Supplementary Material (ESI) for Organic & Biomolecular Chemistry This journal is (c) The Royal Society of Chemistry 2007 data_global #============================================================================== _journal_coden_Cambridge 177 # 0. AUDIT DETAILS _audit_creation_date '2006-06-07 15:58:08' _audit_creation_method ; PLATON option (version :: 40506) SHELXL97-2 & Manual Editing ; _audit_update_record ; ? ; #=============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name # Name of author for correspondence ; Drs. A. Meetsma ; _publ_contact_author_address # Address of author for correspondence ; Crystal Structure Center, Chemical Physics, Materials Science Center, University of Groningen, Nijenborgh 4, NL-9747 AG Groningen, The Netherlands. ; _publ_contact_author_email A.Meetsma@rug.nl _publ_contact_author_fax '+31 50 3634441' _publ_contact_author_phone '+31 50 3634368' _publ_requested_journal 'Chem. Comm.' # Publication choise FI, CI or EI for Inorganic # FM, CM or EM for Metal-organic # FO, CO or EO for Organic _publ_requested_category ? _publ_requested_coeditor_name ? _publ_contact_letter # Include date of submission ; Date of submission : 2007-08-06 11:58:08 Consider this CIF submission for deposition of the first X-ray structure of a manuscript to be submitted to : Chem. Comm (Our Compound_Identification_Code : Q1117) ; loop_ _publ_author_name B.Feringa A.Meetsma M.Pollard _publ_section_exptl_refinement ; The structure was solved by direct methods using the program SIR2004. The positional and anisotropic displacement parameters for the non-hydrogen atoms were refined. A subsequent difference Fourier synthesis resulted in the location of all the hydrogen atoms, which coordinates and isotropic displacement parameters were refined. ; # Insert blank lines between references _publ_section_references ; Allen, F.H. (2000). Acta Cryst. B58, 380-388. Bondi, A. (1964). J. Phys. Chem. 68, 441-451. Bruker, (2000). SMART, SAINTPLUS and XPREP. Software Reference Manual Bruker AXS Inc. Madison, Wisconsin, USA. Burla, M. C., Caliandro, R., Camalli, M., Carrozzini, B., Cascarano, G.L., De Caro, L., Giacovazzo, C., Polidori, G. & Spagna, R. (2005). SIR2004. An improved tool for crystal structure determination and refinement. J. Appl. Cryst. 38, 381-388. Hahn, T. (1983). Ed. International Tables for Crystallography, Volume A, Space-group symmetry, Kluwer Academic Publishers, Dordrecht, The Netherlands. Le Page, Y. (1987). J. Appl. Cryst. 20, 264-269. Le Page, Y. (1988). J. Appl. Cryst. 21, 983-984. Meetsma, A. (2005). Extended version of the program PLUTO. University of Groningen, The Netherlands. (unpublished). Sheldrick, G.M. (1997). SHELXL-97. Program for Crystal Structure Refinement. University of G\"ottingen, Germany. Sheldrick, G.M. (2001). SADABS. Version 2.03. Multi-Scan Absorption Correction Program. University of G\"ottingen, Germany. Spek, A.L. (1987). Acta Cryst. C43, 1233-1235. Spek, A.L. (1988). J. Appl. Cryst. 21, 578-579. Spek, A.L. (1990). Acta Cryst. A46, C-34. Spek, A.L. (2003). J. Appl. Cryst. 36, 7-13. Wilson, A.J.C. (1992). Ed. International Tables for Crystallography, Volume C, Kluwer Academic Publishers, Dordrecht, The Netherlands. ; _publ_section_figure_captions ; Fig. 1. Perspective PLUTO drawing of the molecule illustrating the configuration and the adopted numbering scheme. Fig. 2. Molecular packing viewed down unit cell axes. Fig. 3. Perspective ORTEP drawing of the title compound. Displacement ellipsoids for non-H are represented at the 50% probability level. The H-atoms are drawn with an arbitrary radius. ; #=============================================================================== data_1 _database_code_depnum_ccdc_archive 'CCDC 666199' # 5. CHEMICAL DATA _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H28' # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_structural ? _chemical_formula_sum 'C24 H28' _chemical_formula_iupac ? _chemical_formula_weight 316.48 _chemical_compound_source 'see text' 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' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 11.4202(7) _cell_length_b 13.2038(8) _cell_length_c 13.6607(8) _cell_angle_alpha 106.538(1) _cell_angle_beta 90.402(1) _cell_angle_gamma 115.040(1) _cell_volume 1769.71(19) _cell_formula_units_Z 4 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used 6549 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 29.55 _cell_special_details ; The final unit cell was obtained from the xyz centroids of 6549 reflections after integration using the SAINTPLUS software package (Bruker, 2000). Reduced cell calculations did not indicate any higher metric lattice symmetry and examination of the finalatomic coordinates of the structure did not yield extra symmetry elements (Spek, 1988; Le Page 1987, 1988) ; _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.57 _exptl_crystal_size_mid 0.52 _exptl_crystal_size_min 0.44 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.188 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 0.066 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_process_details '(SADABS, Sheldrick, Bruker, 2001))' _exptl_absorpt_correction_T_min 0.959 _exptl_absorpt_correction_T_max 0.9714 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ; _diffrn_ambient_temperature 100(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine focus sealed Siemens Mo tube ' _diffrn_radiation_monochromator 'parallel mounted graphite' _diffrn_radiation_detector ; CCD area-detector ; _diffrn_measurement_device_type ; Bruker Smart Apex; CCD area detector ; _diffrn_measurement_method '\f and \w scans' _diffrn_special_details ; Crystal into the cold nitrogen stream of the low-temparature unit (KRYOFLEX, (Bruker, 2000)). ; _diffrn_detector_area_resol_mean '4096x4096 / 62x62 (binned 512)' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 16214 _diffrn_reflns_av_R_equivalents 0.0203 _diffrn_reflns_av_sigmaI/netI 0.0365 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 28.28 _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.983 _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) ; # number of unique reflections _reflns_number_total 8438 _reflns_number_gt 6985 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART, Version 5.624, (Bruker, 2001)' _computing_cell_refinement 'SAINTPLUS, Version 6.02A, (Bruker, 2000)' _computing_data_reduction 'XPREP, Version 5.1/NT, (Bruker, 2000)' _computing_structure_solution ; SIR2004 (Burla et al., 2005) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; PLUTO (Meetsma, 2006) PLATON (Spek, 2003) ; _computing_publication_material 'PLATON (Spek, 2003)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0604P)^2^+0.7021P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _chemical_absolute_configuration ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 8438 _refine_ls_number_parameters 657 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0612 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1240 _refine_ls_wR_factor_gt 0.1176 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.353 _refine_diff_density_min -0.314 _refine_diff_density_rms 0.056 _vrn_publ_code_frame_time_sec 5.0 _vrn_publ_code_meas_time_hour 6.8 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags C11 C Uani 0.21758(12) 0.28717(11) 0.41419(10) 1.000 0.0135(3) . . C12 C Uani 0.08547(13) 0.27385(12) 0.44638(10) 1.000 0.0143(3) . . C13 C Uani -0.01071(13) 0.17175(12) 0.35228(10) 1.000 0.0152(4) . . C14 C Uani 0.06524(13) 0.18869(11) 0.26311(10) 1.000 0.0149(4) . . C15 C Uani 0.01551(13) 0.14088(12) 0.15831(11) 1.000 0.0170(4) . . C16 C Uani 0.10335(14) 0.17639(12) 0.08983(11) 1.000 0.0183(4) . . C17 C Uani 0.23303(14) 0.25834(13) 0.12604(11) 1.000 0.0182(4) . . C18 C Uani 0.28492(13) 0.30439(12) 0.23115(10) 1.000 0.0154(4) . . C19 C Uani 0.19931(13) 0.26419(11) 0.30001(10) 1.000 0.0141(3) . . C110 C Uani 0.06643(14) 0.38527(13) 0.45859(11) 1.000 0.0179(4) . . C111 C Uani -0.12661(15) 0.05567(13) 0.12031(12) 1.000 0.0213(4) . . C112 C Uani 0.42511(14) 0.39701(13) 0.26444(12) 1.000 0.0182(4) . . C113 C Uani 0.31358(12) 0.28509(11) 0.47139(10) 1.000 0.0133(3) . . C114 C Uani 0.42584(12) 0.26082(11) 0.42903(10) 1.000 0.0137(4) . . C115 C Uani 0.41536(13) 0.15965(12) 0.47056(11) 1.000 0.0147(4) . . C116 C Uani 0.36423(12) 0.18761(11) 0.57178(10) 1.000 0.0143(4) . . C117 C Uani 0.36881(13) 0.14537(12) 0.65364(11) 1.000 0.0169(4) . . C118 C Uani 0.32291(13) 0.18959(12) 0.74276(11) 1.000 0.0186(4) . . C119 C Uani 0.27902(13) 0.27450(13) 0.74982(11) 1.000 0.0182(4) . . C120 C Uani 0.27189(12) 0.31616(12) 0.66712(10) 1.000 0.0152(4) . . C121 C Uani 0.31097(12) 0.26756(11) 0.57516(10) 1.000 0.0133(3) . . C122 C Uani 0.55958(13) 0.36738(12) 0.47378(11) 1.000 0.0161(4) . . C123 C Uani 0.42461(15) 0.05886(13) 0.64839(13) 1.000 0.0221(4) . . C124 C Uani 0.23019(14) 0.41335(13) 0.68343(11) 1.000 0.0178(4) . . H12 H Uiso 0.0720(14) 0.2535(12) 0.5119(12) 1.000 0.010(3) . . H13 H Uiso -0.0301(16) 0.0936(15) 0.3606(13) 1.000 0.021(4) . . H13' H Uiso -0.0952(16) 0.1758(14) 0.3419(12) 1.000 0.017(4) . . H16 H Uiso 0.0713(16) 0.1431(15) 0.0133(14) 1.000 0.024(4) . . H17 H Uiso 0.2887(16) 0.2847(14) 0.0762(13) 1.000 0.022(4) . . H110 H Uiso 0.1352(18) 0.4558(16) 0.5098(14) 1.000 0.029(5) . . H110' H Uiso -0.0202(16) 0.3754(14) 0.4805(13) 1.000 0.020(4) . . H110" H Uiso 0.0719(16) 0.4036(14) 0.3914(13) 1.000 0.022(4) . . H111 H Uiso -0.1501(19) -0.0156(17) 0.1409(15) 1.000 0.035(5) . . H111' H Uiso -0.1473(19) 0.0273(17) 0.0433(16) 1.000 0.037(5) . . H111" H Uiso -0.184(2) 0.0901(17) 0.1499(15) 1.000 0.040(5) . . H112 H Uiso 0.4866(17) 0.3612(15) 0.2536(14) 1.000 0.028(5) . . H112' H Uiso 0.4398(16) 0.4455(14) 0.3394(14) 1.000 0.022(4) . . H112" H Uiso 0.4464(17) 0.4499(16) 0.2216(14) 1.000 0.029(5) . . H114 H Uiso 0.4143(14) 0.2361(13) 0.3526(12) 1.000 0.011(4) . . H115 H Uiso 0.3525(16) 0.0811(15) 0.4228(13) 1.000 0.021(4) . . H115' H Uiso 0.5011(16) 0.1584(14) 0.4806(13) 1.000 0.020(4) . . H118 H Uiso 0.3244(16) 0.1605(14) 0.8020(13) 1.000 0.023(4) . . H119 H Uiso 0.2518(17) 0.3067(15) 0.8145(14) 1.000 0.024(4) . . H122 H Uiso 0.5650(15) 0.4408(14) 0.4630(12) 1.000 0.019(4) . . H122' H Uiso 0.6310(16) 0.3516(14) 0.4412(13) 1.000 0.022(4) . . H122" H Uiso 0.5784(16) 0.3860(14) 0.5518(14) 1.000 0.021(4) . . H123 H Uiso 0.522(2) 0.0985(19) 0.6544(16) 1.000 0.046(6) . . H123' H Uiso 0.394(2) -0.0061(18) 0.5824(16) 1.000 0.039(5) . . H123" H Uiso 0.401(2) 0.0241(19) 0.7039(17) 1.000 0.051(6) . . H124 H Uiso 0.2656(16) 0.4606(15) 0.6362(13) 1.000 0.023(4) . . H124' H Uiso 0.2628(18) 0.4686(16) 0.7568(15) 1.000 0.032(5) . . H124" H Uiso 0.1333(18) 0.3822(16) 0.6733(14) 1.000 0.029(5) . . C21 C Uani 0.27671(12) 0.71101(11) 0.02841(10) 1.000 0.0125(3) . . C22 C Uani 0.41188(12) 0.72836(11) 0.06756(10) 1.000 0.0133(3) . . C23 C Uani 0.50202(13) 0.83108(12) 0.02870(11) 1.000 0.0149(4) . . C24 C Uani 0.42211(12) 0.80839(11) -0.07105(10) 1.000 0.0139(4) . . C25 C Uani 0.46702(13) 0.85215(11) -0.15229(11) 1.000 0.0152(4) . . C26 C Uani 0.37672(13) 0.80918(12) -0.24129(11) 1.000 0.0161(4) . . C27 C Uani 0.24892(13) 0.72550(12) -0.24872(11) 1.000 0.0162(4) . . C28 C Uani 0.20117(12) 0.68486(11) -0.16579(10) 1.000 0.0137(3) . . C29 C Uani 0.28970(12) 0.73081(11) -0.07452(10) 1.000 0.0131(3) . . C210 C Uani 0.43476(14) 0.61931(12) 0.01835(11) 1.000 0.0175(4) . . C211 C Uani 0.60766(14) 0.93923(12) -0.14534(12) 1.000 0.0182(4) . . C212 C Uani 0.06155(13) 0.59188(12) -0.18105(11) 1.000 0.0165(4) . . C213 C Uani 0.18287(12) 0.71341(11) 0.08761(10) 1.000 0.0124(3) . . C214 C Uani 0.06866(12) 0.73654(11) 0.05888(10) 1.000 0.0130(3) . . C215 C Uani 0.07975(13) 0.83751(11) 0.15635(11) 1.000 0.0148(4) . . C216 C Uani 0.13449(12) 0.81070(11) 0.24209(10) 1.000 0.0140(4) . . C217 C Uani 0.13154(12) 0.85282(11) 0.34742(11) 1.000 0.0159(4) . . C218 C Uani 0.17968(13) 0.80920(12) 0.41214(11) 1.000 0.0176(4) . . C219 C Uani 0.22541(13) 0.72588(12) 0.37205(11) 1.000 0.0170(4) . . C220 C Uani 0.23167(12) 0.68494(11) 0.26651(10) 1.000 0.0144(4) . . C221 C Uani 0.18887(12) 0.73195(11) 0.20119(10) 1.000 0.0128(3) . . C222 C Uani -0.06498(13) 0.63026(12) 0.04484(11) 1.000 0.0162(4) . . C223 C Uani 0.07618(14) 0.93946(13) 0.38895(12) 1.000 0.0208(4) . . C224 C Uani 0.27735(14) 0.59024(12) 0.22956(11) 1.000 0.0165(4) . . H22 H Uiso 0.4271(15) 0.7490(13) 0.1437(12) 1.000 0.014(4) . . H23 H Uiso 0.5201(15) 0.9104(14) 0.0804(12) 1.000 0.016(4) . . H23' H Uiso 0.5879(16) 0.8310(14) 0.0170(13) 1.000 0.022(4) . . H26 H Uiso 0.4043(17) 0.8363(15) -0.3004(13) 1.000 0.025(4) . . H27 H Uiso 0.1900(16) 0.6938(14) -0.3154(13) 1.000 0.021(4) . . H210 H Uiso 0.3698(18) 0.5474(16) 0.0318(14) 1.000 0.029(5) . . H210' H Uiso 0.5226(17) 0.6333(15) 0.0467(13) 1.000 0.023(4) . . H210" H Uiso 0.4325(17) 0.6033(15) -0.0594(14) 1.000 0.026(4) . . H211 H Uiso 0.6377(18) 1.0053(16) -0.0788(15) 1.000 0.030(5) . . H211' H Uiso 0.6164(18) 0.9752(16) -0.2018(14) 1.000 0.031(5) . . H211" H Uiso 0.6650(18) 0.9015(16) -0.1513(14) 1.000 0.029(5) . . H212 H Uiso 0.0003(17) 0.6280(15) -0.1703(14) 1.000 0.028(5) . . H212' H Uiso 0.0499(16) 0.5470(14) -0.1314(13) 1.000 0.021(4) . . H212" H Uiso 0.0367(16) 0.5365(15) -0.2543(14) 1.000 0.024(4) . . H214 H Uiso 0.0800(15) 0.7609(13) -0.0030(12) 1.000 0.013(4) . . H215 H Uiso -0.0064(16) 0.8379(14) 0.1676(12) 1.000 0.016(4) . . H215' H Uiso 0.1418(15) 0.9170(14) 0.1519(12) 1.000 0.016(4) . . H218 H Uiso 0.1796(16) 0.8374(15) 0.4875(14) 1.000 0.023(4) . . H219 H Uiso 0.2526(16) 0.6926(14) 0.4199(12) 1.000 0.018(4) . . H222 H Uiso -0.0823(16) 0.6148(14) 0.1134(14) 1.000 0.023(4) . . H222' H Uiso -0.0715(15) 0.5564(14) -0.0068(13) 1.000 0.018(4) . . H222" H Uiso -0.1357(17) 0.6472(15) 0.0203(13) 1.000 0.025(4) . . H223 H Uiso 0.1123(18) 1.0057(16) 0.3620(14) 1.000 0.029(5) . . H223' H Uiso 0.0987(19) 0.9743(17) 0.4665(16) 1.000 0.037(5) . . H223" H Uiso -0.0214(19) 0.9015(16) 0.3702(14) 1.000 0.033(5) . . H224 H Uiso 0.3773(17) 0.6241(15) 0.2370(13) 1.000 0.024(4) . . H224' H Uiso 0.2434(16) 0.5454(14) 0.1551(13) 1.000 0.020(4) . . H224" H Uiso 0.2501(18) 0.5372(16) 0.2721(14) 1.000 0.031(5) . . 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 C11 0.0136(6) 0.0132(6) 0.0150(6) 0.0053(5) 0.0039(5) 0.0066(5) C12 0.0136(6) 0.0176(6) 0.0139(6) 0.0056(5) 0.0022(5) 0.0085(5) C13 0.0134(6) 0.0175(6) 0.0159(7) 0.0058(5) 0.0014(5) 0.0076(5) C14 0.0168(6) 0.0153(6) 0.0159(7) 0.0055(5) 0.0026(5) 0.0099(5) C15 0.0200(7) 0.0164(6) 0.0174(7) 0.0038(5) 0.0002(5) 0.0118(5) C16 0.0252(7) 0.0233(7) 0.0124(7) 0.0036(5) 0.0013(5) 0.0177(6) C17 0.0238(7) 0.0245(7) 0.0152(7) 0.0089(5) 0.0072(5) 0.0171(6) C18 0.0180(7) 0.0170(6) 0.0167(7) 0.0065(5) 0.0042(5) 0.0120(5) C19 0.0165(6) 0.0157(6) 0.0136(6) 0.0048(5) 0.0021(5) 0.0103(5) C110 0.0169(7) 0.0204(7) 0.0196(7) 0.0060(6) 0.0023(5) 0.0114(6) C111 0.0206(7) 0.0208(7) 0.0198(8) 0.0011(6) -0.0022(6) 0.0102(6) C112 0.0180(7) 0.0207(7) 0.0201(7) 0.0100(6) 0.0066(5) 0.0101(6) C113 0.0137(6) 0.0123(6) 0.0136(6) 0.0036(5) 0.0028(5) 0.0059(5) C114 0.0136(6) 0.0152(6) 0.0137(7) 0.0045(5) 0.0023(5) 0.0078(5) C115 0.0139(6) 0.0152(6) 0.0162(7) 0.0045(5) 0.0014(5) 0.0079(5) C116 0.0102(6) 0.0138(6) 0.0159(7) 0.0043(5) 0.0001(5) 0.0030(5) C117 0.0117(6) 0.0164(6) 0.0203(7) 0.0072(5) -0.0026(5) 0.0034(5) C118 0.0137(6) 0.0234(7) 0.0174(7) 0.0114(6) -0.0002(5) 0.0040(5) C119 0.0125(6) 0.0245(7) 0.0148(7) 0.0060(5) 0.0022(5) 0.0059(5) C120 0.0099(6) 0.0173(6) 0.0162(7) 0.0046(5) 0.0008(5) 0.0044(5) C121 0.0092(6) 0.0143(6) 0.0144(6) 0.0050(5) 0.0005(5) 0.0032(5) C122 0.0132(6) 0.0171(6) 0.0180(7) 0.0048(5) 0.0034(5) 0.0071(5) C123 0.0228(8) 0.0193(7) 0.0268(8) 0.0104(6) -0.0012(6) 0.0098(6) C124 0.0169(7) 0.0212(7) 0.0159(7) 0.0040(5) 0.0039(5) 0.0102(5) C21 0.0111(6) 0.0118(6) 0.0138(6) 0.0032(5) -0.0004(5) 0.0050(5) C22 0.0103(6) 0.0168(6) 0.0127(6) 0.0037(5) 0.0008(5) 0.0066(5) C23 0.0107(6) 0.0169(6) 0.0159(7) 0.0044(5) 0.0019(5) 0.0056(5) C24 0.0140(6) 0.0140(6) 0.0148(7) 0.0029(5) 0.0023(5) 0.0083(5) C25 0.0156(6) 0.0139(6) 0.0185(7) 0.0045(5) 0.0053(5) 0.0092(5) C26 0.0200(7) 0.0176(6) 0.0164(7) 0.0080(5) 0.0064(5) 0.0118(5) C27 0.0186(7) 0.0175(6) 0.0150(7) 0.0038(5) 0.0013(5) 0.0113(5) C28 0.0143(6) 0.0138(6) 0.0147(6) 0.0039(5) 0.0024(5) 0.0081(5) C29 0.0143(6) 0.0140(6) 0.0140(6) 0.0048(5) 0.0037(5) 0.0088(5) C210 0.0161(7) 0.0194(7) 0.0204(7) 0.0057(5) 0.0035(5) 0.0114(5) C211 0.0154(7) 0.0176(7) 0.0230(8) 0.0084(6) 0.0062(5) 0.0072(5) C212 0.0143(6) 0.0178(6) 0.0156(7) 0.0041(5) 0.0001(5) 0.0062(5) C213 0.0113(6) 0.0111(5) 0.0145(6) 0.0044(5) 0.0002(5) 0.0046(5) C214 0.0117(6) 0.0150(6) 0.0145(6) 0.0062(5) 0.0029(5) 0.0070(5) C215 0.0120(6) 0.0140(6) 0.0192(7) 0.0058(5) 0.0034(5) 0.0062(5) C216 0.0092(6) 0.0126(6) 0.0178(7) 0.0045(5) 0.0026(5) 0.0030(5) C217 0.0109(6) 0.0149(6) 0.0176(7) 0.0024(5) 0.0027(5) 0.0036(5) C218 0.0129(6) 0.0211(7) 0.0135(7) 0.0028(5) 0.0025(5) 0.0045(5) C219 0.0123(6) 0.0214(7) 0.0160(7) 0.0076(5) 0.0008(5) 0.0054(5) C220 0.0100(6) 0.0155(6) 0.0159(7) 0.0051(5) 0.0012(5) 0.0040(5) C221 0.0088(6) 0.0135(6) 0.0136(6) 0.0035(5) 0.0013(4) 0.0032(5) C222 0.0114(6) 0.0167(6) 0.0196(7) 0.0059(5) 0.0013(5) 0.0054(5) C223 0.0169(7) 0.0197(7) 0.0221(8) 0.0006(6) 0.0037(6) 0.0087(6) C224 0.0168(7) 0.0186(6) 0.0176(7) 0.0073(5) 0.0021(5) 0.0100(5) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag C11 C12 1.526(2) . . no C11 C19 1.4970(18) . . no C11 C113 1.356(2) . . no C12 C13 1.555(2) . . no C12 C110 1.540(2) . . no C13 C14 1.514(2) . . no C14 C19 1.415(2) . . no C14 C15 1.3933(19) . . no C15 C16 1.402(2) . . no C15 C111 1.510(2) . . no C16 C17 1.392(2) . . no C17 C18 1.403(2) . . no C18 C19 1.407(2) . . no C18 C112 1.510(2) . . no C12 H12 1.000(16) . . no C113 C121 1.4985(19) . . no C13 H13' 1.00(2) . . no C113 C114 1.528(2) . . no C13 H13 1.000(19) . . no C114 C115 1.555(2) . . no C114 C122 1.538(2) . . no C115 C116 1.514(2) . . no C116 C117 1.394(2) . . no C16 H16 1.009(18) . . no C116 C121 1.415(2) . . no C117 C118 1.400(2) . . no C117 C123 1.512(2) . . no C17 H17 0.971(18) . . no C118 C119 1.390(2) . . no C119 C120 1.406(2) . . no C120 C124 1.510(2) . . no C120 C121 1.4073(19) . . no C110 H110' 1.00(2) . . no C110 H110" 1.010(17) . . no C110 H110 0.99(2) . . no C111 H111' 1.00(2) . . no C111 H111" 0.98(2) . . no C111 H111 0.99(2) . . no C112 H112' 1.010(18) . . no C112 H112" 0.99(2) . . no C112 H112 0.99(2) . . no C114 H114 0.991(16) . . no C115 H115' 1.00(2) . . no C115 H115 0.997(18) . . no C118 H118 0.993(17) . . no C119 H119 0.980(19) . . no C21 C29 1.4989(19) . . no C21 C213 1.353(2) . . no C21 C22 1.530(2) . . no C122 H122' 1.002(19) . . no C122 H122" 1.023(18) . . no C22 C210 1.537(2) . . no C122 H122 0.998(18) . . no C22 C23 1.555(2) . . no C123 H123' 0.99(2) . . no C123 H123" 0.98(2) . . no C123 H123 1.00(3) . . no C23 C24 1.516(2) . . no C124 H124 0.994(18) . . no C124 H124" 1.00(2) . . no C24 C25 1.397(2) . . no C24 C29 1.414(2) . . no C124 H124' 1.01(2) . . no C25 C26 1.399(2) . . no C25 C211 1.511(2) . . no C26 C27 1.389(2) . . no C27 C28 1.406(2) . . no C28 C29 1.4061(19) . . no C28 C212 1.512(2) . . no C22 H22 0.991(16) . . no C23 H23 1.016(17) . . no C23 H23' 1.00(2) . . no C26 H26 0.976(18) . . no C27 H27 0.997(18) . . no C213 C214 1.532(2) . . no C213 C221 1.4967(18) . . no C214 C215 1.553(2) . . no C214 C222 1.538(2) . . no C215 C216 1.517(2) . . no C216 C217 1.3935(19) . . no C216 C221 1.414(2) . . no C217 C218 1.402(2) . . no C217 C223 1.509(2) . . no C218 C219 1.389(2) . . no C219 C220 1.4023(19) . . no C220 C224 1.512(2) . . no C220 C221 1.409(2) . . no C210 H210' 0.99(2) . . no C210 H210" 1.020(18) . . no C210 H210 1.00(2) . . no C211 H211' 1.000(19) . . no C211 H211" 0.97(2) . . no C211 H211 1.00(2) . . no C212 H212' 0.996(17) . . no C212 H212" 1.010(18) . . no C212 H212 0.99(2) . . no C214 H214 0.978(16) . . no C215 H215' 1.007(18) . . no C215 H215 1.00(2) . . no C218 H218 0.990(18) . . no C219 H219 0.997(18) . . no C222 H222' 1.000(17) . . no C222 H222" 1.00(2) . . no C222 H222 1.018(18) . . no C223 H223' 1.01(2) . . no C223 H223" 1.00(2) . . no C223 H223 0.98(2) . . no C224 H224' 0.996(17) . . no C224 H224" 0.99(2) . . no C224 H224 1.03(2) . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C12 C11 C19 104.78(12) . . . no C12 C11 C113 125.24(12) . . . no C19 C11 C113 127.38(13) . . . no C11 C12 C13 101.69(11) . . . no C11 C12 C110 112.32(12) . . . no C13 C12 C110 109.46(12) . . . no C12 C13 C14 102.85(12) . . . no C13 C14 C15 127.08(14) . . . no C13 C14 C19 110.48(11) . . . no C15 C14 C19 122.43(13) . . . no C14 C15 C16 116.89(14) . . . no C14 C15 C111 121.56(14) . . . no C16 C15 C111 121.55(13) . . . no C15 C16 C17 121.00(13) . . . no C16 C17 C18 122.47(14) . . . no C17 C18 C19 116.90(14) . . . no C17 C18 C112 119.08(13) . . . no C19 C18 C112 123.95(12) . . . no C11 C19 C14 107.01(12) . . . no C11 C19 C18 133.06(13) . . . no C14 C19 C18 119.90(12) . . . no C13 C12 H12 112.0(9) . . . no C110 C12 H12 109.0(9) . . . no C11 C12 H12 112.3(10) . . . no C114 C113 C121 104.79(12) . . . no C14 C13 H13 110.5(10) . . . no C14 C13 H13' 111.7(9) . . . no C12 C13 H13' 112.7(9) . . . no C11 C113 C114 125.06(12) . . . no C11 C113 C121 127.61(13) . . . no C12 C13 H13 110.6(10) . . . no H13 C13 H13' 108.5(15) . . . no C113 C114 C122 112.14(11) . . . no C115 C114 C122 109.07(12) . . . no C113 C114 C115 101.69(11) . . . no C114 C115 C116 102.75(12) . . . no C17 C16 H16 119.7(11) . . . no C115 C116 C121 110.50(12) . . . no C117 C116 C121 122.50(13) . . . no C15 C16 H16 119.3(11) . . . no C115 C116 C117 126.99(13) . . . no C118 C117 C123 121.21(13) . . . no C116 C117 C118 116.89(14) . . . no C116 C117 C123 121.88(13) . . . no C16 C17 H17 118.2(11) . . . no C18 C17 H17 119.4(11) . . . no C117 C118 C119 121.17(14) . . . no C118 C119 C120 122.35(14) . . . no C119 C120 C121 116.97(14) . . . no C121 C120 C124 124.16(13) . . . no C119 C120 C124 118.80(12) . . . no C113 C121 C120 133.01(13) . . . no C116 C121 C120 119.84(12) . . . no C113 C121 C116 107.11(12) . . . no C12 C110 H110' 111.3(10) . . . no C12 C110 H110" 110.5(10) . . . no C12 C110 H110 112.2(12) . . . no H110' C110 H110" 108.7(15) . . . no H110' C110 H110 108.0(16) . . . no H110" C110 H110 105.9(15) . . . no C15 C111 H111' 112.4(13) . . . no C15 C111 H111" 111.6(13) . . . no C15 C111 H111 110.7(13) . . . no H111' C111 H111" 109.4(18) . . . no H111' C111 H111 105.9(17) . . . no H111" C111 H111 106.5(18) . . . no C18 C112 H112' 110.9(11) . . . no C18 C112 H112" 109.4(12) . . . no C18 C112 H112 111.5(11) . . . no H112' C112 H112" 109.0(15) . . . no H112' C112 H112 109.5(15) . . . no H112" C112 H112 106.5(16) . . . no C113 C114 H114 111.7(10) . . . no C115 C114 H114 112.0(10) . . . no C122 C114 H114 110.1(10) . . . no C114 C115 H115' 112.3(10) . . . no C114 C115 H115 111.4(11) . . . no C116 C115 H115' 111.9(10) . . . no C116 C115 H115 110.5(11) . . . no H115' C115 H115 108.1(15) . . . no C117 C118 H118 118.5(11) . . . no C119 C118 H118 120.3(11) . . . no C118 C119 H119 119.2(11) . . . no C120 C119 H119 118.4(11) . . . no C22 C21 C29 104.70(12) . . . no C22 C21 C213 125.22(12) . . . no C29 C21 C213 127.35(13) . . . no C114 C122 H122' 110.7(10) . . . no C114 C122 H122" 110.7(10) . . . no C114 C122 H122 112.9(10) . . . no C21 C22 C23 101.15(11) . . . no C21 C22 C210 112.47(12) . . . no C23 C22 C210 109.61(12) . . . no H122' C122 H122 107.5(15) . . . no H122" C122 H122 106.2(14) . . . no H122' C122 H122" 108.6(15) . . . no H123' C123 H123" 107.8(19) . . . no H123' C123 H123 105.8(19) . . . no C117 C123 H123' 112.8(14) . . . no C117 C123 H123" 110.8(15) . . . no C117 C123 H123 110.9(14) . . . no C22 C23 C24 102.73(12) . . . no H123" C123 H123 108.5(19) . . . no C120 C124 H124' 109.8(12) . . . no C120 C124 H124" 112.0(12) . . . no C120 C124 H124 112.1(11) . . . no H124' C124 H124" 106.7(17) . . . no H124' C124 H124 107.9(15) . . . no H124" C124 H124 108.1(16) . . . no C23 C24 C25 127.42(13) . . . no C23 C24 C29 110.43(12) . . . no C25 C24 C29 122.13(13) . . . no C24 C25 C26 116.93(14) . . . no C24 C25 C211 121.42(13) . . . no C26 C25 C211 121.63(13) . . . no C25 C26 C27 121.33(13) . . . no C26 C27 C28 122.15(13) . . . no C27 C28 C29 116.98(13) . . . no C27 C28 C212 118.76(12) . . . no C29 C28 C212 124.20(12) . . . no C21 C29 C24 106.88(12) . . . no C21 C29 C28 132.94(13) . . . no C24 C29 C28 120.12(12) . . . no C23 C22 H22 112.5(10) . . . no C210 C22 H22 108.9(10) . . . no C21 C22 H22 112.1(11) . . . no C22 C23 H23 110.9(10) . . . no C24 C23 H23 111.4(10) . . . no C24 C23 H23' 111.7(10) . . . no C22 C23 H23' 112.7(10) . . . no H23 C23 H23' 107.4(15) . . . no C25 C26 H26 119.7(12) . . . no C27 C26 H26 119.0(12) . . . no C26 C27 H27 118.2(11) . . . no C28 C27 H27 119.6(11) . . . no C214 C213 C221 104.92(11) . . . no C21 C213 C221 127.77(13) . . . no C21 C213 C214 124.84(12) . . . no C213 C214 C222 112.82(12) . . . no C215 C214 C222 108.66(12) . . . no C213 C214 C215 101.76(11) . . . no C214 C215 C216 102.65(11) . . . no C215 C216 C217 126.89(13) . . . no C215 C216 C221 110.69(11) . . . no C217 C216 C221 122.41(13) . . . no C216 C217 C223 121.12(13) . . . no C218 C217 C223 121.89(13) . . . no C216 C217 C218 116.97(13) . . . no C217 C218 C219 121.08(13) . . . no C218 C219 C220 122.41(14) . . . no C219 C220 C221 117.04(13) . . . no C221 C220 C224 124.37(12) . . . no C219 C220 C224 118.53(13) . . . no C213 C221 C220 133.04(13) . . . no C216 C221 C220 119.85(12) . . . no C213 C221 C216 107.07(12) . . . no C22 C210 H210' 110.1(11) . . . no C22 C210 H210" 110.4(11) . . . no C22 C210 H210 112.8(12) . . . no H210' C210 H210" 107.1(16) . . . no H210' C210 H210 107.2(17) . . . no H210" C210 H210 109.2(15) . . . no C25 C211 H211' 109.7(12) . . . no C25 C211 H211" 111.3(12) . . . no C25 C211 H211 111.3(12) . . . no H211' C211 H211" 108.9(17) . . . no H211' C211 H211 106.8(16) . . . no H211" C211 H211 108.6(17) . . . no C28 C212 H212' 111.0(11) . . . no C28 C212 H212" 109.6(11) . . . no C28 C212 H212 111.0(11) . . . no H212' C212 H212" 110.2(15) . . . no H212' C212 H212 107.8(16) . . . no H212" C212 H212 107.1(16) . . . no C213 C214 H214 110.5(11) . . . no C215 C214 H214 112.2(10) . . . no C222 C214 H214 110.7(10) . . . no C214 C215 H215' 111.4(9) . . . no C214 C215 H215 112.4(9) . . . no C216 C215 H215' 110.4(10) . . . no C216 C215 H215 111.9(9) . . . no H215' C215 H215 108.1(15) . . . no C217 C218 H218 119.3(11) . . . no C219 C218 H218 119.6(11) . . . no C218 C219 H219 118.7(10) . . . no C220 C219 H219 118.9(10) . . . no C214 C222 H222' 113.0(11) . . . no C214 C222 H222" 109.8(11) . . . no C214 C222 H222 109.9(11) . . . no H222' C222 H222" 107.4(15) . . . no H222' C222 H222 108.1(14) . . . no H222" C222 H222 108.6(15) . . . no C217 C223 H223' 111.1(13) . . . no C217 C223 H223" 111.6(12) . . . no C217 C223 H223 111.6(13) . . . no H223' C223 H223" 108.6(17) . . . no H223' C223 H223 106.2(16) . . . no H223" C223 H223 107.5(17) . . . no C220 C224 H224' 110.7(11) . . . no C220 C224 H224" 110.1(12) . . . no C220 C224 H224 112.5(11) . . . no H224' C224 H224" 111.1(15) . . . no H224' C224 H224 106.8(15) . . . no H224" C224 H224 105.5(16) . . . 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C19 C11 C12 C13 36.11(14) . . . . no C19 C11 C12 C110 -80.80(13) . . . . no C113 C11 C12 C13 -126.66(14) . . . . no C113 C11 C12 C110 116.42(15) . . . . no C12 C11 C19 C14 -27.39(15) . . . . no C12 C11 C19 C18 150.66(17) . . . . no C113 C11 C19 C14 134.89(15) . . . . no C113 C11 C19 C18 -47.1(3) . . . . no C12 C11 C113 C114 160.32(13) . . . . no C12 C11 C113 C121 1.2(2) . . . . no C19 C11 C113 C114 1.4(2) . . . . no C19 C11 C113 C121 -157.69(14) . . . . no C11 C12 C13 C14 -31.30(14) . . . . no C110 C12 C13 C14 87.67(14) . . . . no C12 C13 C14 C15 -162.96(15) . . . . no C12 C13 C14 C19 15.98(16) . . . . no C13 C14 C15 C16 175.14(14) . . . . no C13 C14 C15 C111 -4.3(2) . . . . no C19 C14 C15 C16 -3.7(2) . . . . no C19 C14 C15 C111 176.86(14) . . . . no C13 C14 C19 C11 6.75(16) . . . . no C13 C14 C19 C18 -171.61(13) . . . . no C15 C14 C19 C11 -174.25(14) . . . . no C15 C14 C19 C18 7.4(2) . . . . no C14 C15 C16 C17 -1.9(2) . . . . no C111 C15 C16 C17 177.59(15) . . . . no C15 C16 C17 C18 3.9(3) . . . . no C16 C17 C18 C19 -0.2(2) . . . . no C16 C17 C18 C112 -177.32(15) . . . . no C17 C18 C19 C11 176.93(16) . . . . no C17 C18 C19 C14 -5.2(2) . . . . no C112 C18 C19 C11 -6.1(3) . . . . no C112 C18 C19 C14 171.76(14) . . . . no C29 C21 C22 C23 37.18(13) . . . . no C29 C21 C22 C210 -79.67(14) . . . . no C213 C21 C22 C23 -125.17(15) . . . . no C213 C21 C22 C210 117.98(15) . . . . no C22 C21 C29 C24 -27.70(15) . . . . no C22 C21 C29 C28 149.26(16) . . . . no C213 C21 C29 C24 134.14(15) . . . . no C213 C21 C29 C28 -48.9(2) . . . . no C22 C21 C213 C214 158.88(13) . . . . no C22 C21 C213 C221 -0.6(2) . . . . no C29 C21 C213 C214 0.5(2) . . . . no C29 C21 C213 C221 -158.90(14) . . . . no C21 C22 C23 C24 -32.69(13) . . . . no C210 C22 C23 C24 86.24(14) . . . . no C22 C23 C24 C25 -160.92(14) . . . . no C22 C23 C24 C29 17.37(15) . . . . no C23 C24 C25 C26 173.64(14) . . . . no C23 C24 C25 C211 -4.7(2) . . . . no C29 C24 C25 C26 -4.5(2) . . . . no C29 C24 C25 C211 177.24(14) . . . . no C23 C24 C29 C21 6.08(16) . . . . no C23 C24 C29 C28 -171.35(13) . . . . no C25 C24 C29 C21 -175.53(13) . . . . no C25 C24 C29 C28 7.0(2) . . . . no C24 C25 C26 C27 -1.0(2) . . . . no C211 C25 C26 C27 177.34(14) . . . . no C25 C26 C27 C28 3.9(2) . . . . no C26 C27 C28 C29 -1.4(2) . . . . no C26 C27 C28 C212 -178.81(14) . . . . no C27 C28 C29 C21 179.45(15) . . . . no C27 C28 C29 C24 -3.9(2) . . . . no C212 C28 C29 C21 -3.3(3) . . . . no C212 C28 C29 C24 173.35(14) . . . . no C21 C213 C214 C215 -127.71(14) . . . . no C21 C213 C214 C222 116.04(15) . . . . no C221 C213 C214 C215 35.59(13) . . . . no C221 C213 C214 C222 -80.65(13) . . . . no C21 C213 C221 C216 136.57(15) . . . . no C21 C213 C221 C220 -45.8(2) . . . . no C214 C213 C221 C216 -26.08(15) . . . . no C214 C213 C221 C220 151.58(16) . . . . no C213 C214 C215 C216 -31.53(13) . . . . no C222 C214 C215 C216 87.71(14) . . . . no C214 C215 C216 C217 -161.38(14) . . . . no C214 C215 C216 C221 17.12(15) . . . . no C215 C216 C217 C218 175.35(14) . . . . no C215 C216 C217 C223 -3.4(2) . . . . no C221 C216 C217 C218 -3.0(2) . . . . no C221 C216 C217 C223 178.28(14) . . . . no C215 C216 C221 C213 5.27(16) . . . . no C215 C216 C221 C220 -172.75(13) . . . . no C217 C216 C221 C213 -176.15(13) . . . . no C217 C216 C221 C220 5.8(2) . . . . no C216 C217 C218 C219 -1.4(2) . . . . no C223 C217 C218 C219 177.37(15) . . . . no C217 C218 C219 C220 2.9(2) . . . . no C218 C219 C220 C221 -0.1(2) . . . . no C218 C219 C220 C224 -177.37(14) . . . . no C219 C220 C221 C213 178.50(15) . . . . no C219 C220 C221 C216 -4.1(2) . . . . no C224 C220 C221 C213 -4.4(3) . . . . no C224 C220 C221 C216 172.97(14) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag C11 C124 3.553(2) . . no C12 C120 3.447(2) . . no C12 C124 3.250(2) . . no C12 C218 3.548(2) . 2_566 no C16 C214 3.535(2) . 2_565 no C18 C114 3.440(2) . . no C21 C224 3.549(2) . . no C22 C220 3.452(2) . . no C22 C224 3.249(2) . . no C22 C118 3.546(2) . 2_666 no C28 C214 3.4529(19) . . no C110 C124 3.428(2) . . no C11 H112' 2.935(19) . . no C12 H124" 2.957(18) . . no C12 H218 3.03(2) . 2_566 no C112 C113 3.555(2) . . no C112 C114 3.256(2) . . no C112 C122 3.431(2) . . no C12 H124 3.005(18) . . no C112 C124 3.588(2) . 2_666 no C13 H111 3.09(2) . . no C13 H223 3.09(2) . 1_545 no C13 H218 2.922(19) . 2_566 no C13 H111" 3.02(2) . . no C113 C112 3.555(2) . . no C14 H110" 2.848(18) . . no C114 C18 3.440(2) . . no C114 C112 3.256(2) . . no C15 H212 3.09(2) . 2_565 no C16 H111' 3.03(2) . 2_555 no C16 H214 2.910(18) . 2_565 no C16 H222" 3.017(19) . 2_565 no C17 H222" 3.058(19) . 2_565 no C17 H211" 2.90(2) . 2_665 no C18 H211" 2.92(2) . 2_665 no C18 H114 2.774(17) . . no C118 C22 3.546(2) . 2_666 no C19 H114 2.753(17) . . no C19 H110" 2.837(19) . . no C120 C12 3.447(2) . . no C21 H224' 3.063(18) . . no C21 H212' 2.940(18) . . no C22 H118 3.016(19) . 2_666 no C22 H224 2.962(18) . . no C22 H224' 2.951(18) . . no C122 C112 3.431(2) . . no C23 H211 2.96(2) . . no C23 H118 2.982(18) . 2_666 no C124 C12 3.250(2) . . no C24 H211 3.05(2) . 2_675 no C24 H210" 2.809(19) . . no C124 C11 3.553(2) . . no C124 C110 3.428(2) . . no C124 C112 3.588(2) . 2_666 no C25 H112 3.03(2) . 2_665 no C25 H23 2.945(18) . 2_675 no C26 H114 3.018(17) . 2_665 no C26 H122' 2.917(17) . 2_665 no C26 H123" 3.04(2) . 1_564 no C27 H13' 3.041(19) . 2_565 no C27 H111" 2.82(2) . 2_565 no C27 H122' 3.089(18) . 2_665 no C28 H111" 3.01(2) . 2_565 no C28 H214 2.796(17) . . no C29 H214 2.732(18) . . no C29 H210" 2.84(2) . . no C210 C224 3.438(2) . . no C110 H124 2.947(18) . . no C110 H124" 3.041(19) . . no C111 H13' 2.929(16) . . no C211 C215 3.579(2) . 2_675 no C111 H16 3.051(19) . 2_555 no C212 C224 3.518(2) . 2_565 no C112 H114 2.686(16) . . no C212 C214 3.271(2) . . no C212 C213 3.558(2) . . no C112 H122 2.917(16) . . no C212 C222 3.415(2) . . no C213 C212 3.558(2) . . no C113 H112' 3.073(18) . . no C113 H124 2.977(18) . . no C114 H26 3.06(2) . 2_665 no C214 C28 3.4529(19) . . no C214 C16 3.535(2) . 2_565 no C114 H112' 2.974(18) . . no C214 C212 3.271(2) . . no C114 H112 3.006(19) . . no C215 C211 3.579(2) . 2_675 no C115 H123' 2.94(2) . . no C116 H223' 3.10(2) . 1_545 no C116 H122" 2.813(18) . . no C118 H210' 3.076(18) . 2_666 no C118 H22 2.911(18) . 2_666 no C218 C12 3.548(2) . 2_566 no C119 H223" 2.95(2) . 2_566 no C120 H12 2.780(16) . . no C220 C22 3.452(2) . . no C120 H223" 2.98(2) . 2_566 no C121 H122" 2.851(19) . . no C121 H12 2.771(17) . . no C122 H219 3.064(19) . 2_666 no C122 H124 3.090(19) . 2_666 no C122 H112 3.085(18) . . no C122 H112' 2.923(19) . . no C222 C212 3.415(2) . . no C122 H112' 3.002(18) . 2_666 no C123 H22 3.093(16) . 2_666 no C123 H115' 2.918(17) . . no C224 C21 3.549(2) . . no C124 H12 2.666(16) . . no C224 C210 3.438(2) . . no C124 H110 2.890(19) . . no C224 C212 3.518(2) . 2_565 no C224 C22 3.249(2) . . no C210 H224 3.051(17) . . no C210 H224' 2.917(18) . . no C211 H114 3.034(16) . 2_665 no C211 H23' 2.924(17) . . no C211 H23 2.885(18) . 2_675 no C211 H215' 2.702(18) . 2_675 no C212 H222' 2.877(17) . . no C212 H214 2.729(16) . . no C213 H224' 2.950(18) . . no C213 H222' 3.071(18) . 2_565 no C213 H212' 3.075(17) . . no C214 H212' 2.983(17) . . no C214 H16 3.01(2) . 2_565 no C214 H212 2.988(18) . . no C215 H223 2.949(19) . . no C215 H16 3.011(19) . 2_565 no C216 H222 2.800(18) . . no C217 H115 2.876(19) . 1_565 no C218 H123' 3.00(2) . 1_565 no C218 H12 2.922(17) . 2_566 no C219 H123 2.94(2) . 2_666 no C220 H123 2.94(2) . 2_666 no C220 H22 2.788(17) . . no C221 H222 2.874(19) . . no C221 H22 2.772(18) . . no C222 H212 3.032(19) . . no C222 H212' 2.970(18) . 2_565 no C222 H119 3.10(2) . 2_566 no C222 H224' 3.051(17) . 2_565 no C222 H212' 2.913(18) . . no C223 H115 2.86(2) . 1_565 no C223 H13 2.88(2) . 1_565 no C223 H12 3.088(15) . 2_566 no C223 H215 2.900(16) . . no C224 H22 2.662(17) . . no C224 H210 2.900(19) . . no H110' H13' 2.55(2) . . no H110" C14 2.848(18) . . no H110" C19 2.837(19) . . no H111' H16 2.42(3) . . no H111' C16 3.03(2) . 2_555 no H111" C13 3.02(2) . . no H111" H13' 2.55(3) . . no H111" C27 2.82(2) . 2_565 no H111" C28 3.01(2) . 2_565 no H112' C11 2.935(19) . . no H112' C113 3.073(18) . . no H112' C114 2.974(18) . . no H112' C122 2.923(19) . . no H112' C122 3.002(18) . 2_666 no H112' H122" 2.39(3) . 2_666 no H112' H122 2.24(3) . . no H112" H17 2.47(3) . . no H115' C123 2.918(17) . . no H115' H122' 2.57(3) . . no H122' C26 2.917(17) . 2_665 no H122' C27 3.089(18) . 2_665 no H122' H115' 2.57(3) . . no H122' H26 2.54(3) . 2_665 no H122" C121 2.851(19) . . no H122" H112' 2.39(3) . 2_666 no H122" C116 2.813(18) . . no H123' C218 3.00(2) . 1_545 no H123' H218 2.47(3) . 1_545 no H123' C115 2.94(2) . . no H123" H118 2.40(3) . . no H123" C26 3.04(2) . 1_546 no H123" H26 2.48(3) . 1_546 no H12 H124" 2.25(2) . . no H12 C120 2.780(16) . . no H12 C121 2.771(17) . . no H12 C124 2.666(16) . . no H12 C218 2.922(17) . 2_566 no H12 C223 3.088(15) . 2_566 no H124' H119 2.44(3) . . no H13 C223 2.88(2) . 1_545 no H13 H223 2.37(3) . 1_545 no H13' H218 2.55(2) . 2_566 no H13' C111 2.929(16) . . no H13' H110' 2.55(2) . . no H13' H111" 2.55(3) . . no H13' H27 2.49(3) . 2_565 no H13' C27 3.041(19) . 2_565 no H124" H12 2.25(2) . . no H124" C12 2.957(18) . . no H124" C110 3.041(19) . . no H210' H23' 2.55(3) . . no H210' C118 3.076(17) . 2_666 no H210" C24 2.809(19) . . no H210" C29 2.84(2) . . no H16 C215 3.011(19) . 2_565 no H16 H214 2.56(3) . 2_565 no H16 C214 3.01(2) . 2_565 no H16 C111 3.051(19) . 2_555 no H16 H111' 2.42(3) . . no H211' H26 2.42(3) . . no H211' H215' 2.49(3) . 2_675 no H17 H23' 2.59(3) . 2_665 no H17 H112" 2.47(3) . . no H211" H215' 2.48(3) . 2_675 no H211" C18 2.92(2) . 2_665 no H211" C17 2.90(2) . 2_665 no H212' C222 2.913(18) . . no H212' H222' 2.21(3) . . no H212' C222 2.970(18) . 2_565 no H212' H222 2.39(3) . 2_565 no H212' C214 2.983(17) . . no H212' C21 2.940(18) . . no H212' C213 3.075(17) . . no H212" H27 2.45(3) . . no H215' C211 2.702(18) . 2_675 no H215' H211' 2.49(3) . 2_675 no H215' H211" 2.48(3) . 2_675 no H222' H212' 2.21(3) . . no H222' C213 3.071(18) . 2_565 no H222' C212 2.877(17) . . no H222' H224' 2.43(3) . 2_565 no H22 C123 3.093(16) . 2_666 no H22 H118 2.57(3) . 2_666 no H22 C118 2.911(18) . 2_666 no H22 C220 2.788(17) . . no H22 C221 2.772(18) . . no H22 C224 2.662(17) . . no H22 H224 2.25(2) . . no H222" H215 2.55(2) . . no H222" C16 3.017(19) . 2_565 no H222" C17 3.058(19) . 2_565 no H23 C211 2.885(18) . 2_675 no H23 H211 2.49(3) . 2_675 no H23 C25 2.945(18) . 2_675 no H23' C211 2.924(17) . . no H23' H210' 2.55(3) . . no H23' H17 2.59(3) . 2_665 no H223' C116 3.10(2) . 1_565 no H223' H218 2.43(3) . . no H223" C119 2.95(2) . 2_566 no H223" C120 2.98(2) . 2_566 no H224' C210 2.917(18) . . no H224' C22 2.951(18) . . no H224' C21 3.063(18) . . no H224' C222 3.051(17) . 2_565 no H224' H222' 2.43(3) . 2_565 no H224' C213 2.950(18) . . no H224' H210 2.23(3) . . no H26 C114 3.06(2) . 2_665 no H26 H123" 2.48(3) . 1_564 no H26 H211' 2.42(3) . . no H26 H122' 2.54(3) . 2_665 no H224" H219 2.43(3) . . no H27 H212" 2.45(3) . . no H27 H13' 2.49(3) . 2_565 no H110 H124 2.24(3) . . no H110 C124 2.890(19) . . no H111 H118 2.43(3) . 2_556 no H111 C13 3.09(2) . . no H112 C114 3.006(19) . . no H112 C25 3.03(2) . 2_665 no H112 C122 3.085(18) . . no H112 H114 2.32(2) . . no H114 C18 2.774(17) . . no H114 H112 2.32(2) . . no H114 C19 2.753(17) . . no H114 C112 2.686(16) . . no H114 C211 3.034(16) . 2_665 no H114 C26 3.018(17) . 2_665 no H115 C223 2.86(2) . 1_545 no H115 H223 2.53(3) . 1_545 no H115 C217 2.876(19) . 1_545 no H118 C22 3.016(19) . 2_666 no H118 C23 2.982(18) . 2_666 no H118 H22 2.57(3) . 2_666 no H118 H123" 2.40(3) . . no H118 H111 2.43(3) . 2_556 no H119 C222 3.10(2) . 2_566 no H119 H124' 2.44(3) . . no H122 C112 2.917(16) . . no H122 H112' 2.24(3) . . no H122 H122 2.60(3) . 2_666 no H122 H124 2.49(3) . 2_666 no H123 C219 2.94(2) . 2_666 no H123 C220 2.94(2) . 2_666 no H124 C113 2.977(18) . . no H124 H122 2.49(3) . 2_666 no H124 H110 2.24(3) . . no H124 C122 3.090(19) . 2_666 no H124 C12 3.005(18) . . no H124 C110 2.947(18) . . no H210 C224 2.900(19) . . no H210 H224' 2.23(3) . . no H211 C23 2.96(2) . . no H211 C24 3.05(2) . 2_675 no H211 H23 2.49(3) . 2_675 no H212 C214 2.988(18) . . no H212 C222 3.032(19) . . no H212 H214 2.34(2) . . no H212 C15 3.09(2) . 2_565 no H214 C28 2.796(17) . . no H214 C29 2.732(18) . . no H214 C212 2.729(16) . . no H214 H212 2.34(2) . . no H214 C16 2.910(18) . 2_565 no H214 H16 2.56(3) . 2_565 no H215 C223 2.900(16) . . no H215 H222" 2.55(2) . . no H215 H222 2.56(2) . . no H218 H123' 2.47(3) . 1_565 no H218 H223' 2.43(3) . . no H218 C12 3.03(2) . 2_566 no H218 C13 2.922(19) . 2_566 no H218 H13' 2.55(2) . 2_566 no H219 H224" 2.43(3) . . no H219 C122 3.064(19) . 2_666 no H222 C216 2.800(18) . . no H222 C221 2.874(19) . . no H222 H215 2.56(2) . . no H222 H212' 2.39(3) . 2_565 no H223 C13 3.09(2) . 1_565 no H223 C215 2.949(19) . . no H223 H13 2.37(3) . 1_565 no H223 H115 2.53(3) . 1_565 no H224 C22 2.962(18) . . no H224 C210 3.051(17) . . no H224 H22 2.25(2) . . no # Loop Mechanism for Extra Tables(s) #loop_ #_publ_manuscript_incl_extra_item #'_geom_extra_tableA_col_1' #'_geom_extra_tableA_col_2' #'_geom_extra_tableA_col_3' #'_geom_extra_table_head_A' #'_geom_table_footnote_A' #'_geom_extra_tableB_col_1' #'_geom_extra_tableB_col_2' #'_geom_extra_tableB_col_3' #'_geom_extra_table_head_B' #'_geom_table_footnote_B' # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 # ? ? ? # #loop_ #_geom_extra_tableB_col_1 #_geom_extra_tableB_col_2 #_geom_extra_tableB_col_3 # ? ? ? # #_geom_table_footnote_A #; # ? #; # #_geom_table_footnote_B #; # ? #; # #_geom_table_footnote_A #; # ? #; # #_geom_table_footnote_B #; # ? #; #===END of Crystallographic Information File # Attachment 'q1118.cif' # CIF-file generated for C24H28 C2/c q1118 #============================================================================== data_2 _database_code_depnum_ccdc_archive 'CCDC 666200' # 5. CHEMICAL DATA _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H28' # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_structural ? _chemical_formula_sum 'C24 H28' _chemical_formula_iupac ? _chemical_formula_weight 316.48 _chemical_compound_source 'see text' 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' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 2/c' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,y,1/2-z 3 -x,-y,-z 4 x,-y,1/2+z 5 1/2+x,1/2+y,z 6 1/2-x,1/2+y,1/2-z 7 1/2-x,1/2-y,-z 8 1/2+x,1/2-y,1/2+z _cell_length_a 38.531(9) _cell_length_b 5.981(1) _cell_length_c 16.016(4) _cell_angle_alpha 90 _cell_angle_beta 93.416(4) _cell_angle_gamma 90 _cell_volume 3684.4(14) _cell_formula_units_Z 8 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used 7794 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 29.50 _cell_special_details ; The final unit cell was obtained from the xyz centroids of 7794 reflections after integration using the SAINTPLUS software package (Bruker, 2000). Reduced cell calculations did not indicate any higher metric lattice symmetry and examination of the finalatomic coordinates of the structure did not yield extra symmetry elements (Spek, 1988; Le Page 1987, 1988) ; _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.57 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.141 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 0.064 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_process_details '(SADABS, Sheldrick, Bruker, 2001))' _exptl_absorpt_correction_T_min 0.9616 _exptl_absorpt_correction_T_max 0.9905 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ; _diffrn_ambient_temperature 100(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine focus sealed Siemens Mo tube ' _diffrn_radiation_monochromator 'parallel mounted graphite' _diffrn_radiation_detector ; CCD area-detector ; _diffrn_measurement_device_type ; Bruker Smart Apex; CCD area detector ; _diffrn_measurement_method '\f and \w scans' _diffrn_special_details ; Crystal into the cold nitrogen stream of the low-temparature unit (KRYOFLEX, (Bruker, 2000)). ; _diffrn_detector_area_resol_mean '4096x4096 / 62x62 (binned 512)' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 12897 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0397 _diffrn_reflns_limit_h_min -47 _diffrn_reflns_limit_h_max 47 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 26.02 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _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) ; # number of unique reflections _reflns_number_total 3628 _reflns_number_gt 2970 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART, Version 5.624, (Bruker, 2001)' _computing_cell_refinement 'SAINTPLUS, Version 6.02A, (Bruker, 2000)' _computing_data_reduction 'XPREP, Version 5.1/NT, (Bruker, 2000)' _computing_structure_solution ; SIR2004 (Burla et al., 2005) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; PLUTO (Meetsma, 2006) PLATON (Spek, 2003) ; _computing_publication_material 'PLATON (Spek, 2003)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0674P)^2^+2.0136P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary direct _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _chemical_absolute_configuration ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3628 _refine_ls_number_parameters 329 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0566 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1211 _refine_ls_wR_factor_gt 0.1137 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.262 _refine_diff_density_min -0.195 _refine_diff_density_rms 0.044 _vrn_publ_code_frame_time_sec 20.0 _vrn_publ_code_meas_time_hour 16.3 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags C1 C Uani 0.13492(3) 0.3407(2) 0.27600(8) 1.000 0.0181(4) . . C2 C Uani 0.14417(4) 0.4351(2) 0.19124(9) 1.000 0.0212(4) . . C3 C Uani 0.16677(4) 0.6421(3) 0.21788(9) 1.000 0.0238(4) . . C4 C Uani 0.18404(3) 0.5695(2) 0.30060(9) 1.000 0.0209(4) . . C5 C Uani 0.21443(3) 0.6560(2) 0.34070(9) 1.000 0.0238(4) . . C6 C Uani 0.22648(4) 0.5491(3) 0.41433(10) 1.000 0.0273(5) . . C7 C Uani 0.20958(4) 0.3636(3) 0.44529(10) 1.000 0.0253(5) . . C8 C Uani 0.17888(3) 0.2759(2) 0.40577(9) 1.000 0.0208(4) . . C9 C Uani 0.16551(3) 0.3903(2) 0.33405(8) 1.000 0.0188(4) . . C10 C Uani 0.16489(4) 0.2676(3) 0.14094(10) 1.000 0.0250(5) . . C11 C Uani 0.23305(4) 0.8543(3) 0.30553(12) 1.000 0.0318(5) . . C12 C Uani 0.16388(4) 0.0615(3) 0.43790(10) 1.000 0.0250(4) . . C13 C Uani 0.10366(3) 0.2478(2) 0.28939(8) 1.000 0.0183(4) . . C14 C Uani 0.07845(3) 0.1606(2) 0.21889(9) 1.000 0.0210(4) . . C15 C Uani 0.06461(4) -0.0560(3) 0.25906(9) 1.000 0.0241(4) . . C16 C Uani 0.06441(3) 0.0064(2) 0.35043(9) 1.000 0.0202(4) . . C17 C Uani 0.04452(3) -0.0873(2) 0.41176(9) 1.000 0.0235(4) . . C18 C Uani 0.04742(4) 0.0138(3) 0.49057(10) 1.000 0.0266(5) . . C19 C Uani 0.06812(4) 0.2018(3) 0.50651(9) 1.000 0.0248(5) . . C20 C Uani 0.08845(3) 0.2965(2) 0.44562(8) 1.000 0.0202(4) . . C21 C Uani 0.08716(3) 0.1878(2) 0.36749(8) 1.000 0.0187(4) . . C22 C Uani 0.04851(4) 0.3246(3) 0.19736(10) 1.000 0.0251(5) . . C23 C Uani 0.02151(4) -0.2886(3) 0.39414(12) 1.000 0.0294(5) . . C24 C Uani 0.10786(4) 0.5118(3) 0.46371(9) 1.000 0.0229(4) . . H2 H Uiso 0.1236(4) 0.482(3) 0.1564(9) 1.000 0.021(4) . . H3 H Uiso 0.1833(4) 0.683(3) 0.1745(10) 1.000 0.031(4) . . H3' H Uiso 0.1523(4) 0.783(3) 0.2269(10) 1.000 0.034(5) . . H6 H Uiso 0.2478(5) 0.606(3) 0.4437(11) 1.000 0.035(5) . . H7 H Uiso 0.2189(4) 0.283(3) 0.4969(10) 1.000 0.025(4) . . H10 H Uiso 0.1846(5) 0.212(3) 0.1762(11) 1.000 0.032(4) . . H10' H Uiso 0.1730(4) 0.339(3) 0.0879(11) 1.000 0.029(4) . . H10" H Uiso 0.1507(4) 0.130(3) 0.1242(10) 1.000 0.029(4) . . H11 H Uiso 0.2412(5) 0.821(3) 0.2478(13) 1.000 0.048(5) . . H11' H Uiso 0.2530(6) 0.903(4) 0.3459(13) 1.000 0.061(6) . . H11" H Uiso 0.2175(5) 0.987(3) 0.2975(11) 1.000 0.039(5) . . H12 H Uiso 0.1460(4) 0.090(3) 0.4798(11) 1.000 0.032(4) . . H12' H Uiso 0.1830(5) -0.030(3) 0.4680(10) 1.000 0.033(4) . . H12" H Uiso 0.1527(5) -0.030(3) 0.3916(11) 1.000 0.036(5) . . H14 H Uiso 0.0904(4) 0.129(3) 0.1676(10) 1.000 0.020(4) . . H15 H Uiso 0.0408(5) -0.102(3) 0.2317(11) 1.000 0.035(5) . . H15' H Uiso 0.0809(4) -0.190(3) 0.2513(10) 1.000 0.030(4) . . H18 H Uiso 0.0340(5) -0.050(3) 0.5357(11) 1.000 0.035(5) . . H19 H Uiso 0.0684(4) 0.275(3) 0.5626(11) 1.000 0.030(4) . . H22 H Uiso 0.0364(4) 0.362(3) 0.2486(10) 1.000 0.026(4) . . H22' H Uiso 0.0322(4) 0.259(3) 0.1553(11) 1.000 0.032(4) . . H22" H Uiso 0.0571(4) 0.471(3) 0.1718(11) 1.000 0.035(5) . . H23 H Uiso 0.0352(5) -0.426(3) 0.3845(11) 1.000 0.040(5) . . H23' H Uiso 0.0046(6) -0.271(4) 0.3444(15) 1.000 0.066(7) . . H23" H Uiso 0.0069(6) -0.323(4) 0.4393(14) 1.000 0.057(6) . . H24 H Uiso 0.0967(4) 0.601(3) 0.5066(11) 1.000 0.031(4) . . H24' H Uiso 0.1086(4) 0.603(3) 0.4113(11) 1.000 0.034(5) . . H24" H Uiso 0.1315(5) 0.476(3) 0.4870(11) 1.000 0.039(5) . . 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 C1 0.0170(6) 0.0169(7) 0.0203(7) -0.0009(5) 0.0004(5) 0.0025(5) C2 0.0180(7) 0.0232(8) 0.0221(7) 0.0035(6) -0.0003(5) 0.0014(6) C3 0.0196(7) 0.0220(8) 0.0301(8) 0.0042(6) 0.0048(6) 0.0010(6) C4 0.0154(6) 0.0197(7) 0.0279(7) -0.0031(6) 0.0039(5) 0.0029(5) C5 0.0137(6) 0.0219(8) 0.0362(8) -0.0076(6) 0.0043(6) 0.0016(6) C6 0.0128(7) 0.0328(9) 0.0359(9) -0.0113(7) -0.0013(6) 0.0023(6) C7 0.0162(7) 0.0327(9) 0.0267(8) -0.0029(6) -0.0017(6) 0.0083(6) C8 0.0155(6) 0.0235(8) 0.0234(7) -0.0020(6) 0.0021(5) 0.0057(6) C9 0.0137(6) 0.0198(7) 0.0228(7) -0.0036(5) 0.0014(5) 0.0022(5) C10 0.0229(7) 0.0295(9) 0.0229(8) 0.0009(6) 0.0031(6) 0.0024(7) C11 0.0181(7) 0.0256(9) 0.0522(11) -0.0054(8) 0.0068(7) -0.0035(7) C12 0.0206(7) 0.0267(8) 0.0278(8) 0.0058(7) 0.0021(6) 0.0068(6) C13 0.0173(7) 0.0165(7) 0.0208(7) -0.0012(5) -0.0003(5) 0.0026(5) C14 0.0169(7) 0.0240(8) 0.0221(7) -0.0039(6) 0.0006(5) -0.0010(6) C15 0.0184(7) 0.0215(8) 0.0321(8) -0.0048(6) -0.0002(6) -0.0018(6) C16 0.0140(6) 0.0186(7) 0.0278(7) -0.0006(6) -0.0006(5) 0.0035(5) C17 0.0137(6) 0.0214(8) 0.0355(8) 0.0058(6) 0.0017(6) 0.0041(6) C18 0.0193(7) 0.0301(9) 0.0310(8) 0.0091(7) 0.0066(6) 0.0057(6) C19 0.0212(7) 0.0300(9) 0.0233(8) 0.0009(6) 0.0021(6) 0.0073(6) C20 0.0144(6) 0.0230(8) 0.0229(7) 0.0003(6) -0.0013(5) 0.0056(5) C21 0.0123(6) 0.0193(7) 0.0243(7) 0.0025(6) -0.0005(5) 0.0035(5) C22 0.0209(7) 0.0281(9) 0.0255(8) -0.0041(7) -0.0046(6) 0.0002(6) C23 0.0191(8) 0.0241(9) 0.0454(10) 0.0053(7) 0.0047(7) -0.0008(6) C24 0.0196(7) 0.0250(8) 0.0237(8) -0.0062(6) -0.0016(6) 0.0037(6) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.5318(19) . . no C1 C9 1.4870(17) . . no C1 C13 1.3551(17) . . no C2 C3 1.559(2) . . no C2 C10 1.538(2) . . no C3 C4 1.511(2) . . no C4 C5 1.4006(18) . . no C4 C9 1.4111(17) . . no C5 C6 1.396(2) . . no C5 C11 1.512(2) . . no C6 C7 1.393(2) . . no C7 C8 1.409(2) . . no C8 C9 1.4080(19) . . no C8 C12 1.510(2) . . no C13 C14 1.5362(18) . . no C13 C21 1.4807(18) . . no C14 C15 1.555(2) . . no C14 C22 1.538(2) . . no C15 C16 1.511(2) . . no C16 C17 1.3986(19) . . no C16 C21 1.4113(17) . . no C17 C18 1.398(2) . . no C17 C23 1.512(2) . . no C18 C19 1.393(2) . . no C19 C20 1.406(2) . . no C20 C21 1.4084(18) . . no C20 C24 1.509(2) . . no C2 H2 0.983(15) . . no C3 H3 1.001(16) . . no C3 H3' 1.025(17) . . no C6 H6 0.983(19) . . no C7 H7 1.005(16) . . no C10 H10 0.977(19) . . no C10 H10' 1.017(18) . . no C10 H10" 1.015(17) . . no C11 H11 1.01(2) . . no C11 H11' 1.02(2) . . no C11 H11" 0.998(18) . . no C12 H12 1.005(17) . . no C12 H12' 1.016(18) . . no C12 H12" 0.998(18) . . no C14 H14 0.984(16) . . no C15 H15 1.030(19) . . no C15 H15' 1.030(17) . . no C18 H18 0.990(18) . . no C19 H19 0.999(18) . . no C22 H22 0.993(16) . . no C22 H22' 0.976(17) . . no C22 H22" 1.030(18) . . no C23 H23 0.994(18) . . no C23 H23' 1.00(2) . . no C23 H23" 0.97(2) . . no C24 H24 0.988(17) . . no C24 H24' 1.003(18) . . no C24 H24" 0.987(19) . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C9 105.25(10) . . . no C2 C1 C13 123.19(12) . . . no C9 C1 C13 131.44(12) . . . no C1 C2 C3 101.88(11) . . . no C1 C2 C10 112.30(11) . . . no C3 C2 C10 111.21(13) . . . no C2 C3 C4 102.80(12) . . . no C3 C4 C5 127.49(12) . . . no C3 C4 C9 110.18(11) . . . no C5 C4 C9 122.32(12) . . . no C4 C5 C6 116.42(12) . . . no C4 C5 C11 121.41(13) . . . no C6 C5 C11 122.17(13) . . . no C5 C6 C7 121.77(14) . . . no C6 C7 C8 122.31(14) . . . no C7 C8 C9 116.24(12) . . . no C7 C8 C12 119.43(13) . . . no C9 C8 C12 124.20(12) . . . no C1 C9 C4 108.32(11) . . . no C1 C9 C8 130.62(11) . . . no C4 C9 C8 120.67(11) . . . no C1 C13 C14 123.50(11) . . . no C1 C13 C21 131.57(12) . . . no C14 C13 C21 104.72(10) . . . no C13 C14 C15 101.31(11) . . . no C13 C14 C22 112.42(11) . . . no C15 C14 C22 110.68(11) . . . no C14 C15 C16 102.51(12) . . . no C15 C16 C17 128.02(12) . . . no C15 C16 C21 109.79(12) . . . no C17 C16 C21 122.15(12) . . . no C16 C17 C18 116.30(12) . . . no C16 C17 C23 121.86(13) . . . no C18 C17 C23 121.83(13) . . . no C17 C18 C19 121.91(14) . . . no C18 C19 C20 122.31(14) . . . no C19 C20 C21 116.02(12) . . . no C19 C20 C24 120.07(12) . . . no C21 C20 C24 123.75(11) . . . no C13 C21 C16 108.41(11) . . . no C13 C21 C20 130.13(11) . . . no C16 C21 C20 121.03(11) . . . no C1 C2 H2 112.7(9) . . . no C3 C2 H2 110.3(10) . . . no C10 C2 H2 108.3(9) . . . no C2 C3 H3 111.9(10) . . . no C2 C3 H3' 113.1(9) . . . no C4 C3 H3 114.5(9) . . . no C4 C3 H3' 109.1(9) . . . no H3 C3 H3' 105.7(14) . . . no C5 C6 H6 118.2(10) . . . no C7 C6 H6 120.1(10) . . . no C6 C7 H7 121.6(10) . . . no C8 C7 H7 116.1(10) . . . no C2 C10 H10 109.2(11) . . . no C2 C10 H10' 111.0(10) . . . no C2 C10 H10" 112.2(9) . . . no H10 C10 H10' 111.0(14) . . . no H10 C10 H10" 105.3(14) . . . no H10' C10 H10" 107.9(13) . . . no C5 C11 H11 111.4(10) . . . no C5 C11 H11' 110.2(13) . . . no C5 C11 H11" 112.2(11) . . . no H11 C11 H11' 111.9(16) . . . no H11 C11 H11" 104.8(15) . . . no H11' C11 H11" 106.2(17) . . . no C8 C12 H12 112.1(10) . . . no C8 C12 H12' 109.7(11) . . . no C8 C12 H12" 111.7(10) . . . no H12 C12 H12' 106.3(14) . . . no H12 C12 H12" 107.8(15) . . . no H12' C12 H12" 109.0(15) . . . no C13 C14 H14 111.9(9) . . . no C15 C14 H14 112.0(10) . . . no C22 C14 H14 108.5(10) . . . no C14 C15 H15 111.4(10) . . . no C14 C15 H15' 111.8(9) . . . no C16 C15 H15 115.0(10) . . . no C16 C15 H15' 110.3(9) . . . no H15 C15 H15' 105.9(14) . . . no C17 C18 H18 118.4(10) . . . no C19 C18 H18 119.7(11) . . . no C18 C19 H19 119.6(10) . . . no C20 C19 H19 118.1(10) . . . no C14 C22 H22 110.0(10) . . . no C14 C22 H22' 110.0(10) . . . no C14 C22 H22" 112.2(9) . . . no H22 C22 H22' 110.2(13) . . . no H22 C22 H22" 108.4(14) . . . no H22' C22 H22" 106.1(14) . . . no C17 C23 H23 112.1(11) . . . no C17 C23 H23' 114.2(14) . . . no C17 C23 H23" 113.1(14) . . . no H23 C23 H23' 106.8(17) . . . no H23 C23 H23" 106.2(18) . . . no H23' C23 H23" 103.7(19) . . . no C20 C24 H24 111.3(10) . . . no C20 C24 H24' 110.0(10) . . . no C20 C24 H24" 108.9(11) . . . no H24 C24 H24' 108.9(14) . . . no H24 C24 H24" 106.5(14) . . . no H24' C24 H24" 111.3(14) . . . 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 C1 C2 C3 -32.87(13) . . . . no C9 C1 C2 C10 86.20(13) . . . . no C13 C1 C2 C3 143.36(13) . . . . no C13 C1 C2 C10 -97.57(15) . . . . no C2 C1 C9 C4 22.07(13) . . . . no C2 C1 C9 C8 -150.56(13) . . . . no C13 C1 C9 C4 -153.72(13) . . . . no C13 C1 C9 C8 33.7(2) . . . . no C2 C1 C13 C14 19.45(18) . . . . no C2 C1 C13 C21 -166.62(12) . . . . no C9 C1 C13 C14 -165.41(12) . . . . no C9 C1 C13 C21 8.5(2) . . . . no C1 C2 C3 C4 31.31(13) . . . . no C10 C2 C3 C4 -88.53(13) . . . . no C2 C3 C4 C5 159.01(13) . . . . no C2 C3 C4 C9 -19.47(15) . . . . no C3 C4 C5 C6 -175.62(14) . . . . no C3 C4 C5 C11 4.3(2) . . . . no C9 C4 C5 C6 2.69(19) . . . . no C9 C4 C5 C11 -177.44(13) . . . . no C3 C4 C9 C1 -1.25(14) . . . . no C3 C4 C9 C8 172.25(12) . . . . no C5 C4 C9 C1 -179.82(11) . . . . no C5 C4 C9 C8 -6.32(19) . . . . no C4 C5 C6 C7 1.3(2) . . . . no C11 C5 C6 C7 -178.59(15) . . . . no C5 C6 C7 C8 -1.7(2) . . . . no C6 C7 C8 C9 -1.8(2) . . . . no C6 C7 C8 C12 174.09(15) . . . . no C7 C8 C9 C1 177.45(13) . . . . no C7 C8 C9 C4 5.59(19) . . . . no C12 C8 C9 C1 1.8(2) . . . . no C12 C8 C9 C4 -170.02(13) . . . . no C1 C13 C14 C15 140.27(13) . . . . no C1 C13 C14 C22 -101.56(14) . . . . no C21 C13 C14 C15 -35.04(12) . . . . no C21 C13 C14 C22 83.13(13) . . . . no C1 C13 C21 C16 -151.32(13) . . . . no C1 C13 C21 C20 36.3(2) . . . . no C14 C13 C21 C16 23.46(13) . . . . no C14 C13 C21 C20 -148.91(12) . . . . no C13 C14 C15 C16 33.43(12) . . . . no C22 C14 C15 C16 -85.99(13) . . . . no C14 C15 C16 C17 156.80(12) . . . . no C14 C15 C16 C21 -20.90(14) . . . . no C15 C16 C17 C18 -175.21(14) . . . . no C15 C16 C17 C23 5.6(2) . . . . no C21 C16 C17 C18 2.23(18) . . . . no C21 C16 C17 C23 -177.01(12) . . . . no C15 C16 C21 C13 -1.30(14) . . . . no C15 C16 C21 C20 171.90(12) . . . . no C17 C16 C21 C13 -179.15(11) . . . . no C17 C16 C21 C20 -5.96(18) . . . . no C16 C17 C18 C19 2.0(2) . . . . no C23 C17 C18 C19 -178.81(14) . . . . no C17 C18 C19 C20 -2.6(2) . . . . no C18 C19 C20 C21 -1.0(2) . . . . no C18 C19 C20 C24 174.53(14) . . . . no C19 C20 C21 C13 176.67(13) . . . . no C19 C20 C21 C16 5.12(18) . . . . no C24 C20 C21 C13 1.3(2) . . . . no C24 C20 C21 C16 -170.23(12) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag C1 C24 3.398(2) . . no C5 C12 3.530(2) . 1_565 no C8 C20 3.5817(19) . . no C8 C21 3.5896(19) . . no C8 C24 3.262(2) . . no C9 C20 3.5995(19) . . no C9 C24 3.213(2) . . no C12 C13 3.410(2) . . no C12 C24 3.491(3) . . no C12 C5 3.530(2) . 1_545 no C12 C21 3.191(2) . . no C12 C20 3.237(2) . . no C13 C12 3.410(2) . . no C17 C24 3.487(2) . 1_545 no C20 C12 3.237(2) . . no C20 C9 3.5995(19) . . no C20 C8 3.5817(19) . . no C21 C12 3.191(2) . . no C21 C8 3.5896(19) . . no C24 C17 3.487(2) . 1_565 no C24 C8 3.262(2) . . no C24 C12 3.491(3) . . no C24 C9 3.213(2) . . no C24 C1 3.398(2) . . no C1 H24' 2.906(17) . . no C1 H12" 2.943(18) . . no C2 H14 2.774(17) . . no C3 H11" 3.067(19) . . no C3 H11 3.072(19) . . no C4 H10 2.924(18) . . no C4 H12" 3.087(18) . 1_565 no C5 H12' 3.073(17) . 1_565 no C5 H11 3.039(19) . 6_545 no C7 H7 2.986(16) . 7_556 no C8 H11" 2.918(18) . 1_545 no C8 H24" 2.596(19) . . no C9 H10 2.880(18) . . no C9 H24' 2.878(16) . . no C9 H24" 2.892(18) . . no C10 H14 3.042(16) . . no C11 H3 2.941(16) . . no C11 H11 3.099(18) . 6_555 no C12 H24" 2.905(18) . . no C13 H24' 2.884(18) . . no C13 H12" 2.940(18) . . no C14 H2 2.816(17) . . no C15 H23' 3.04(2) . . no C16 H24' 3.078(17) . 1_545 no C16 H22 2.853(17) . . no C17 H24' 3.087(16) . 1_545 no C17 H24 3.076(17) . 1_545 no C18 H23" 3.06(2) . 3_556 no C20 H23 2.772(19) . 1_565 no C20 H12 2.569(16) . . no C21 H12 2.869(17) . . no C21 H12" 2.847(19) . . no C21 H23 3.079(19) . 1_565 no C21 H22 2.845(16) . . no C22 H18 3.089(18) . 4_554 no C23 H15 2.966(18) . . no C24 H12 2.923(17) . . no C24 H23 3.027(19) . 1_565 no H2 C14 2.816(17) . . no H2 H14 2.48(2) . . no H2 H22" 2.59(2) . . no H3 C11 2.941(16) . . no H3 H10' 2.50(2) . . no H3 H11 2.59(3) . . no H6 H11' 2.39(3) . . no H6 H6 2.49(3) . 7_566 no H7 H12' 2.36(3) . . no H7 C7 2.986(16) . 7_556 no H7 H7 2.43(2) . 7_556 no H10 C4 2.924(18) . . no H10 C9 2.880(18) . . no H10' H3 2.50(2) . . no H10' H24" 2.47(2) . 4_564 no H10" H14 2.47(2) . . no H11 C3 3.072(19) . . no H11 H3 2.59(3) . . no H11 C5 3.039(19) . 6_555 no H11 C11 3.099(18) . 6_545 no H11' H6 2.39(3) . . no H11" C3 3.067(19) . . no H11" C8 2.918(18) . 1_565 no H12 C20 2.569(16) . . no H12 C21 2.869(17) . . no H12 C24 2.923(17) . . no H12 H24" 2.38(3) . . no H12' C5 3.073(17) . 1_545 no H12' H7 2.36(3) . . no H12" C1 2.943(18) . . no H12" C4 3.087(18) . 1_545 no H12" C13 2.940(18) . . no H12" C21 2.847(19) . . no H14 C2 2.774(17) . . no H14 C10 3.042(16) . . no H14 H2 2.48(2) . . no H14 H10" 2.47(2) . . no H15 C23 2.966(18) . . no H15 H22' 2.49(3) . . no H15 H23' 2.55(3) . . no H15 H23' 2.31(3) . 2_555 no H15' H22" 2.54(2) . 1_545 no H18 H23" 2.44(3) . . no H18 C22 3.089(18) . 4_555 no H18 H22' 2.29(3) . 4_555 no H19 H24 2.43(2) . . no H19 H22" 2.38(2) . 4_565 no H22 C16 2.853(17) . . no H22 C21 2.845(16) . . no H22 H23 2.52(2) . 1_565 no H22' H15 2.49(3) . . no H22' H18 2.29(3) . 4_554 no H22" H2 2.59(2) . . no H22" H15' 2.54(2) . 1_565 no H22" H19 2.38(2) . 4_564 no H23 C20 2.772(19) . 1_545 no H23 C21 3.079(19) . 1_545 no H23 C24 3.027(19) . 1_545 no H23 H22 2.52(2) . 1_545 no H23' C15 3.04(2) . . no H23' H15 2.55(3) . . no H23' H15 2.31(3) . 2_555 no H23" H18 2.44(3) . . no H23" C18 3.06(2) . 3_556 no H24 C17 3.076(17) . 1_565 no H24 H19 2.43(2) . . no H24' C1 2.906(17) . . no H24' C9 2.878(16) . . no H24' C13 2.884(18) . . no H24' C16 3.078(17) . 1_565 no H24' C17 3.087(16) . 1_565 no H24" C8 2.596(19) . . no H24" C9 2.892(18) . . no H24" C12 2.905(18) . . no H24" H12 2.38(3) . . no H24" H10' 2.47(2) . 4_565 no # Loop Mechanism for Extra Tables(s) #loop_ #_publ_manuscript_incl_extra_item #'_geom_extra_tableA_col_1' #'_geom_extra_tableA_col_2' #'_geom_extra_tableA_col_3' #'_geom_extra_table_head_A' #'_geom_table_footnote_A' #'_geom_extra_tableB_col_1' #'_geom_extra_tableB_col_2' #'_geom_extra_tableB_col_3' #'_geom_extra_table_head_B' #'_geom_table_footnote_B' # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 # ? ? ? # #loop_ #_geom_extra_tableB_col_1 #_geom_extra_tableB_col_2 #_geom_extra_tableB_col_3 # ? ? ? # #_geom_table_footnote_A #; # ? #; # #_geom_table_footnote_B #; # ? #; # #_geom_table_footnote_A #; # ? #; # #_geom_table_footnote_B #; # ? #; #===END of Crystallographic Information File