Supplementary Material (ESI) for Organic & Biomolecular Chemistry This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Org.Biomol.Chem. _journal_coden_cambridge 0177 _audit_creation_date 2006-09-08 _audit_creation_method 'by CrystalStructure 3.7.0' _audit_update_record ? _publ_contact_author_name 'Robert Gawley' _publ_contact_author_address ; Department of Chemistry and Biochemistry University of Arkansas Fayetteville AR 72701 UNITED STATES OF AMERICA ; _publ_section_title ; Diastereoselectivity of Polar and Radical Couplings in Electrophilic Substitutions of Rigid 2-Lithio-N-methylpyrrolidines ; _publ_section_references ; ENTER OTHER REFERENCES Rigaku/MSC and Rigaku Corporation. (2004). CrystalStructure 3.7.0. Single Crystal Structure Analysis Software. Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX, USA 77381-5209. Rigaku, 3-9-12 Akishima, Tokyo 196-8666, Japan. Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10, Chemical Crystallography Laboratory, Oxford, UK. Larson, A. C. (1970), Crystallographic Computing, 291-294. ed F. R. Ahmed, Munksgaard, Copenhagen. ; _publ_contact_author_email BGAWLEY@UARK.EDU loop_ _publ_author_name R.Gawley D.B.Eddings M.Santiago # Attachment '11a.cif.txt' data_CO2_New_1b _database_code_depnum_ccdc_archive 'CCDC 610644' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C11 H22 I N O ' _chemical_formula_moiety 'C11 H22 I N O ' _chemical_formula_weight 311.21 _chemical_melting_point ? _chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk' #============================================================================== # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2+X,1/2-Y,-Z 3 -X,1/2+Y,1/2-Z 4 1/2-X,-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 7.1485(11) _cell_length_b 13.160(2) _cell_length_c 14.239(2) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_volume 1339.5(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 3141 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 34.6 _cell_measurement_temperature 173.1 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_diffrn 1.543 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 624.00 _exptl_absorpt_coefficient_mu 2.367 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.340 _exptl_absorpt_correction_T_max 0.492 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 18861 _diffrn_reflns_av_R_equivalents 0.037 _diffrn_reflns_theta_max 34.58 _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 34.58 _diffrn_measured_fraction_theta_full 0.960 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 11 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3087 _reflns_number_gt 2593 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1033 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 3087 _refine_ls_number_parameters 151 _refine_ls_goodness_of_fit_ref 1.762 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/\s^2^(Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 1.51 _refine_diff_density_min -1.30 _refine_ls_extinction_method 'Larson (1970) Crystallographic Computing eq. 22' _refine_ls_extinction_coef 20(6) _refine_ls_abs_structure_details 'Flack, H. D. (1983), Acta Cryst. A39, 876-881.' _refine_ls_abs_structure_Flack 0.25(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; I I -0.474 1.812 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I(1) I -0.56802(5) -0.50428(3) -0.15159(2) 0.03782(10) Uani 1.00 1 d . . . O(1) O -0.1737(6) -0.2131(2) -0.4080(3) 0.0507(14) Uani 1.00 1 d . . . N(1) N -0.0474(6) -0.4157(3) -0.3332(3) 0.0300(11) Uani 1.00 1 d . . . C(1) C -0.3037(9) -0.2934(4) -0.3970(4) 0.0401(16) Uani 1.00 1 d . . . C(2) C -0.2004(9) -0.3936(4) -0.4073(4) 0.0324(13) Uani 1.00 1 d . . . C(3) C -0.3209(6) -0.4894(3) -0.4057(3) 0.0262(10) Uani 1.00 1 d . . . C(4) C -0.4469(6) -0.5101(3) -0.4887(3) 0.0296(11) Uani 1.00 1 d . . . C(5) C -0.5445(7) -0.6105(4) -0.4724(4) 0.0378(15) Uani 1.00 1 d . . . C(6) C -0.4060(9) -0.6951(4) -0.4553(5) 0.0476(18) Uani 1.00 1 d . . . C(7) C -0.2691(8) -0.6733(4) -0.3754(4) 0.0391(16) Uani 1.00 1 d . . . C(8) C -0.1800(9) -0.5717(4) -0.3917(4) 0.0336(14) Uani 1.00 1 d . . . C(9) C -0.0597(8) -0.5300(4) -0.3144(4) 0.0368(14) Uani 1.00 1 d . . . C(10) C -0.0800(9) -0.3615(4) -0.2430(4) 0.0514(19) Uani 1.00 1 d . . . C(11) C 0.1377(8) -0.3884(5) -0.3709(4) 0.0463(18) Uani 1.00 1 d . . . H(1) H -0.1484 -0.2142 -0.3593 0.061 Uiso 1.00 1 c R . . H(2) H -0.3592 -0.2913 -0.3364 0.048 Uiso 1.00 1 c R . . H(3) H -0.3983 -0.2873 -0.4435 0.048 Uiso 1.00 1 c R . . H(4) H -0.1413 -0.3920 -0.4670 0.039 Uiso 1.00 1 c R . . H(5) H -0.3960 -0.4860 -0.3507 0.031 Uiso 1.00 1 c R . . H(6) H -0.5365 -0.4571 -0.4944 0.035 Uiso 1.00 1 c R . . H(7) H -0.3733 -0.5132 -0.5442 0.035 Uiso 1.00 1 c R . . H(8) H -0.6195 -0.6055 -0.4175 0.045 Uiso 1.00 1 c R . . H(9) H -0.6219 -0.6253 -0.5249 0.045 Uiso 1.00 1 c R . . H(10) H -0.4717 -0.7563 -0.4422 0.057 Uiso 1.00 1 c R . . H(11) H -0.3364 -0.7029 -0.5117 0.057 Uiso 1.00 1 c R . . H(12) H -0.3355 -0.6720 -0.3176 0.047 Uiso 1.00 1 c R . . H(13) H -0.1751 -0.7243 -0.3728 0.047 Uiso 1.00 1 c R . . H(14) H -0.1075 -0.5756 -0.4475 0.040 Uiso 1.00 1 c R . . H(15) H 0.0614 -0.5597 -0.3164 0.044 Uiso 1.00 1 c R . . H(16) H -0.1151 -0.5429 -0.2550 0.044 Uiso 1.00 1 c R . . H(17) H -0.0227 -0.2964 -0.2442 0.062 Uiso 1.00 1 c R . . H(18) H -0.0318 -0.3996 -0.1917 0.062 Uiso 1.00 1 c R . . H(19) H -0.2114 -0.3539 -0.2360 0.062 Uiso 1.00 1 c R . . H(20) H 0.1911 -0.4462 -0.4006 0.056 Uiso 1.00 1 c R . . H(21) H 0.2166 -0.3668 -0.3210 0.056 Uiso 1.00 1 c R . . H(22) H 0.1251 -0.3350 -0.4153 0.056 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 I(1) 0.03607(19) 0.0490(2) 0.02844(18) -0.0030(2) 0.00153(12) 0.0021(2) O(1) 0.054(2) 0.035(2) 0.063(3) -0.009(2) 0.001(2) 0.005(2) N(1) 0.029(2) 0.030(2) 0.031(2) -0.0023(19) 0.0008(19) -0.0024(17) C(1) 0.035(2) 0.028(2) 0.057(4) 0.003(2) 0.006(3) 0.002(2) C(2) 0.034(2) 0.029(2) 0.034(2) -0.000(2) -0.006(2) 0.001(2) C(3) 0.029(2) 0.025(2) 0.024(2) 0.005(2) -0.0018(17) 0.0017(19) C(4) 0.029(2) 0.025(2) 0.034(2) 0.008(2) -0.0049(19) -0.001(2) C(5) 0.033(2) 0.032(2) 0.049(3) -0.006(2) -0.005(2) 0.001(2) C(6) 0.051(3) 0.028(2) 0.064(4) -0.002(2) -0.014(3) 0.003(3) C(7) 0.048(3) 0.022(2) 0.046(3) 0.009(2) -0.008(3) 0.000(2) C(8) 0.033(2) 0.038(2) 0.031(2) 0.005(2) -0.004(2) -0.002(2) C(9) 0.036(2) 0.038(3) 0.036(2) 0.007(2) -0.010(2) 0.005(2) C(10) 0.073(4) 0.051(3) 0.030(3) -0.024(4) -0.004(3) -0.005(2) C(11) 0.032(2) 0.052(4) 0.056(4) -0.004(2) -0.001(3) 0.007(3) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SHELXS97 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.7.0' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 O(1) C(1) 1.416(7) ? . . N(1) C(2) 1.548(7) ? . . N(1) C(9) 1.530(6) ? . . N(1) C(10) 1.487(7) ? . . N(1) C(11) 1.473(7) ? . . C(1) C(2) 1.518(8) ? . . C(2) C(3) 1.527(7) ? . . C(3) C(4) 1.510(6) ? . . C(3) C(8) 1.493(7) ? . . C(4) C(5) 1.513(7) ? . . C(5) C(6) 1.510(8) ? . . C(6) C(7) 1.528(9) ? . . C(7) C(8) 1.499(8) ? . . C(8) C(9) 1.500(8) ? . . C(1) H(2) 0.950 ? . . C(1) H(3) 0.950 ? . . C(2) H(4) 0.950 ? . . C(3) H(5) 0.950 ? . . C(4) H(6) 0.950 ? . . C(4) H(7) 0.950 ? . . C(5) H(8) 0.950 ? . . C(5) H(9) 0.950 ? . . C(6) H(10) 0.950 ? . . C(6) H(11) 0.950 ? . . C(7) H(12) 0.950 ? . . C(7) H(13) 0.950 ? . . C(8) H(14) 0.950 ? . . C(9) H(15) 0.950 ? . . C(9) H(16) 0.950 ? . . C(10) H(17) 0.950 ? . . C(10) H(18) 0.950 ? . . C(10) H(19) 0.950 ? . . C(11) H(20) 0.950 ? . . C(11) H(21) 0.950 ? . . C(11) H(22) 0.950 ? . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 C(2) N(1) C(9) 105.2(4) ? . . . C(2) N(1) C(10) 112.8(4) ? . . . C(2) N(1) C(11) 109.9(4) ? . . . C(9) N(1) C(10) 108.2(4) ? . . . C(9) N(1) C(11) 110.8(4) ? . . . C(10) N(1) C(11) 109.8(4) ? . . . O(1) C(1) C(2) 108.5(5) ? . . . N(1) C(2) C(1) 116.2(4) ? . . . N(1) C(2) C(3) 103.5(4) ? . . . C(1) C(2) C(3) 116.2(5) ? . . . C(2) C(3) C(4) 118.3(4) ? . . . C(2) C(3) C(8) 102.7(4) ? . . . C(4) C(3) C(8) 112.1(4) ? . . . C(3) C(4) C(5) 108.2(4) ? . . . C(4) C(5) C(6) 111.5(4) ? . . . C(5) C(6) C(7) 113.7(5) ? . . . C(6) C(7) C(8) 108.9(4) ? . . . C(3) C(8) C(7) 112.4(5) ? . . . C(3) C(8) C(9) 102.7(4) ? . . . C(7) C(8) C(9) 117.2(5) ? . . . N(1) C(9) C(8) 105.4(4) ? . . . C(1) O(1) H(1) 92.4 ? . . . O(1) C(1) H(2) 110.7 ? . . . O(1) C(1) H(3) 109.1 ? . . . C(2) C(1) H(2) 108.4 ? . . . C(2) C(1) H(3) 110.6 ? . . . H(2) C(1) H(3) 109.5 ? . . . N(1) C(2) H(4) 107.5 ? . . . C(1) C(2) H(4) 106.4 ? . . . C(3) C(2) H(4) 106.4 ? . . . C(2) C(3) H(5) 107.0 ? . . . C(4) C(3) H(5) 108.5 ? . . . C(8) C(3) H(5) 107.8 ? . . . C(3) C(4) H(6) 109.7 ? . . . C(3) C(4) H(7) 109.2 ? . . . C(5) C(4) H(6) 110.0 ? . . . C(5) C(4) H(7) 110.3 ? . . . H(6) C(4) H(7) 109.5 ? . . . C(4) C(5) H(8) 109.1 ? . . . C(4) C(5) H(9) 109.1 ? . . . C(6) C(5) H(8) 106.7 ? . . . C(6) C(5) H(9) 110.9 ? . . . H(8) C(5) H(9) 109.5 ? . . . C(5) C(6) H(10) 109.4 ? . . . C(5) C(6) H(11) 106.7 ? . . . C(7) C(6) H(10) 109.2 ? . . . C(7) C(6) H(11) 108.3 ? . . . H(10) C(6) H(11) 109.5 ? . . . C(6) C(7) H(12) 109.2 ? . . . C(6) C(7) H(13) 110.4 ? . . . C(8) C(7) H(12) 109.3 ? . . . C(8) C(7) H(13) 109.6 ? . . . H(12) C(7) H(13) 109.5 ? . . . C(3) C(8) H(14) 107.2 ? . . . C(7) C(8) H(14) 108.3 ? . . . C(9) C(8) H(14) 108.7 ? . . . N(1) C(9) H(15) 110.3 ? . . . N(1) C(9) H(16) 110.7 ? . . . C(8) C(9) H(15) 110.5 ? . . . C(8) C(9) H(16) 110.4 ? . . . H(15) C(9) H(16) 109.5 ? . . . N(1) C(10) H(17) 110.4 ? . . . N(1) C(10) H(18) 110.7 ? . . . N(1) C(10) H(19) 107.3 ? . . . H(17) C(10) H(18) 109.5 ? . . . H(17) C(10) H(19) 109.5 ? . . . H(18) C(10) H(19) 109.5 ? . . . N(1) C(11) H(20) 109.2 ? . . . N(1) C(11) H(21) 109.5 ? . . . N(1) C(11) H(22) 109.7 ? . . . H(20) C(11) H(21) 109.5 ? . . . H(20) C(11) H(22) 109.5 ? . . . H(21) C(11) H(22) 109.5 ? . . . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C(2) N(1) C(9) C(8) 13.1(5) ? . . . . C(9) N(1) C(2) C(1) 143.2(5) ? . . . . C(9) N(1) C(2) C(3) 14.6(5) ? . . . . C(10) N(1) C(2) C(1) 25.4(6) ? . . . . C(10) N(1) C(2) C(3) -103.1(4) ? . . . . C(11) N(1) C(2) C(1) -97.5(6) ? . . . . C(11) N(1) C(2) C(3) 133.9(4) ? . . . . C(10) N(1) C(9) C(8) 134.0(5) ? . . . . C(11) N(1) C(9) C(8) -105.6(5) ? . . . . O(1) C(1) C(2) N(1) 62.8(6) ? . . . . O(1) C(1) C(2) C(3) -175.1(4) ? . . . . N(1) C(2) C(3) C(4) -161.1(4) ? . . . . N(1) C(2) C(3) C(8) -37.2(5) ? . . . . C(1) C(2) C(3) C(4) 70.3(6) ? . . . . C(1) C(2) C(3) C(8) -165.7(5) ? . . . . C(2) C(3) C(4) C(5) 177.7(4) ? . . . . C(2) C(3) C(8) C(7) 172.6(4) ? . . . . C(2) C(3) C(8) C(9) 45.8(5) ? . . . . C(4) C(3) C(8) C(7) -59.4(6) ? . . . . C(4) C(3) C(8) C(9) 173.8(4) ? . . . . C(8) C(3) C(4) C(5) 58.5(5) ? . . . . C(3) C(4) C(5) C(6) -55.7(6) ? . . . . C(4) C(5) C(6) C(7) 54.7(7) ? . . . . C(5) C(6) C(7) C(8) -51.9(7) ? . . . . C(6) C(7) C(8) C(3) 53.6(6) ? . . . . C(6) C(7) C(8) C(9) 172.1(5) ? . . . . C(3) C(8) C(9) N(1) -36.5(5) ? . . . . C(7) C(8) C(9) N(1) -160.2(5) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 I(1) O(1) 3.418(4) ? . 44403 O(1) I(1) 3.418(4) ? . 45403 I(1) H(1) 3.430 ? . 44403 I(1) H(4) 3.318 ? . 44504 I(1) H(5) 3.100 ? . . I(1) H(7) 3.513 ? . 44504 I(1) H(9) 3.328 ? . 34504 I(1) H(10) 3.538 ? . 45403 I(1) H(14) 3.335 ? . 44504 I(1) H(16) 3.593 ? . . I(1) H(19) 3.443 ? . . I(1) H(21) 3.386 ? . 45501 O(1) H(1) 0.717 ? . . O(1) H(3) 2.888 ? . 54402 O(1) H(6) 2.812 ? . 54402 O(1) H(20) 3.572 ? . 44402 O(1) H(22) 2.966 ? . 44402 N(1) H(1) 2.773 ? . . C(1) H(1) 1.615 ? . . C(1) H(22) 3.202 ? . 44402 C(2) H(1) 2.485 ? . . C(3) H(20) 3.535 ? . 45501 C(4) H(18) 3.129 ? . 44404 C(4) H(20) 2.997 ? . 45501 C(5) H(11) 3.230 ? . 43402 C(5) H(13) 3.233 ? . 43402 C(5) H(18) 3.173 ? . 44404 C(5) H(20) 3.049 ? . 45501 C(6) H(9) 3.129 ? . 53402 C(6) H(10) 3.490 ? . 53402 C(6) H(11) 3.389 ? . 43402 C(6) H(13) 3.289 ? . 43402 C(7) H(9) 3.185 ? . 53402 C(7) H(10) 3.482 ? . 53402 C(7) H(17) 3.142 ? . 54403 C(8) H(10) 3.597 ? . 53402 C(10) H(1) 2.596 ? . . C(10) H(7) 3.293 ? . 44504 C(10) H(9) 3.429 ? . 44504 C(10) H(11) 3.454 ? . 44504 C(10) H(13) 3.051 ? . 55403 C(11) H(1) 3.076 ? . . C(11) H(3) 3.521 ? . 54402 C(11) H(5) 3.584 ? . 65501 C(11) H(6) 3.056 ? . 65501 C(11) H(8) 3.409 ? . 65501 H(1) I(1) 3.430 ? . 45403 H(1) O(1) 0.717 ? . . H(1) N(1) 2.773 ? . . H(1) C(1) 1.615 ? . . H(1) C(2) 2.485 ? . . H(1) C(10) 2.596 ? . . H(1) C(11) 3.076 ? . . H(1) H(2) 1.845 ? . . H(1) H(3) 2.357 ? . . H(1) H(3) 3.329 ? . 54402 H(1) H(4) 2.798 ? . . H(1) H(6) 3.173 ? . 54402 H(1) H(15) 3.283 ? . 55403 H(1) H(16) 3.359 ? . 55403 H(1) H(17) 2.158 ? . . H(1) H(18) 3.512 ? . . H(1) H(19) 2.582 ? . . H(1) H(21) 3.337 ? . . H(1) H(22) 2.643 ? . . H(2) H(1) 1.845 ? . . H(2) H(12) 3.470 ? . 45403 H(2) H(21) 3.198 ? . 45501 H(3) O(1) 2.888 ? . 44402 H(3) C(11) 3.521 ? . 44402 H(3) H(1) 2.357 ? . . H(3) H(1) 3.329 ? . 44402 H(3) H(4) 3.195 ? . 44402 H(3) H(21) 3.422 ? . 45501 H(3) H(22) 3.487 ? . 45501 H(3) H(22) 2.581 ? . 44402 H(4) I(1) 3.318 ? . 44404 H(4) H(1) 2.798 ? . . H(4) H(3) 3.195 ? . 54402 H(5) I(1) 3.100 ? . . H(5) C(11) 3.584 ? . 45501 H(5) H(20) 3.081 ? . 45501 H(5) H(21) 3.211 ? . 45501 H(6) O(1) 2.812 ? . 44402 H(6) C(11) 3.056 ? . 45501 H(6) H(1) 3.173 ? . 44402 H(6) H(18) 3.418 ? . 44404 H(6) H(20) 2.366 ? . 45501 H(6) H(21) 3.260 ? . 45501 H(6) H(22) 3.115 ? . 45501 H(7) I(1) 3.513 ? . 44404 H(7) C(10) 3.293 ? . 44404 H(7) H(16) 3.091 ? . 44404 H(7) H(18) 2.488 ? . 44404 H(7) H(19) 3.298 ? . 44404 H(8) C(11) 3.409 ? . 45501 H(8) H(11) 3.127 ? . 43402 H(8) H(14) 3.536 ? . 45501 H(8) H(15) 2.764 ? . 45501 H(8) H(20) 2.508 ? . 45501 H(9) I(1) 3.328 ? . 34404 H(9) C(6) 3.129 ? . 43402 H(9) C(7) 3.185 ? . 43402 H(9) C(10) 3.429 ? . 44404 H(9) H(10) 2.983 ? . 43402 H(9) H(11) 2.780 ? . 43402 H(9) H(13) 2.486 ? . 43402 H(9) H(17) 3.447 ? . 44404 H(9) H(18) 2.638 ? . 44404 H(9) H(20) 3.237 ? . 45501 H(10) I(1) 3.538 ? . 44403 H(10) C(6) 3.490 ? . 43402 H(10) C(7) 3.482 ? . 43402 H(10) C(8) 3.597 ? . 43402 H(10) H(9) 2.983 ? . 53402 H(10) H(11) 2.742 ? . 43402 H(10) H(13) 3.020 ? . 43402 H(10) H(14) 2.882 ? . 43402 H(11) C(5) 3.230 ? . 53402 H(11) C(6) 3.389 ? . 53402 H(11) C(10) 3.454 ? . 44404 H(11) H(8) 3.127 ? . 53402 H(11) H(9) 2.780 ? . 53402 H(11) H(10) 2.742 ? . 53402 H(11) H(13) 3.080 ? . 43402 H(11) H(14) 3.548 ? . 43402 H(11) H(17) 3.462 ? . 44404 H(11) H(18) 3.047 ? . 44404 H(11) H(19) 3.298 ? . 44404 H(12) H(2) 3.470 ? . 44403 H(12) H(17) 3.164 ? . 54403 H(12) H(21) 3.345 ? . 54403 H(13) C(5) 3.233 ? . 53402 H(13) C(6) 3.289 ? . 53402 H(13) C(10) 3.051 ? . 54403 H(13) H(9) 2.486 ? . 53402 H(13) H(10) 3.020 ? . 53402 H(13) H(11) 3.080 ? . 53402 H(13) H(17) 2.383 ? . 54403 H(13) H(18) 2.890 ? . 54403 H(13) H(19) 3.598 ? . 54403 H(13) H(21) 3.350 ? . 54403 H(14) I(1) 3.335 ? . 44404 H(14) H(8) 3.536 ? . 65501 H(14) H(10) 2.882 ? . 53402 H(14) H(11) 3.548 ? . 53402 H(15) H(1) 3.283 ? . 54403 H(15) H(8) 2.764 ? . 65501 H(15) H(17) 3.244 ? . 54403 H(16) I(1) 3.593 ? . . H(16) H(1) 3.359 ? . 54403 H(16) H(7) 3.091 ? . 44504 H(16) H(17) 3.479 ? . 54403 H(17) C(7) 3.142 ? . 55403 H(17) H(1) 2.158 ? . . H(17) H(9) 3.447 ? . 44504 H(17) H(11) 3.462 ? . 44504 H(17) H(12) 3.164 ? . 55403 H(17) H(13) 2.383 ? . 55403 H(17) H(15) 3.244 ? . 55403 H(17) H(16) 3.479 ? . 55403 H(18) C(4) 3.129 ? . 44504 H(18) C(5) 3.173 ? . 44504 H(18) H(1) 3.512 ? . . H(18) H(6) 3.418 ? . 44504 H(18) H(7) 2.488 ? . 44504 H(18) H(9) 2.638 ? . 44504 H(18) H(11) 3.047 ? . 44504 H(18) H(13) 2.890 ? . 55403 H(19) I(1) 3.443 ? . . H(19) H(1) 2.582 ? . . H(19) H(7) 3.298 ? . 44504 H(19) H(11) 3.298 ? . 44504 H(19) H(13) 3.598 ? . 55403 H(20) O(1) 3.572 ? . 54402 H(20) C(3) 3.535 ? . 65501 H(20) C(4) 2.997 ? . 65501 H(20) C(5) 3.049 ? . 65501 H(20) H(5) 3.081 ? . 65501 H(20) H(6) 2.366 ? . 65501 H(20) H(8) 2.508 ? . 65501 H(20) H(9) 3.237 ? . 65501 H(21) I(1) 3.386 ? . 65501 H(21) H(1) 3.337 ? . . H(21) H(2) 3.198 ? . 65501 H(21) H(3) 3.422 ? . 65501 H(21) H(5) 3.211 ? . 65501 H(21) H(6) 3.260 ? . 65501 H(21) H(12) 3.345 ? . 55403 H(21) H(13) 3.350 ? . 55403 H(22) O(1) 2.966 ? . 54402 H(22) C(1) 3.202 ? . 54402 H(22) H(1) 2.643 ? . . H(22) H(3) 3.487 ? . 65501 H(22) H(3) 2.581 ? . 54402 H(22) H(6) 3.115 ? . 65501 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF