21' _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w = 1/[\s^2^(F)]' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1/[\s^2^(F)]'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 704.8(2) _cod_database_code 2005545 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,-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 C1 0.0603(18) 0.0425(15) 0.0463(16) -0.0012(14) 0.0178(13) 0.0015(14) C2 0.0683(19) 0.0444(16) 0.0548(18) 0.0095(15) 0.0196(15) -0.0056(14) C3 0.0648(18) 0.063(2) 0.071(2) -0.0074(17) 0.0233(16) -0.0128(17) C4 0.103(3) 0.055(2) 0.089(3) -0.017(2) 0.043(2) -0.006(2) C5 0.086(3) 0.0477(18) 0.079(2) 0.0136(17) 0.038(2) 0.0098(18) C6 0.0605(17) 0.0550(18) 0.0582(17) 0.0103(16) 0.0270(14) 0.0102(16) C7 0.061(2) 0.106(3) 0.076(2) 0.014(2) 0.0203(18) 0.010(3) C8 0.065(2) 0.149(5) 0.102(3) -0.019(3) 0.012(2) 0.008(3) C9 0.099(3) 0.141(4) 0.093(3) -0.034(4) 0.005(3) -0.026(3) C10 0.096(4) 0.112(6) 0.051(3) -0.002(3) 0.020(3) -0.014(3) C11 0.075(2) 0.0566(19) 0.0505(18) 0.0046(18) 0.0206(16) -0.0047(15) C12 0.075(2) 0.113(4) 0.116(3) -0.020(3) 0.026(2) -0.030(3) C13 0.091(3) 0.168(5) 0.120(4) 0.068(3) 0.028(3) 0.046(4) C14 0.121(6) 0.055(3) 0.073(4) 0.004(3) 0.045(4) -0.015(3) C15 0.094(5) 0.085(4) 0.075(4) -0.003(3) 0.054(4) -0.009(3) O16 0.0830(15) 0.0581(14) 0.0563(12) -0.0045(12) 0.0218(11) -0.0078(11) O17 0.0722(14) 0.0848(18) 0.0772(15) 0.0189(13) 0.0387(12) 0.0118(14) 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_calc_attached_atom C1 0.5240(4) 0.5143 0.3385(3) 0.051(3) Uani ? ? C2 0.6802(4) 0.5422(5) 0.4424(3) 0.058(3) Uani ? ? C3 0.7642(4) 0.6968(6) 0.4597(3) 0.068(4) Uani ? ? C4 0.6937(5) 0.8376(6) 0.3743(4) 0.084(5) Uani ? ? C5 0.5165(4) 0.8279(5) 0.3030(4) 0.073(4) Uani ? ? C6 0.4267(3) 0.6710(5) 0.3139(3) 0.059(3) Uani ? ? C7 0.2532(4) 0.6603(7) 0.2521(4) 0.083(5) Uani ? ? C8 0.1831(5) 0.4903(8) 0.2084(6) 0.108(7) Uani ? ? C9 0.2440(6) 0.4186(9) 0.0915(5) 0.115(6) Uani ? ? C10 0.4131(7) 0.4669(9) 0.0888(5) 0.088(8) Uani ? ? C11 0.5533(4) 0.4334(6) 0.2093(3) 0.062(3) Uani ? ? C12 0.9424(5) 0.7051(7) 0.5196(5) 0.105(6) Uani ? ? C13 0.1630(6) 0.8002(8) 0.1776(6) 0.130(7) Uani ? ? C14 0.5801(10) 0.2551(8) 0.2352(6) 0.085(8) Uani ? ? C15 0.7066(8) 0.5066(8) 0.1742(6) 0.086(8) Uani ? ? O16 0.6671(3) 0.6467(4) 0.5518(2) 0.068(2) Uani ? ? O17 0.3078(3) 0.6844(5) 0.3942(2) 0.080(3) Uani ? ? C10' 0.396(2) 0.334(3) 0.1372(17) 0.103(6) Uiso ? ? C14' 0.681(2) 0.292(2) 0.2464(17) 0.090(5) Uiso ? ? C15' 0.597(2) 0.543(2) 0.1159(15) 0.082(5) Uiso ? ? H1 0.45681 0.43330 0.37285 0.056 Uiso calc C1 H2 0.71832 0.42984 0.42934 0.063 Uiso calc C2 H4a 0.75616 0.85092 0.30512 0.093 Uiso calc C4 H4b 0.70881 0.93653 0.43224 0.093 Uiso calc C4 H5a 0.50793 0.84757 0.20627 0.080 Uiso calc C5 H5b 0.45976 0.91739 0.33858 0.080 Uiso calc C5 H8a 0.06257 0.49877 0.18031 0.119 Uiso calc C8 H8b 0.21442 0.41473 0.28613 0.119 Uiso calc C8 H9a 0.24282 0.29715 0.09608 0.126 Uiso calc C9 H9b 0.17181 0.45537 0.00512 0.126 Uiso calc C9 H10a 0.44469 0.40948 0.01401 0.097 Uiso calc C10 H10b 0.41766 0.58715 0.07551 0.097 Uiso calc C10 H12a 0.97877 0.82103 0.52353 0.115 Uiso calc C12 H12b 0.96736 0.65887 0.61169 0.115 Uiso calc C12 H12c 1.00040 0.64096 0.46376 0.115 Uiso calc C12 H13a 0.04671 0.76989 0.14298 0.143 Uiso calc C13 H13b 0.17134 0.89595 0.23850 0.143 Uiso calc C13 H13c 0.21014 0.82896 0.10137 0.143 Uiso calc C13 H14a 0.67270 0.23873 0.31469 0.093 Uiso calc C14 H14b 0.48032 0.20526 0.25238 0.093 Uiso calc C14 H14c 0.60516 0.20205 0.15580 0.093 Uiso calc C14 H15a 0.72312 0.45346 0.09176 0.094 Uiso calc C15 H15b 0.69158 0.62625 0.15881 0.094 Uiso calc C15 H15c 0.80343 0.48685 0.24956 0.094 Uiso calc C15 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -4 1 1 -3 -3 2 2 2 2 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 C2 C1 C6 109.9(2) yes C2 C1 C11 112.0(2) yes C6 C1 C11 114.3(2) yes C1 C2 C3 123.0(3) yes C1 C2 O16 115.0(3) yes C3 C2 O16 60.9(2) yes C2 C3 C4 119.5(3) yes C2 C3 C12 120.9(4) yes C2 C3 O16 59.5(2) yes C4 C3 C12 115.6(4) yes C4 C3 O16 113.2(3) yes C12 C3 O16 115.0(3) yes C3 C4 C5 117.3(4) yes C4 C5 C6 118.1(3) yes C1 C6 C5 117.9(3) yes C1 C6 C7 118.3(3) yes C1 C6 O17 113.2(3) yes C5 C6 C7 119.5(3) yes C5 C6 O17 114.2(3) yes C7 C6 O17 59.1(2) yes C6 C7 C8 117.4(4) yes C6 C7 C13 121.2(4) yes C6 C7 O17 60.6(3) yes C8 C7 C13 115.7(4) yes C8 C7 O17 115.3(4) yes C13 C7 O17 114.7(4) yes C7 C8 C9 113.1(4) yes C8 C9 C10 115.1(5) yes C8 C9 C10' 112.0(9) yes C10 C9 C10' 49.1(8) yes C9 C10 C11 119.9(5) yes C1 C11 C10 111.3(3) yes C1 C11 C14 108.2(4) yes C1 C11 C15 110.8(3) yes C1 C11 C10' 108.9(7) yes C1 C11 C14' 110.6(7) yes C1 C11 C15' 115.6(7) yes C10 C11 C14 112.2(4) yes C10 C11 C15 105.8(4) yes C14 C11 C15 108.6(4) yes C10' C11 C14' 100.8(10) yes C10' C11 C15' 109.4(10) yes C14' C11 C15' 110.5(10) yes C2 O16 C3 59.6(2) yes C6 O17 C7 60.3(3) yes C9 C10' C11 119.5(13) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag C1 C2 1.510(4) yes C1 C6 1.519(4) yes C1 C11 1.569(4) yes C2 C3 1.449(6) yes C2 O16 1.448(4) yes C3 C4 1.491(6) yes C3 C12 1.496(6) yes C3 O16 1.469(4) yes C4 C5 1.512(6) yes C5 C6 1.519(6) yes C6 C7 1.464(5) yes C6 O17 1.468(4) yes C7 C8 1.543(8) yes C7 C13 1.490(8) yes C7 O17 1.445(4) yes C8 C9 1.548(8) yes C9 C10 1.504(8) yes C9 C10' 1.444(19) yes C10 C11 1.526(7) yes C11 C14 1.498(8) yes C11 C15 1.563(8) yes C11 C14' 1.576(19) yes C11 C15' 1.435(17) yes 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 _geom_torsion_publ_flag C6 C1 C2 C3 -31.1(3) yes C1 C2 C3 C4 1.5(3) yes C2 C3 C4 C5 17.7(4) yes C3 C4 C5 C6 -5.0(3) yes C4 C5 C6 C1 -26.8(3) yes C5 C6 C1 C2 43.0(3) yes C11 C1 C6 C7 72.9(3) yes C1 C6 C7 C8 -3.6(3) yes C6 C7 C8 C9 -67.3(5) yes C7 C8 C9 C10 32.2(5) yes C7 C8 C9 C10' 86.0(9) yes C8 C9 C10 C11 56.3(5) yes C8 C9 C10' C11 -65.2(11) yes C9 C10 C11 C1 -56.8(5) yes C9 C10' C11 C1 60.7(10) yes C10 C11 C1 C6 -31.3(3) yes C10' C11 C1 C6 -80.7(8) yes