#------------------------------------------------------------------------------ #$Date: 2011-01-02 21:00:31 +0100 (Sun, 02 Jan 2011) $ #$Revision: 5310 $ #$URL: svn://www.crystallography.net/cod/cif/2/2100413.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_2100413 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 Vapour 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 ' ?' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-C 2bc 2' _symmetry_space_group_name_H-M 'C m c a' _atom_sites_solution_hydrogens difmap _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 26.828(4) _cell_length_b 7.1810(10) _cell_length_c 14.306(2) _cell_measurement_reflns_used 4431 _cell_measurement_temperature 175.0(10) _cell_measurement_theta_max 27.46 _cell_measurement_theta_min 2.85 _cell_volume 2756.1(7) _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 175.0(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 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 10119 _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 3.23 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.073 _exptl_absorpt_correction_T_max 0.9978 _exptl_absorpt_correction_T_min 0.9612 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS, Sheldrick, Bruker, 2000))' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.284 _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 0.223 _refine_diff_density_min -0.196 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 124 _refine_ls_number_reflns 1434 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.057 _refine_ls_R_factor_all 0.0580 _refine_ls_R_factor_gt 0.0388 _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^)+(0.0492P)^2^+1.0967P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0910 _refine_ls_wR_factor_ref 0.1002 _reflns_number_gt 1085 _reflns_number_total 1434 _reflns_threshold_expression I>2\s(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. '_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 ; _cod_database_code 2100413 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 0.0248(10) 0.0196(9) 0.0148(8) 0.0000 0.0000 -0.0019(7) C2 0.0262(8) 0.0201(6) 0.0154(6) 0.0019(5) 0.0016(5) -0.0015(5) C3 0.0285(7) 0.0203(6) 0.0130(6) 0.0015(5) 0.0006(5) -0.0019(5) C4 0.0307(9) 0.0243(7) 0.0204(7) 0.0055(6) 0.0017(6) 0.0012(5) C5 0.0409(9) 0.0214(7) 0.0223(7) 0.0054(6) 0.0001(6) 0.0039(5) C6 0.0236(8) 0.0227(6) 0.0186(6) 0.0009(5) -0.0003(5) 0.0055(5) C7 0.0295(8) 0.0250(7) 0.0288(7) 0.0013(6) 0.0037(6) 0.0013(6) C8 0.0271(8) 0.0364(8) 0.0424(9) 0.0040(7) 0.0070(7) 0.0064(7) C9 0.0230(9) 0.0513(10) 0.0420(9) -0.0006(7) -0.0062(7) 0.0133(8) C10 0.0374(10) 0.0486(10) 0.0278(8) -0.0049(8) -0.0092(7) 0.0002(7) C11 0.0320(9) 0.0340(8) 0.0211(7) 0.0030(7) 0.0000(6) -0.0012(6) 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 0.02718(7) 0.00000 0.00000 0.0197(5) Uani 1.000 C C2 0.05303(5) -0.14399(17) 0.04909(8) 0.0206(4) Uani 1.000 C C3 0.02673(5) -0.29472(17) 0.08762(8) 0.0206(4) Uani 1.000 C C4 0.05186(6) -0.44615(18) 0.13392(9) 0.0251(4) Uani 1.000 C C5 0.02622(6) -0.58729(19) 0.17496(9) 0.0282(4) Uani 1.000 C C6 0.10736(5) -0.13391(18) 0.07267(9) 0.0216(4) Uani 1.000 C C7 0.14277(5) -0.24639(19) 0.02938(10) 0.0278(4) Uani 1.000 C C8 0.19159(6) -0.2491(2) 0.06005(11) 0.0353(5) Uani 1.000 C C9 0.20620(6) -0.1376(2) 0.13407(11) 0.0388(5) Uani 1.000 C C10 0.17173(6) -0.0245(2) 0.17770(11) 0.0379(5) Uani 1.000 C C11 0.12281(6) -0.0235(2) 0.14762(9) 0.0290(5) Uani 1.000 H H4 0.0886(6) -0.447(2) 0.1352(10) 0.031(4) Uiso 1.000 H H5 0.0443(5) -0.686(2) 0.2063(10) 0.034(4) Uiso 1.000 H H7 0.1330(6) -0.324(2) -0.0237(11) 0.035(4) Uiso 1.000 H H8 0.2168(6) -0.328(2) 0.0272(11) 0.048(5) Uiso 1.000 H H9 0.2406(7) -0.139(2) 0.1527(11) 0.043(5) Uiso 1.000 H H10 0.1809(6) 0.056(2) 0.2295(13) 0.054(5) Uiso 1.000 H H11 0.0975(5) 0.053(2) 0.1780(10) 0.027(4) 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_555 121.95(15) no C1 C1 C2 5_555 . 119.02(8) no C1 C1 C2 5_555 3_555 119.02(8) no C1 C2 C3 . . 120.43(13) no C1 C2 C6 . . 123.22(12) no C3 C2 C6 . . 115.95(11) no C2 C3 C4 . . 121.80(12) no C2 C3 C3 . 7_555 120.15(11) no C3 C3 C4 7_555 . 117.90(12) no C3 C4 C5 . . 121.66(14) no C4 C5 C5 . 7_555 120.42(13) no C2 C6 C7 . . 122.40(12) no C2 C6 C11 . . 119.29(12) no C7 C6 C11 . . 117.93(13) no C6 C7 C8 . . 120.92(13) no C7 C8 C9 . . 120.22(14) no C8 C9 C10 . . 119.78(15) no C9 C10 C11 . . 119.93(14) no C6 C11 C10 . . 121.22(14) no C3 C4 H4 . . 118.8(8) no C5 C4 H4 . . 119.6(8) no C4 C5 H5 . . 119.5(8) no C5 C5 H5 7_555 . 120.0(8) no C6 C7 H7 . . 119.6(9) no C8 C7 H7 . . 119.5(9) no C7 C8 H8 . . 120.0(9) no C9 C8 H8 . . 119.7(9) no C8 C9 H9 . . 118.6(9) no C10 C9 H9 . . 121.6(9) no C9 C10 H10 . . 121.7(9) no C11 C10 H10 . . 118.4(9) no C6 C11 H11 . . 117.1(8) no C10 C11 H11 . . 121.7(8) 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 . 1.4294(15) no C1 C2 3_555 1.4294(15) no C1 C1 5_555 1.458(3) no C2 C3 . 1.4047(18) no C2 C6 . 1.4978(19) no C3 C4 . 1.4407(19) no C3 C3 7_555 1.4342(19) no C4 C5 . 1.358(2) no C5 C5 7_555 1.407(2) no C6 C7 . 1.3923(19) no C6 C11 . 1.3965(19) no C7 C8 . 1.381(2) no C8 C9 . 1.384(2) no C9 C10 . 1.380(2) no C10 C11 . 1.381(2) no C4 H4 . 0.986(16) no C5 H5 . 0.969(14) no C7 H7 . 0.978(15) no C8 H8 . 1.000(16) no C9 H9 . 0.961(19) no C10 H10 . 0.972(17) no C11 H11 . 0.976(14) 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 3.5876(19) 3_555 no C4 C7 3.200(2) . no C4 C11 3.588(2) . no C6 C6 2.8323(19) 3_555 no C6 C11 3.3736(19) 3_555 no C6 C7 3.239(2) 3_555 no C7 C4 3.200(2) . no C7 C6 3.239(2) 3_555 no C7 C11 3.233(2) 3_555 no C8 C8 3.574(2) 13_545 no C11 C2 3.5876(19) 3_555 no C11 C4 3.588(2) . no C11 C6 3.3736(19) 3_555 no C11 C7 3.233(2) 3_555 no C3 H5 3.086(14) 6_555 no C4 H5 2.959(14) 6_555 no C4 H11 2.956(14) 6_545 no C5 H11 3.016(14) 6_545 no C6 H4 2.472(14) . no C7 H4 2.545(15) . no C7 H7 3.097(14) 3_545 no C8 H8 2.812(16) 13_545 no C9 H10 3.019(16) 6_545 no C11 H7 3.073(15) 3_555 no H4 C6 2.472(14) . no H4 C7 2.545(15) . no H4 H7 2.58(2) 3_545 no H5 H11 2.39(2) 1_545 no H5 C3 3.086(14) 6_545 no H5 C4 2.959(14) 6_545 no H7 C7 3.097(14) 3_545 no H7 C11 3.073(15) 3_555 no H7 H4 2.58(2) 3_545 no H8 H8 2.59(2) 3_545 no H8 C8 2.812(16) 13_545 no H8 H8 2.24(2) 13_545 no H10 C9 3.019(16) 6_555 no H11 H5 2.39(2) 1_565 no H11 C4 2.956(14) 6_555 no H11 C5 3.016(14) 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 . . -172.78(10) no C2 C1 C2 C6 3_555 . . 14.78(14) no C1 C1 C2 C3 5_555 . . 7.22(12) no C1 C1 C2 C6 5_555 . . -165.22(8) no C1 C2 C3 C4 . . . 177.23(10) no C1 C2 C3 C3 . . 7_555 -7.30(16) no C6 C2 C3 C4 . . . -9.80(17) no C6 C2 C3 C3 . . 7_555 165.67(11) no C1 C2 C6 C7 . . . -109.75(14) no C1 C2 C6 C11 . . . 77.54(15) no C3 C2 C6 C7 . . . 77.51(16) no C3 C2 C6 C11 . . . -95.21(15) no C2 C3 C4 C5 . . . 176.85(12) no C3 C3 C4 C5 7_555 . . 1.28(18) no C2 C3 C3 C2 . 7_555 7_555 0.02(18) no C2 C3 C3 C4 . 7_555 7_555 -175.64(11) no C4 C3 C3 C2 . 7_555 7_555 175.64(11) no C4 C3 C3 C4 . 7_555 7_555 0.02(18) no C3 C4 C5 C5 . . 7_555 -1.3(2) no C4 C5 C5 C4 . 7_555 7_555 0.0(2) no C2 C6 C7 C8 . . . -172.50(13) no C11 C6 C7 C8 . . . 0.3(2) no C2 C6 C11 C10 . . . 173.46(13) no C7 C6 C11 C10 . . . 0.4(2) no C6 C7 C8 C9 . . . -0.8(2) no C7 C8 C9 C10 . . . 0.5(2) no C8 C9 C10 C11 . . . 0.2(2) no C9 C10 C11 C6 . . . -0.7(2) no