#------------------------------------------------------------------------------ #$Date: 2012-02-03 18:16:24 +0100 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/04/2100416.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_2100416 loop_ _publ_author_name 'Jurchescu, Oana D.' 'Meetsma, Auke' 'Palstra, Thomas T.M.' _publ_section_title ; Low-temperature structure of rubrene single crystals grown by vapor transport ; _journal_coeditor_code BK5027 _journal_issue 2 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 330 _journal_page_last 334 _journal_volume 62 _journal_year 2006 _chemical_formula_moiety 'C42 H28' _chemical_formula_sum 'C42 H28' _chemical_formula_weight 532.68 _chemical_name_systematic ' ?' _space_group_IT_number 64 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-C 2ac 2' _symmetry_space_group_name_H-M 'C m c a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary direct _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 26.938(5) _cell_length_b 7.2110(10) _cell_length_c 14.461(3) _cell_measurement_reflns_used 3697 _cell_measurement_temperature 275.0(10) _cell_measurement_theta_max 27.19 _cell_measurement_theta_min 2.82 _cell_volume 2809.0(9) _computing_cell_refinement 'SAINT, Bruker Version 6.02A, 2000' _computing_data_collection 'SMART, Bruker Version 5.624, 2001' _computing_data_reduction 'XPREP, Bruker Version 5.1/NT, 2000' _computing_molecular_graphics ; PLUTO (Meetsma, 2004) PLATON (Spek, 2003) ; _computing_publication_material 'PLATON (Spek, 2003)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution ; SIR-97 (Altomare et al., 1999) ; _diffrn_ambient_temperature 275.0(10) _diffrn_detector_area_resol_mean '4096x4096 / 62x62 (binned 512)' _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type ; Bruker Smart Apex; CCD area detector ; _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator 'parallel mounted graphite' _diffrn_radiation_source 'fine focus sealed Siemens Mo tube ' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0503 _diffrn_reflns_av_sigmaI/netI 0.0511 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 10370 _diffrn_reflns_reduction_process ; Intensity data were corrected for Lorentz and polarization effects, decay and absorption and reduced to F~o~^2^ using SAINT (Bruker, 2000) and SADABS (Sheldrick, 2001) ; _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_min 3.20 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.071 _exptl_absorpt_correction_T_max 0.9957 _exptl_absorpt_correction_T_min 0.9477 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS, Sheldrick, Bruker, 2000))' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.259 _exptl_crystal_density_method 'not measured' _exptl_crystal_description platelet _exptl_crystal_F_000 1120 _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.03 _refine_diff_density_max 0.174 _refine_diff_density_min -0.156 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 124 _refine_ls_number_reflns 1466 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.050 _refine_ls_R_factor_all 0.0675 _refine_ls_R_factor_gt 0.0419 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ;calc w=1/[\s^2^(Fo^2^)+(0.0656P)^2^+0.4032P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1097 _refine_ls_wR_factor_ref 0.1248 _reflns_number_gt 1036 _reflns_number_total 1466 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file bk5027.cif _[local]_cod_data_source_block 275K _[local]_cod_cif_authors_sg_Hall '-C 2bc 2' _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. '_exptl_absorpt_correction_type' value 'Multi-Scan' changed to 'multi-scan' 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. '_exptl_absorpt_correction_type' value 'Multi-Scan' changed to 'multi-scan' 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_original_cell_volume 2809.1(9) _cod_database_code 2100416 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2-y,1/2+z 3 x,-y,-z 4 -x,1/2+y,1/2-z 5 -x,-y,-z 6 x,1/2+y,1/2-z 7 -x,y,z 8 x,1/2-y,1/2+z 9 1/2+x,1/2+y,z 10 1/2-x,-y,1/2+z 11 1/2+x,1/2-y,-z 12 1/2-x,y,1/2-z 13 1/2-x,1/2-y,-z 14 1/2+x,y,1/2-z 15 1/2-x,1/2+y,z 16 1/2+x,-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 C1 0.0327(11) 0.0304(10) 0.0251(9) 0.0000 0.0000 -0.0019(8) C2 0.0346(9) 0.0310(7) 0.0248(7) 0.0035(6) 0.0017(6) -0.0013(6) C3 0.0402(8) 0.0297(7) 0.0230(7) 0.0023(6) 0.0009(6) -0.0012(5) C4 0.0454(11) 0.0365(8) 0.0343(8) 0.0069(7) 0.0020(7) 0.0043(7) C5 0.0584(11) 0.0337(8) 0.0379(9) 0.0075(7) 0.0014(8) 0.0080(7) C6 0.0340(9) 0.0351(7) 0.0295(7) 0.0033(6) -0.0003(6) 0.0063(6) C7 0.0391(10) 0.0411(9) 0.0473(10) 0.0035(8) 0.0062(8) 0.0020(8) C8 0.0383(11) 0.0596(11) 0.0700(13) 0.0077(9) 0.0104(9) 0.0108(10) C9 0.0377(12) 0.0814(14) 0.0687(14) -0.0016(10) -0.0074(10) 0.0196(12) C10 0.0566(13) 0.0780(13) 0.0452(11) -0.0076(11) -0.0159(9) 0.0001(10) C11 0.0442(11) 0.0551(10) 0.0354(9) 0.0028(8) -0.0015(8) -0.0026(8) loop_ _atom_site_type_symbol _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 C C1 0.02714(7) 0.00000 0.00000 0.0294(6) Uani 1.000 C C2 0.05290(5) -0.14318(18) 0.04901(9) 0.0301(4) Uani 1.000 C C3 0.02661(5) -0.29299(18) 0.08757(9) 0.0310(4) Uani 1.000 C C4 0.05169(7) -0.4439(2) 0.13369(10) 0.0387(5) Uani 1.000 C C5 0.02612(7) -0.5841(2) 0.17468(11) 0.0433(5) Uani 1.000 C C6 0.10704(6) -0.13275(19) 0.07255(10) 0.0329(4) Uani 1.000 C C7 0.14248(6) -0.2446(2) 0.03009(12) 0.0425(6) Uani 1.000 C C8 0.19109(7) -0.2464(3) 0.06060(15) 0.0560(7) Uani 1.000 C C9 0.20544(8) -0.1361(3) 0.13363(15) 0.0626(8) Uani 1.000 C C10 0.17115(8) -0.0238(3) 0.17662(14) 0.0599(7) Uani 1.000 C C11 0.12231(7) -0.0226(2) 0.14648(11) 0.0449(6) Uani 1.000 H H4 0.0890(7) -0.441(2) 0.1366(12) 0.053(5) Uiso 1.000 H H5 0.0450(6) -0.684(2) 0.2061(12) 0.053(5) Uiso 1.000 H H7 0.1322(6) -0.324(2) -0.0219(12) 0.048(5) Uiso 1.000 H H8 0.2160(7) -0.324(3) 0.0268(14) 0.078(6) Uiso 1.000 H H9 0.2404(9) -0.138(3) 0.1536(15) 0.083(7) Uiso 1.000 H H10 0.1794(8) 0.057(3) 0.2296(16) 0.085(7) Uiso 1.000 H H11 0.0964(7) 0.050(2) 0.1780(13) 0.054(5) Uiso 1.000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 C1 C2 . 3_555 122.02(15) no C1 C1 C2 5_555 . 118.99(8) no C1 C1 C2 5_555 3_555 118.99(8) no C1 C2 C3 . . 120.39(13) no C1 C2 C6 . . 123.20(12) no C3 C2 C6 . . 115.98(12) no C2 C3 C4 . . 121.75(13) no C2 C3 C3 . 7_555 120.22(12) no C3 C3 C4 7_555 . 117.89(13) no C3 C4 C5 . . 121.65(16) no C4 C5 C5 . 7_555 120.45(15) no C2 C6 C7 . . 122.53(13) no C2 C6 C11 . . 119.32(14) no C7 C6 C11 . . 117.77(15) no C6 C7 C8 . . 120.95(16) no C7 C8 C9 . . 120.35(18) no C8 C9 C10 . . 119.8(2) no C9 C10 C11 . . 119.90(19) no C6 C11 C10 . . 121.18(16) no C3 C4 H4 . . 118.1(9) no C5 C4 H4 . . 120.2(9) no C4 C5 H5 . . 118.7(9) no C5 C5 H5 7_555 . 120.8(9) no C6 C7 H7 . . 118.7(9) no C8 C7 H7 . . 120.3(9) no C7 C8 H8 . . 119.0(11) no C9 C8 H8 . . 120.6(11) no C8 C9 H9 . . 119.0(13) no C10 C9 H9 . . 121.1(13) no C9 C10 H10 . . 123.1(13) no C11 C10 H10 . . 117.0(13) no C6 C11 H11 . . 116.7(11) no C10 C11 H11 . . 122.1(11) no 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 C1 C2 . 1.4317(16) no C1 C2 3_555 1.4317(16) no C1 C1 5_555 1.462(3) no C2 C3 . 1.4069(19) no C2 C6 . 1.500(2) no C3 C4 . 1.444(2) no C3 C3 7_555 1.4336(19) no C4 C5 . 1.359(2) no C5 C5 7_555 1.407(3) no C6 C7 . 1.393(2) no C6 C11 . 1.394(2) no C7 C8 . 1.382(3) no C8 C9 . 1.378(3) no C9 C10 . 1.377(3) no C10 C11 . 1.386(3) no C4 H4 . 1.006(19) no C5 H5 . 0.992(16) no C7 H7 . 0.985(16) no C8 H8 . 1.00(2) no C9 H9 . 0.99(2) no C10 H10 . 0.99(2) no C11 H11 . 0.984(18) no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_2 _geom_contact_publ_flag C2 C11 3.594(2) 3_555 no C4 C7 3.208(2) . no C4 C11 3.589(2) . no C6 C11 3.385(2) 3_555 no C6 C6 2.841(2) 3_555 no C6 C7 3.243(2) 3_555 no C7 C4 3.208(2) . no C7 C6 3.243(2) 3_555 no C7 C11 3.245(2) 3_555 no C11 C7 3.245(2) 3_555 no C11 C6 3.385(2) 3_555 no C11 C2 3.594(2) 3_555 no C11 C4 3.589(2) . no C4 H11 2.978(19) 6_545 no C4 H5 2.985(16) 6_555 no C5 H11 3.010(19) 6_545 no C6 H4 2.457(15) . no C7 H4 2.540(17) . no C8 H8 2.849(19) 13_545 no C9 H10 3.05(2) 6_545 no C11 H7 3.092(16) 3_555 no H4 C6 2.457(15) . no H4 C7 2.540(17) . no H5 H11 2.40(2) 1_545 no H5 C4 2.985(16) 6_545 no H7 C11 3.092(16) 3_555 no H8 C8 2.849(19) 13_545 no H8 H8 2.26(3) 13_545 no H10 C9 3.05(2) 6_555 no H11 H5 2.40(2) 1_565 no H11 C4 2.978(19) 6_555 no H11 C5 3.010(19) 6_555 no 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_site_symmetry_1 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C2 C1 C2 C3 3_555 . . -172.82(11) no C2 C1 C2 C6 3_555 . . 14.93(15) no C1 C1 C2 C3 5_555 . . 7.18(14) no C1 C1 C2 C6 5_555 . . -165.07(9) no C1 C2 C3 C4 . . . 177.10(11) no C1 C2 C3 C3 . . 7_555 -7.27(18) no C6 C2 C3 C4 . . . -10.11(19) no C6 C2 C3 C3 . . 7_555 165.52(12) no C1 C2 C6 C7 . . . -109.65(15) no C1 C2 C6 C11 . . . 77.62(17) no C3 C2 C6 C7 . . . 77.78(18) no C3 C2 C6 C11 . . . -94.94(16) no C2 C3 C4 C5 . . . 176.86(14) no C3 C3 C4 C5 7_555 . . 1.1(2) no C2 C3 C3 C2 . 7_555 7_555 0.00(19) no C2 C3 C3 C4 . 7_555 7_555 -175.80(12) no C4 C3 C3 C2 . 7_555 7_555 175.80(12) no C4 C3 C3 C4 . 7_555 7_555 0.00(19) no C3 C4 C5 C5 . . 7_555 -1.2(2) no C4 C5 C5 C4 . 7_555 7_555 0.0(2) no C2 C6 C7 C8 . . . -172.64(16) no C11 C6 C7 C8 . . . 0.2(2) no C2 C6 C11 C10 . . . 173.26(15) no C7 C6 C11 C10 . . . 0.2(2) no C6 C7 C8 C9 . . . -0.4(3) no C7 C8 C9 C10 . . . 0.2(3) no C8 C9 C10 C11 . . . 0.2(3) no C9 C10 C11 C6 . . . -0.4(3) no