data_trux150 _audit_creation_date 07-06-27 _audit_creation_method CRYSTALS_ver_12.39 _oxford_structure_analysis_title 'Cadimer 150K 05-07' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 5.6073(5) _cell_length_b 18.2810(8) _cell_length_c 7.6481(6) _cell_angle_alpha 90 _cell_angle_beta 106.2288(15) _cell_angle_gamma 90 _cell_volume 752.74(10) _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall '?' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x+1/2,y+1/2,-z+1/2' 'x+1/2,-y+1/2,z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C9 H8 O2 # Dc = 1.31 Fooo = 312.00 Mu = 0.92 M = 148.16 # Found Formula = C9 H8 O2 # Dc = 1.31 FOOO = 312.00 Mu = 0.92 M = 148.16 _chemical_formula_sum 'C9 H8 O2' _chemical_formula_moiety 'C9 H8 O2' _chemical_compound_source ? _chemical_formula_weight 148.16 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 150 _exptl_crystal_description 'prism' _exptl_crystal_colour 'colourless' _exptl_crystal_size_min 0.12 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_max 0.41 _exptl_crystal_density_diffrn 1.307 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 312 _exptl_absorpt_coefficient_mu 0.092 # Sheldrick geometric approximatio 0.98 0.99 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SORTAV (Blessing)' _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 0.99 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' _computing_data_collection 'COLLECT (Nonius BV, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS 86 (Sheldrick, 1986)' _computing_structure_refinement 'CRYSTALS (Betteridge et al 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 9386 _reflns_number_total 2043 _diffrn_reflns_av_R_equivalents 0.051 # Number of reflections with Friedels Law is 2043 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 2094 _diffrn_reflns_theta_min 4.019 _diffrn_reflns_theta_max 29.490 _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 25.066 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _reflns_limit_h_min -7 _reflns_limit_h_max 7 _reflns_limit_k_min 0 _reflns_limit_k_max 25 _reflns_limit_l_min 0 _reflns_limit_l_max 10 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.23 _refine_diff_density_max 0.39 _refine_ls_number_reflns 1223 _refine_ls_number_restraints 0 _refine_ls_number_parameters 100 #_refine_ls_R_factor_ref 0.0470 _refine_ls_wR_factor_ref 0.0507 _refine_ls_goodness_of_fit_ref 1.1385 #_reflns_number_all 2042 _refine_ls_R_factor_all 0.0874 _refine_ls_wR_factor_all 0.0528 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 1223 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_gt 0.0507 _refine_ls_shift/su_max 0.003405 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration '.' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 10.7 -7.52 7.26 ; # Check this file using the IUCr facility at: # http://journals.iucr.org/services/cif/checking/checkfull.html # The content below is held in the file 'script/refcif.dat'. This is a text # file which you may edit to reflect local conditions. # Items which need looking at are represented by a '?'. # Items for which there are choices are prefixed with 'choose from'. _publ_contact_letter ; ; _publ_contact_author_name 'Volker Enkelmann' _publ_contact_author_address ; Max-Planck-Institute for Polymer Research P.O. Box 3148 D_55021 Mainz Germany ; _publ_contact_author_phone 'Int+6131 379133' _publ_contact_author_fax 'Int+6131 379100' _publ_contact_author_email 've@mpip-mainz.mpg.de' # Insert your own references if required - in alphabetical order _publ_section_references ; Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Blessing, SORTAV ( ) Nonius BV, COLLECT Software, (1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens O1 O 0.2721(2) 0.03856(8) 0.62091(17) 0.0272 1.0000 Uani . . . . . . O2 O -0.0587(2) 0.00647(8) 0.71392(18) 0.0277 1.0000 Uani . . . . . . H1 H -0.1403 -0.0041 0.5915 0.0500 1.0000 Uiso R . . . . . C4 C 0.6439(3) 0.11552(10) 1.1351(2) 0.0204 1.0000 Uani . . . . . . C1 C 0.1735(3) 0.02588(10) 0.7429(2) 0.0201 1.0000 Uani . . . . . . C3 C 0.5818(3) 0.05562(10) 0.9937(2) 0.0194 1.0000 Uani . . . . . . C9 C 0.5274(3) 0.12058(11) 1.2729(3) 0.0248 1.0000 Uani . . . . . . C2 C 0.3148(3) 0.02423(10) 0.9412(2) 0.0194 1.0000 Uani . . . . . . C5 C 0.8376(3) 0.16410(10) 1.1386(3) 0.0238 1.0000 Uani . . . . . . C6 C 0.9136(4) 0.21473(12) 1.2777(3) 0.0324 1.0000 Uani . . . . . . C7 C 0.7964(4) 0.21895(12) 1.4140(3) 0.0368 1.0000 Uani . . . . . . C8 C 0.6035(4) 0.17152(12) 1.4117(3) 0.0339 1.0000 Uani . . . . . . H31 H 0.6266 0.0699 0.8877 0.0265 1.0000 Uiso R . . . . . H91 H 0.3941 0.0884 1.2718 0.0331 1.0000 Uiso R . . . . . H21 H 0.2196 0.0438 1.0152 0.0262 1.0000 Uiso R . . . . . H51 H 0.9170 0.1625 1.0440 0.0326 1.0000 Uiso R . . . . . H61 H 1.0471 0.2470 1.2793 0.0426 1.0000 Uiso R . . . . . H71 H 0.8487 0.2540 1.5088 0.0464 1.0000 Uiso R . . . . . H81 H 0.5227 0.1739 1.5055 0.0444 1.0000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0211(6) 0.0404(8) 0.0186(6) 0.0013(6) 0.0029(5) -0.0079(6) O2 0.0141(6) 0.0467(9) 0.0192(6) 0.0003(6) -0.0003(5) -0.0048(6) C4 0.0164(8) 0.0219(8) 0.0215(8) -0.0015(6) 0.0029(6) -0.0017(7) C1 0.0164(8) 0.0237(8) 0.0186(8) -0.0018(7) 0.0021(6) 0.0008(7) C3 0.0156(8) 0.0264(9) 0.0166(7) -0.0001(7) 0.0050(6) -0.0029(7) C9 0.0213(8) 0.0280(9) 0.0263(9) -0.0062(8) 0.0086(7) -0.0073(8) C2 0.0138(7) 0.0269(9) 0.0170(7) -0.0029(7) 0.0038(6) -0.0002(7) C5 0.0188(8) 0.0261(9) 0.0259(9) 0.0010(7) 0.0054(7) -0.0042(7) C6 0.0282(10) 0.0271(10) 0.0397(12) -0.0041(8) 0.0058(9) -0.0121(8) C7 0.0381(11) 0.0317(10) 0.0377(12) -0.0136(9) 0.0059(9) -0.0101(9) C8 0.0351(11) 0.0389(12) 0.0312(10) -0.0140(9) 0.0148(9) -0.0099(9) _refine_ls_extinction_method 'None' _oxford_refine_ls_scale 6.87(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1 . C1 . 1.232(2) yes O2 . H1 . 0.940 no O2 . C1 . 1.307(2) yes C4 . C3 . 1.510(2) yes C4 . C9 . 1.389(3) yes C4 . C5 . 1.398(2) yes C1 . C2 . 1.503(2) yes C3 . C2 2_657 1.598(3) yes C3 . C2 . 1.548(2) yes C3 . H31 . 0.950 no C9 . C8 . 1.387(3) yes C9 . H91 . 0.950 no C2 . H21 . 0.950 no C5 . C6 . 1.385(3) yes C5 . H51 . 0.950 no C6 . C7 . 1.381(3) yes C6 . H61 . 0.950 no C7 . C8 . 1.383(3) yes C7 . H71 . 0.950 no C8 . H81 . 0.950 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag H1 . O2 . C1 . 114.111 no C3 . C4 . C9 . 121.91(16) yes C3 . C4 . C5 . 119.78(17) yes C9 . C4 . C5 . 118.10(17) yes O2 . C1 . O1 . 124.02(16) yes O2 . C1 . C2 . 112.62(15) yes O1 . C1 . C2 . 123.13(15) yes C4 . C3 . C2 2_657 116.65(14) yes C4 . C3 . C2 . 117.85(15) yes C2 2_657 C3 . C2 . 89.01(13) yes C4 . C3 . H31 . 110.463 no C2 2_657 C3 . H31 . 110.918 no C2 . C3 . H31 . 110.326 no C4 . C9 . C8 . 121.07(18) yes C4 . C9 . H91 . 119.169 no C8 . C9 . H91 . 119.761 no C3 . C2 . C1 . 116.96(15) yes C3 . C2 . C3 2_657 90.99(13) yes C1 . C2 . C3 2_657 112.07(15) yes C3 . C2 . H21 . 111.662 no C1 . C2 . H21 . 111.634 no C3 2_657 C2 . H21 . 111.977 no C4 . C5 . C6 . 120.65(18) yes C4 . C5 . H51 . 119.546 no C6 . C5 . H51 . 119.802 no C5 . C6 . C7 . 120.55(19) yes C5 . C6 . H61 . 119.766 no C7 . C6 . H61 . 119.682 no C6 . C7 . C8 . 119.40(19) yes C6 . C7 . H71 . 120.193 no C8 . C7 . H71 . 120.404 no C9 . C8 . C7 . 120.2(2) yes C9 . C8 . H81 . 119.973 no C7 . C8 . H81 . 119.818 no