#------------------------------------------------------------------------------ #$Date: 2012-02-03 19:16:24 +0200 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/28/2012897.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_2012897 loop_ _publ_author_name 'Usman, Anwar' 'Razak, Ibrahim Abdul' 'Fun, Hoong-Kun' 'Chantrapromma, Suchada' 'Zhang, Yan' 'Xu, Jian-Hua' _publ_section_title ;11-Methyl-12a-phenyl-9a,12a-dihydrophenanthro[9',10':5,6][1,4]dioxino[2,3-d]oxazole and 9a-(10-hydroxyphenanthren-9-yl)-11,12a-diphenyl-9a,12a-dihydrophenanthro[9',10':5,6][1,4]dioxino[2,3-d]oxazole ; _journal_issue 8 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first o477 _journal_page_last o479 _journal_volume 58 _journal_year 2002 _chemical_formula_moiety 'C24 H17 N O3' _chemical_formula_sum 'C24 H17 N O3' _chemical_formula_weight 367.39 _chemical_melting_point 439.0(10) _chemical_name_systematic ; 11-Methyl-12a-phenyl-9a,12a-dihydrophenanthro[9',10':5,6][1,4]dioxino [2,3-d]oxazole ; _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' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL97 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.7633(4) _cell_length_b 10.9896(4) _cell_length_c 16.6210(7) _cell_measurement_reflns_used 3641 _cell_measurement_temperature 213(2) _cell_measurement_theta_max 28.32 _cell_measurement_theta_min 2.42 _cell_volume 1783.35(12) _computing_cell_refinement 'SAINT (Siemens, 1996)' _computing_data_collection 'SMART (Siemens, 1996)' _computing_data_reduction 'SAINT and SADABS (Sheldrick, 1996)' _computing_molecular_graphics SHELXTL _computing_publication_material 'SHELXTL, PARST (Nardelli, 1995) and PLATON (Spek, 1990)' _computing_structure_refinement SHELXTL _computing_structure_solution 'SHELXTL (Sheldrick, 1997)' _diffrn_ambient_temperature 213(2) _diffrn_detector_area_resol_mean 8.33 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type 'Siemens SMART CCD area-detector' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.104 _diffrn_reflns_av_sigmaI/netI 0.083 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 8619 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 2.42 _diffrn_standards_decay_% negligible _diffrn_standards_interval_count none _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.091 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.368 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description slab _exptl_crystal_F_000 768 _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.16 _refine_diff_density_max 0.23 _refine_diff_density_min -0.20 _refine_ls_extinction_coef 0.016(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXTL (Sheldrick, 1997)' _refine_ls_goodness_of_fit_ref 0.960 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 255 _refine_ls_number_reflns 1795 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.960 _refine_ls_R_factor_all 0.083 _refine_ls_R_factor_gt 0.052 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0605P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.109 _refine_ls_wR_factor_ref 0.122 _reflns_number_gt 1254 _reflns_number_total 1795 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file sk1563.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M P212121 _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: '_chemical_melting_point' value '439(1)K' was changed to '439.0(10)' - the value should be numeric and without a unit designator. Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana The following automatic conversions were performed: '_chemical_melting_point' value '439(1)K' was changed to '439.0(10)' - the value should be numeric and without a unit designator. '_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 2012897 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 0.6729(3) 0.6238(2) 0.17570(14) 0.0370(7) Uani d . 1 . . O O2 0.6269(3) 0.7719(2) 0.30598(15) 0.0369(8) Uani d . 1 . . O O3 0.4103(3) 0.6924(3) 0.28999(16) 0.0454(8) Uani d . 1 . . O N1 0.4359(4) 0.6013(3) 0.1691(2) 0.0395(9) Uani d . 1 . . N C1 0.7268(4) 0.5947(3) 0.2501(2) 0.0265(9) Uani d . 1 . . C C2 0.8128(4) 0.4914(3) 0.2546(2) 0.0267(9) Uani d . 1 . . C C3 0.8365(4) 0.4169(3) 0.1876(3) 0.0360(10) Uani d . 1 . . C H3 0.7943 0.4353 0.1389 0.043 Uiso calc R 1 . . H C4 0.9200(4) 0.3181(4) 0.1925(3) 0.0476(12) Uani d . 1 . . C H4 0.9359 0.2702 0.1474 0.057 Uiso calc R 1 . . H C5 0.9812(5) 0.2895(4) 0.2652(4) 0.0546(14) Uani d . 1 . . C H5 1.0363 0.2207 0.2693 0.066 Uiso calc R 1 . . H C6 0.9611(4) 0.3618(4) 0.3311(3) 0.0502(13) Uani d . 1 . . C H6 1.0032 0.3408 0.3794 0.060 Uiso calc R 1 . . H C7 0.8803(4) 0.4652(4) 0.3285(2) 0.0317(10) Uani d . 1 . . C C8 0.8631(4) 0.5488(4) 0.3955(2) 0.0358(11) Uani d . 1 . . C C9 0.9335(5) 0.5347(5) 0.4698(3) 0.0477(12) Uani d . 1 . . C H9 0.9899 0.4674 0.4773 0.057 Uiso calc R 1 . . H C10 0.9200(5) 0.6177(5) 0.5301(3) 0.0589(15) Uani d . 1 . . C H10 0.9675 0.6067 0.5781 0.071 Uiso calc R 1 . . H C11 0.8364(5) 0.7180(5) 0.5206(3) 0.0564(14) Uani d . 1 . . C H11 0.8289 0.7745 0.5620 0.068 Uiso calc R 1 . . H C12 0.7649(5) 0.7349(4) 0.4512(2) 0.0417(11) Uani d . 1 . . C H12 0.7077 0.8021 0.4456 0.050 Uiso calc R 1 . . H C13 0.7776(4) 0.6506(4) 0.3879(2) 0.0303(9) Uani d . 1 . . C C14 0.7072(4) 0.6687(3) 0.3130(2) 0.0301(10) Uani d . 1 . . C C15 0.5178(4) 0.7603(4) 0.2525(3) 0.0346(10) Uani d . 1 . . C H15 0.4834 0.8416 0.2392 0.041 Uiso calc R 1 . . H C16 0.3698(5) 0.6071(4) 0.2343(3) 0.0413(11) Uani d . 1 . . C C17 0.5460(4) 0.6908(3) 0.1740(2) 0.0302(9) Uani d . 1 . . C C18 0.5520(4) 0.7733(4) 0.1017(2) 0.0288(9) Uani d . 1 . . C C19 0.4348(5) 0.8356(4) 0.0793(2) 0.0473(13) Uani d . 1 . . C H19 0.3533 0.8224 0.1069 0.057 Uiso calc R 1 . . H C20 0.4385(6) 0.9175(4) 0.0158(3) 0.0550(14) Uani d . 1 . . C H20 0.3594 0.9592 0.0013 0.066 Uiso calc R 1 . . H C21 0.5564(5) 0.9374(4) -0.0253(3) 0.0487(13) Uani d . 1 . . C H21 0.5585 0.9927 -0.0676 0.058 Uiso calc R 1 . . H C22 0.6723(5) 0.8755(5) -0.0039(3) 0.0553(14) Uani d . 1 . . C H22 0.7528 0.8879 -0.0326 0.066 Uiso calc R 1 . . H C23 0.6715(4) 0.7942(4) 0.0602(2) 0.0429(11) Uani d . 1 . . C H23 0.7515 0.7541 0.0749 0.052 Uiso calc R 1 . . H C24 0.2524(5) 0.5318(4) 0.2599(3) 0.0618(15) Uani d . 1 . . C H24A 0.1744 0.5830 0.2692 0.093 Uiso calc R 1 . . H H24B 0.2754 0.4894 0.3086 0.093 Uiso calc R 1 . . H H24C 0.2312 0.4738 0.2185 0.093 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 0.0383(17) 0.0472(16) 0.0254(14) 0.0200(15) -0.0043(14) -0.0010(13) O2 0.0447(18) 0.0379(15) 0.0281(15) 0.0144(14) -0.0037(14) -0.0060(13) O3 0.0397(18) 0.0591(19) 0.0374(16) 0.0076(16) 0.0132(15) -0.0066(15) N1 0.042(2) 0.0354(19) 0.041(2) -0.0004(18) 0.005(2) -0.0009(17) C1 0.024(2) 0.0299(19) 0.025(2) 0.0023(18) 0.0018(19) 0.0025(18) C2 0.018(2) 0.029(2) 0.033(2) -0.0047(17) 0.0049(19) 0.0025(18) C3 0.027(2) 0.034(2) 0.046(3) 0.002(2) 0.010(2) 0.004(2) C4 0.035(3) 0.038(2) 0.070(3) 0.007(2) 0.009(3) -0.004(2) C5 0.031(3) 0.038(3) 0.095(4) 0.014(2) 0.006(3) 0.009(3) C6 0.027(3) 0.050(3) 0.073(3) 0.005(2) -0.003(3) 0.023(3) C7 0.019(2) 0.036(2) 0.040(2) -0.0027(18) 0.001(2) 0.014(2) C8 0.023(2) 0.048(2) 0.036(2) -0.007(2) 0.003(2) 0.013(2) C9 0.031(3) 0.069(3) 0.043(3) -0.002(3) -0.008(2) 0.021(3) C10 0.049(3) 0.093(4) 0.035(3) -0.015(3) -0.013(3) 0.014(3) C11 0.054(3) 0.084(4) 0.031(3) -0.016(3) -0.005(3) -0.006(3) C12 0.039(3) 0.054(3) 0.032(2) -0.007(2) -0.004(2) -0.001(2) C13 0.023(2) 0.043(2) 0.025(2) -0.006(2) -0.0009(18) 0.0048(19) C14 0.030(2) 0.028(2) 0.033(2) 0.0020(19) -0.003(2) 0.0040(19) C15 0.038(3) 0.040(2) 0.0255(19) 0.010(2) 0.001(2) 0.001(2) C16 0.039(3) 0.038(2) 0.047(3) 0.011(2) 0.012(2) 0.002(2) C17 0.031(2) 0.031(2) 0.028(2) 0.009(2) -0.001(2) 0.0002(18) C18 0.029(2) 0.037(2) 0.0200(19) 0.003(2) -0.0037(19) -0.0032(17) C19 0.035(3) 0.068(3) 0.039(2) 0.018(3) 0.005(2) 0.009(2) C20 0.052(3) 0.071(3) 0.042(3) 0.030(3) 0.003(3) 0.021(3) C21 0.059(3) 0.049(3) 0.038(3) 0.011(3) 0.004(3) 0.011(2) C22 0.043(3) 0.076(3) 0.047(3) -0.007(3) 0.008(3) 0.022(3) C23 0.024(2) 0.066(3) 0.039(2) 0.005(2) -0.002(2) 0.008(2) C24 0.054(3) 0.052(3) 0.079(4) 0.000(3) 0.027(3) 0.005(3) 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 . 1.381(4) yes O1 C17 . 1.441(4) yes O2 C14 . 1.384(4) yes O2 C15 . 1.393(5) yes O3 C16 . 1.375(5) yes O3 C15 . 1.431(5) yes N1 C16 . 1.264(5) yes N1 C17 . 1.459(5) yes C1 C14 . 1.339(5) ? C1 C2 . 1.414(5) ? C2 C3 . 1.401(5) ? C2 C7 . 1.423(5) ? C3 C4 . 1.360(5) ? C3 H3 . 0.9300 ? C4 C5 . 1.385(7) ? C4 H4 . 0.9300 ? C5 C6 . 1.367(7) ? C5 H5 . 0.9300 ? C6 C7 . 1.384(6) ? C6 H6 . 0.9300 ? C7 C8 . 1.454(6) ? C8 C13 . 1.402(5) ? C8 C9 . 1.420(6) ? C9 C10 . 1.362(6) ? C9 H9 . 0.9300 ? C10 C11 . 1.381(7) ? C10 H10 . 0.9300 ? C11 C12 . 1.361(6) ? C11 H11 . 0.9300 ? C12 C13 . 1.407(5) ? C12 H12 . 0.9300 ? C13 C14 . 1.436(5) ? C15 C17 . 1.537(6) ? C15 H15 . 0.9800 ? C16 C24 . 1.476(6) ? C17 C18 . 1.507(5) ? C18 C23 . 1.375(6) ? C18 C19 . 1.384(6) ? C19 C20 . 1.387(6) ? C19 H19 . 0.9300 ? C20 C21 . 1.356(6) ? C20 H20 . 0.9300 ? C21 C22 . 1.367(6) ? C21 H21 . 0.9300 ? C22 C23 . 1.389(6) ? C22 H22 . 0.9300 ? C23 H23 . 0.9300 ? C24 H24A . 0.9600 ? C24 H24B . 0.9600 ? C24 H24C . 0.9600 ? 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 0.0000 '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' N N 0.0061 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 '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 C1 O1 C17 117.6(3) C14 O2 C15 114.3(3) C16 O3 C15 105.9(3) C16 N1 C17 107.2(3) C14 C1 O1 120.3(3) C14 C1 C2 122.1(3) O1 C1 C2 117.4(3) C3 C2 C1 121.7(4) C3 C2 C7 119.4(3) C1 C2 C7 118.9(3) C4 C3 C2 121.1(4) C4 C3 H3 119.4 C2 C3 H3 119.4 C3 C4 C5 119.5(4) C3 C4 H4 120.2 C5 C4 H4 120.2 C6 C5 C4 120.3(4) C6 C5 H5 119.8 C4 C5 H5 119.8 C5 C6 C7 122.3(4) C5 C6 H6 118.9 C7 C6 H6 118.9 C6 C7 C2 117.2(4) C6 C7 C8 124.1(4) C2 C7 C8 118.7(3) C13 C8 C9 117.0(4) C13 C8 C7 120.2(4) C9 C8 C7 122.7(4) C10 C9 C8 121.3(4) C10 C9 H9 119.3 C8 C9 H9 119.3 C9 C10 C11 120.5(4) C9 C10 H10 119.8 C11 C10 H10 119.8 C12 C11 C10 120.7(5) C12 C11 H11 119.7 C10 C11 H11 119.7 C11 C12 C13 119.9(5) C11 C12 H12 120.1 C13 C12 H12 120.1 C8 C13 C12 120.7(4) C8 C13 C14 118.3(4) C12 C13 C14 120.9(4) C1 C14 O2 120.9(3) C1 C14 C13 121.6(3) O2 C14 C13 117.3(3) O2 C15 O3 109.3(3) O2 C15 C17 116.8(3) O3 C15 C17 104.0(3) O2 C15 H15 108.8 O3 C15 H15 108.8 C17 C15 H15 108.8 N1 C16 O3 117.7(4) N1 C16 C24 128.0(4) O3 C16 C24 114.4(4) O1 C17 N1 106.9(3) O1 C17 C18 106.9(3) N1 C17 C18 112.9(3) O1 C17 C15 113.0(3) N1 C17 C15 104.5(3) C18 C17 C15 112.6(3) C23 C18 C19 118.9(4) C23 C18 C17 122.3(4) C19 C18 C17 118.7(4) C18 C19 C20 120.3(4) C18 C19 H19 119.9 C20 C19 H19 119.9 C21 C20 C19 120.6(5) C21 C20 H20 119.7 C19 C20 H20 119.7 C20 C21 C22 119.4(4) C20 C21 H21 120.3 C22 C21 H21 120.3 C21 C22 C23 121.0(5) C21 C22 H22 119.5 C23 C22 H22 119.5 C18 C23 C22 119.8(4) C18 C23 H23 120.1 C22 C23 H23 120.1 C16 C24 H24A 109.5 C16 C24 H24B 109.5 H24A C24 H24B 109.5 C16 C24 H24C 109.5 H24A C24 H24C 109.5 H24B C24 H24C 109.5 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 C17 O1 C1 C14 -31.7(5) C17 O1 C1 C2 154.2(3) C14 C1 C2 C3 -177.7(4) O1 C1 C2 C3 -3.7(5) C14 C1 C2 C7 0.2(5) O1 C1 C2 C7 174.2(3) C1 C2 C3 C4 179.7(4) C7 C2 C3 C4 1.7(6) C2 C3 C4 C5 1.0(6) C3 C4 C5 C6 -1.9(7) C4 C5 C6 C7 0.0(7) C5 C6 C7 C2 2.7(6) C5 C6 C7 C8 -175.9(4) C3 C2 C7 C6 -3.5(5) C1 C2 C7 C6 178.5(4) C3 C2 C7 C8 175.2(4) C1 C2 C7 C8 -2.8(5) C6 C7 C8 C13 -179.1(4) C2 C7 C8 C13 2.3(5) C6 C7 C8 C9 2.9(6) C2 C7 C8 C9 -175.7(4) C13 C8 C9 C10 -1.1(6) C7 C8 C9 C10 177.0(4) C8 C9 C10 C11 0.3(7) C9 C10 C11 C12 0.8(8) C10 C11 C12 C13 -1.0(7) C9 C8 C13 C12 0.9(6) C7 C8 C13 C12 -177.2(4) C9 C8 C13 C14 178.8(4) C7 C8 C13 C14 0.7(5) C11 C12 C13 C8 0.1(6) C11 C12 C13 C14 -177.7(4) O1 C1 C14 O2 3.5(6) C2 C1 C14 O2 177.3(3) O1 C1 C14 C13 -170.9(3) C2 C1 C14 C13 2.9(6) C15 O2 C14 C1 33.0(5) C15 O2 C14 C13 -152.4(3) C8 C13 C14 C1 -3.3(6) C12 C13 C14 C1 174.6(4) C8 C13 C14 O2 -177.9(3) C12 C13 C14 O2 0.0(5) C14 O2 C15 O3 77.5(4) C14 O2 C15 C17 -40.1(5) C16 O3 C15 O2 -133.2(3) C16 O3 C15 C17 -7.8(4) C17 N1 C16 O3 1.9(5) C17 N1 C16 C24 -177.4(4) C15 O3 C16 N1 4.2(5) C15 O3 C16 C24 -176.4(3) C1 O1 C17 N1 -92.7(4) C1 O1 C17 C18 146.1(3) C1 O1 C17 C15 21.7(5) C16 N1 C17 O1 113.4(4) C16 N1 C17 C18 -129.4(4) C16 N1 C17 C15 -6.7(4) O2 C15 C17 O1 13.5(5) O3 C15 C17 O1 -107.0(3) O2 C15 C17 N1 129.3(4) O3 C15 C17 N1 8.8(4) O2 C15 C17 C18 -107.7(4) O3 C15 C17 C18 131.8(3) O1 C17 C18 C23 -12.9(5) N1 C17 C18 C23 -130.1(4) C15 C17 C18 C23 111.8(4) O1 C17 C18 C19 170.9(3) N1 C17 C18 C19 53.7(5) C15 C17 C18 C19 -64.4(5) C23 C18 C19 C20 0.1(7) C17 C18 C19 C20 176.4(4) C18 C19 C20 C21 0.3(7) C19 C20 C21 C22 0.3(8) C20 C21 C22 C23 -1.2(8) C19 C18 C23 C22 -1.0(6) C17 C18 C23 C22 -177.1(4) C21 C22 C23 C18 1.5(7)