data_General _audit_creation_date '2006-09-27' _audit_creation_method 'by CrystalStructure 3.7.0' #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name ' Takayuki Ishida' _publ_contact_author_address ; Department of Applied Physics and Chemistry, The University of Electro-Communications, Chofu, Tokyo 182-8585, Japan ; _publ_contact_author_email ' ishi@pc.uec.ac.jp ' _publ_contact_author_fax ' +81-424-43-5501 ' _publ_contact_author_phone ' +81-424-43-5490 ' _publ_requested_journal ' Chem. Mater.' _publ_author_name ; Atsushi Okazawa Takashi Nogami Takayuki Ishida ; _publ_section_references ; Rigaku/MSC and Rigaku Corporation. (2003). CrystalStructure. Single Crystal Structure Analysis Software. Version 3.5.1. 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. ; #============================================================================== data__[Cu(2pyNO)2(ClO4)2] #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C18 H26 Cl2 Cu N4 O10 ' _chemical_formula_moiety 'C18 H26 Cl2 Cu N4 O10 ' _chemical_formula_weight 592.88 #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 '+X,+Y,+Z' 2 '1/2-X,1/2+Y,1/2-Z' 3 '-X,-Y,-Z' 4 '1/2+X,1/2-Y,1/2+Z' #------------------------------------------------------------------------------ _cell_length_a 6.176(3) _cell_length_b 20.503(10) _cell_length_c 9.516(4) _cell_angle_alpha 90.0000 _cell_angle_beta 104.33(4) _cell_angle_gamma 90.0000 _cell_volume 1167.4(10) _cell_formula_units_Z 2 _cell_measurement_reflns_used 17509 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 30.1 _cell_measurement_temperature 90. #------------------------------------------------------------------------------ _exptl_crystal_description 'platelet' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.686 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 610.00 _exptl_absorpt_coefficient_mu 1.227 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Higashi, T. (1999). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.629 _exptl_absorpt_correction_T_max 0.885 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 14834 _diffrn_reflns_av_R_equivalents 0.063 _diffrn_reflns_theta_max 30.03 _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.980 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using all reflections. The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3349 _reflns_number_gt 2419 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0592 _refine_ls_wR_factor_ref 0.1085 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 3349 _refine_ls_number_parameters 174 _refine_ls_goodness_of_fit_ref 1.475 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0010Fo^2^ + 3.0000\s(Fo^2^)]' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 2.64 _refine_diff_density_min -1.05 _refine_ls_extinction_method 'Larson (1970) Crystallographic Computing eq. 22' _refine_ls_extinction_coef 1166(81) 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) ; '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) ; 'Cl' 'Cl' 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Cu' 'Cu' 0.320 1.265 ; 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 Cu(1) Cu 0.0000 0.0000 0.0000 0.0170(2) Uani 1.00 2 d S . . Cl(1) Cl 0.0672(2) 0.11102(6) -0.28028(13) 0.0187(3) Uani 1.00 1 d . . . O(1) O -0.1820(5) 0.0649(2) 0.0654(4) 0.0238(9) Uani 1.00 1 d . . . O(2) O 0.1279(7) 0.0914(2) -0.1297(4) 0.0320(11) Uani 1.00 1 d . . . O(3) O 0.2655(6) 0.1351(2) -0.3161(4) 0.0351(12) Uani 1.00 1 d . . . O(4) O -0.0968(7) 0.1611(2) -0.3009(5) 0.0477(14) Uani 1.00 1 d . . . O(5) O -0.0190(6) 0.0556(2) -0.3696(4) 0.0280(10) Uani 1.00 1 d . . . N(2) N 0.2237(6) 0.0331(2) 0.1642(4) 0.0171(10) Uani 1.00 1 d . . . N(1) N -0.0610(6) 0.1072(2) 0.1514(4) 0.0168(10) Uani 1.00 1 d . . . C(1) C 0.1522(8) 0.0846(2) 0.2278(5) 0.0175(12) Uani 1.00 1 d . . . C(2) C 0.2746(8) 0.1108(2) 0.3573(5) 0.0217(13) Uani 1.00 1 d . . . C(3) C 0.4816(8) 0.0838(2) 0.4194(5) 0.0224(13) Uani 1.00 1 d . . . C(4) C 0.5592(8) 0.0324(2) 0.3523(5) 0.0215(13) Uani 1.00 1 d . . . C(5) C 0.4248(8) 0.0072(2) 0.2258(5) 0.0201(13) Uani 1.00 1 d . . . C(6) C -0.1395(8) 0.1774(2) 0.1432(6) 0.0207(13) Uani 1.00 1 d . . . C(9) C 0.0500(10) 0.2210(2) 0.1203(7) 0.0307(16) Uani 1.00 1 d . . . C(8) C -0.2141(11) 0.1951(3) 0.2785(7) 0.0379(19) Uani 1.00 1 d . . . C(7) C -0.3369(10) 0.1830(3) 0.0113(8) 0.0449(19) Uani 1.00 1 d . . . H(1) H 0.2187 0.1464 0.4018 0.026 Uiso 1.00 1 c R . . H(2) H 0.5698 0.1005 0.5084 0.026 Uiso 1.00 1 c R . . H(3) H 0.7032 0.0145 0.3924 0.025 Uiso 1.00 1 c R . . H(4) H 0.4756 -0.0293 0.1814 0.024 Uiso 1.00 1 c R . . H(11) H 0.1780 0.2154 0.1987 0.039 Uiso 1.00 1 c R . . H(12) H 0.0857 0.2093 0.0321 0.039 Uiso 1.00 1 c R . . H(13) H 0.0038 0.2653 0.1157 0.039 Uiso 1.00 1 c R . . H(8) H -0.0912 0.1915 0.3610 0.050 Uiso 1.00 1 c R . . H(9) H -0.2680 0.2387 0.2705 0.050 Uiso 1.00 1 c R . . H(10) H -0.3298 0.1664 0.2888 0.050 Uiso 1.00 1 c R . . H(7) H -0.3914 0.2265 0.0033 0.049 Uiso 1.00 1 c R . . H(6) H -0.2908 0.1718 -0.0737 0.049 Uiso 1.00 1 c R . . H(5) H -0.4520 0.1542 0.0222 0.049 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 Cu(1) 0.0171(4) 0.0160(4) 0.0170(4) 0.0006(3) 0.0026(3) -0.0029(3) Cl(1) 0.0203(6) 0.0184(6) 0.0175(5) 0.0014(4) 0.0050(4) 0.0005(4) O(1) 0.0171(17) 0.023(2) 0.029(2) 0.0005(15) 0.0007(16) -0.0096(17) O(2) 0.044(2) 0.033(2) 0.0172(19) -0.015(2) 0.0039(18) 0.0033(17) O(3) 0.037(2) 0.042(2) 0.031(2) -0.016(2) 0.0174(19) -0.007(2) O(4) 0.037(2) 0.035(2) 0.062(3) 0.019(2) -0.005(2) -0.006(2) O(5) 0.028(2) 0.027(2) 0.027(2) -0.0044(17) 0.0023(17) -0.0080(18) N(2) 0.0163(19) 0.017(2) 0.018(2) -0.0020(16) 0.0054(17) -0.0008(17) N(1) 0.0187(19) 0.016(2) 0.016(2) -0.0013(17) 0.0052(17) -0.0015(17) C(1) 0.018(2) 0.018(2) 0.017(2) -0.0022(19) 0.007(2) 0.001(2) C(2) 0.025(2) 0.022(2) 0.020(2) -0.001(2) 0.007(2) -0.003(2) C(3) 0.022(2) 0.025(3) 0.019(2) -0.003(2) 0.003(2) 0.001(2) C(4) 0.018(2) 0.026(3) 0.019(2) -0.001(2) 0.001(2) 0.006(2) C(5) 0.019(2) 0.020(2) 0.021(2) 0.002(2) 0.005(2) 0.003(2) C(6) 0.021(2) 0.014(2) 0.027(2) -0.000(2) 0.007(2) -0.003(2) C(9) 0.039(3) 0.020(3) 0.039(3) -0.001(2) 0.019(2) -0.000(2) C(8) 0.050(3) 0.021(3) 0.054(4) -0.001(2) 0.035(3) -0.005(3) C(7) 0.037(3) 0.023(3) 0.062(4) 0.010(2) -0.012(3) -0.001(3) #============================================================================== _computing_data_collection 'PROCESS-AUTO' _computing_cell_refinement 'PROCESS-AUTO' _computing_data_reduction 'CrystalStructure' _computing_structure_solution 'SIR92' _computing_structure_refinement 'CRYSTALS' _computing_publication_material 'CrystalStructure 3.7.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ; 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 Cu(1) O(1) 1.942(4) ? . . Cu(1) O(1) 1.942(4) ? . 555_3 Cu(1) O(2) 2.478(4) ? . . Cu(1) O(2) 2.478(4) ? . 555_3 Cu(1) N(2) 1.935(3) ? . . Cu(1) N(2) 1.935(3) ? . 555_3 Cl(1) O(2) 1.446(4) ? . . Cl(1) O(3) 1.438(4) ? . . Cl(1) O(4) 1.421(5) ? . . Cl(1) O(5) 1.439(4) ? . . O(1) N(1) 1.294(5) ? . . N(2) C(1) 1.343(7) ? . . N(2) C(5) 1.345(6) ? . . N(1) C(1) 1.415(6) ? . . N(1) C(6) 1.515(7) ? . . C(1) C(2) 1.385(6) ? . . C(2) C(3) 1.385(7) ? . . C(3) C(4) 1.378(8) ? . . C(4) C(5) 1.382(6) ? . . C(6) C(9) 1.530(8) ? . . C(6) C(8) 1.516(10) ? . . C(6) C(7) 1.522(8) ? . . C(2) H(1) 0.950 ? . . C(3) H(2) 0.950 ? . . C(4) H(3) 0.950 ? . . C(5) H(4) 0.950 ? . . C(9) H(11) 0.950 ? . . C(9) H(12) 0.950 ? . . C(9) H(13) 0.950 ? . . C(8) H(8) 0.950 ? . . C(8) H(9) 0.950 ? . . C(8) H(10) 0.950 ? . . C(7) H(7) 0.950 ? . . C(7) H(6) 0.950 ? . . C(7) H(5) 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 O(1) Cu(1) O(1) 180.0(2) ? . . 555_3 O(1) Cu(1) O(2) 85.56(16) ? . . . O(1) Cu(1) O(2) 94.44(16) ? . . 555_3 O(1) Cu(1) N(2) 81.63(16) ? . . . O(1) Cu(1) N(2) 98.37(16) ? . . 555_3 O(1) Cu(1) O(2) 94.44(16) ? 555_3 . . O(1) Cu(1) O(2) 85.56(16) ? 555_3 . 555_3 O(1) Cu(1) N(2) 98.37(16) ? 555_3 . . O(1) Cu(1) N(2) 81.63(16) ? 555_3 . 555_3 O(2) Cu(1) O(2) 180.00(19) ? . . 555_3 O(2) Cu(1) N(2) 83.40(16) ? . . . O(2) Cu(1) N(2) 96.60(16) ? . . 555_3 O(2) Cu(1) N(2) 96.60(16) ? 555_3 . . O(2) Cu(1) N(2) 83.40(16) ? 555_3 . 555_3 N(2) Cu(1) N(2) 180.0(2) ? . . 555_3 O(2) Cl(1) O(3) 107.7(2) ? . . . O(2) Cl(1) O(4) 109.8(3) ? . . . O(2) Cl(1) O(5) 109.4(2) ? . . . O(3) Cl(1) O(4) 109.8(2) ? . . . O(3) Cl(1) O(5) 110.1(2) ? . . . O(4) Cl(1) O(5) 110.0(2) ? . . . Cu(1) O(1) N(1) 111.8(2) ? . . . Cu(1) O(2) Cl(1) 131.9(2) ? . . . Cu(1) N(2) C(1) 113.0(3) ? . . . Cu(1) N(2) C(5) 127.7(3) ? . . . C(1) N(2) C(5) 119.0(4) ? . . . O(1) N(1) C(1) 115.1(4) ? . . . O(1) N(1) C(6) 118.4(3) ? . . . C(1) N(1) C(6) 125.7(4) ? . . . N(2) C(1) N(1) 113.2(4) ? . . . N(2) C(1) C(2) 122.5(4) ? . . . N(1) C(1) C(2) 124.3(5) ? . . . C(1) C(2) C(3) 117.9(5) ? . . . C(2) C(3) C(4) 119.9(4) ? . . . C(3) C(4) C(5) 119.1(4) ? . . . N(2) C(5) C(4) 121.5(5) ? . . . N(1) C(6) C(9) 108.5(4) ? . . . N(1) C(6) C(8) 110.2(4) ? . . . N(1) C(6) C(7) 107.2(4) ? . . . C(9) C(6) C(8) 112.6(4) ? . . . C(9) C(6) C(7) 108.9(5) ? . . . C(8) C(6) C(7) 109.4(5) ? . . . C(1) C(2) H(1) 121.1 ? . . . C(3) C(2) H(1) 121.0 ? . . . C(2) C(3) H(2) 120.1 ? . . . C(4) C(3) H(2) 120.1 ? . . . C(3) C(4) H(3) 120.4 ? . . . C(5) C(4) H(3) 120.5 ? . . . N(2) C(5) H(4) 119.3 ? . . . C(4) C(5) H(4) 119.2 ? . . . C(6) C(9) H(11) 109.6 ? . . . C(6) C(9) H(12) 109.3 ? . . . C(6) C(9) H(13) 109.5 ? . . . H(11) C(9) H(12) 109.5 ? . . . H(11) C(9) H(13) 109.5 ? . . . H(12) C(9) H(13) 109.5 ? . . . C(6) C(8) H(8) 109.5 ? . . . C(6) C(8) H(9) 109.4 ? . . . C(6) C(8) H(10) 109.5 ? . . . H(8) C(8) H(9) 109.5 ? . . . H(8) C(8) H(10) 109.5 ? . . . H(9) C(8) H(10) 109.5 ? . . . C(6) C(7) H(7) 109.5 ? . . . C(6) C(7) H(6) 109.6 ? . . . C(6) C(7) H(5) 109.3 ? . . . H(7) C(7) H(6) 109.5 ? . . . H(7) C(7) H(5) 109.5 ? . . . H(6) C(7) H(5) 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 O(1) Cu(1) O(2) Cl(1) -101.6(3) ? . . . . O(2) Cu(1) O(1) N(1) -66.6(3) ? . . . . O(1) Cu(1) O(2) Cl(1) -78.4(3) ? . . 555_3 555_3 O(2) Cu(1) O(1) N(1) 113.4(3) ? 555_3 . . . O(1) Cu(1) N(2) C(1) -5.5(3) ? . . . . O(1) Cu(1) N(2) C(5) 167.9(5) ? . . . . N(2) Cu(1) O(1) N(1) 17.4(3) ? . . . . O(1) Cu(1) N(2) C(1) -174.5(3) ? . . 555_3 555_3 O(1) Cu(1) N(2) C(5) 12.1(5) ? . . 555_3 555_3 N(2) Cu(1) O(1) N(1) -162.6(3) ? 555_3 . . . O(1) Cu(1) O(2) Cl(1) 78.4(3) ? 555_3 . . . O(2) Cu(1) O(1) N(1) -113.4(3) ? . . 555_3 555_3 O(1) Cu(1) O(2) Cl(1) 101.6(3) ? 555_3 . 555_3 555_3 O(2) Cu(1) O(1) N(1) 66.6(3) ? 555_3 . 555_3 555_3 O(1) Cu(1) N(2) C(1) 174.5(3) ? 555_3 . . . O(1) Cu(1) N(2) C(5) -12.1(5) ? 555_3 . . . N(2) Cu(1) O(1) N(1) 162.6(3) ? . . 555_3 555_3 O(1) Cu(1) N(2) C(1) 5.5(3) ? 555_3 . 555_3 555_3 O(1) Cu(1) N(2) C(5) -167.9(5) ? 555_3 . 555_3 555_3 N(2) Cu(1) O(1) N(1) -17.4(3) ? 555_3 . 555_3 555_3 O(2) Cu(1) N(2) C(1) 81.0(3) ? . . . . O(2) Cu(1) N(2) C(5) -105.6(4) ? . . . . N(2) Cu(1) O(2) Cl(1) 176.3(3) ? . . . . O(2) Cu(1) N(2) C(1) 99.0(3) ? . . 555_3 555_3 O(2) Cu(1) N(2) C(5) -74.4(5) ? . . 555_3 555_3 N(2) Cu(1) O(2) Cl(1) -3.7(3) ? 555_3 . . . O(2) Cu(1) N(2) C(1) -99.0(3) ? 555_3 . . . O(2) Cu(1) N(2) C(5) 74.4(4) ? 555_3 . . . N(2) Cu(1) O(2) Cl(1) 3.7(3) ? . . 555_3 555_3 O(2) Cu(1) N(2) C(1) -81.0(3) ? 555_3 . 555_3 555_3 O(2) Cu(1) N(2) C(5) 105.6(5) ? 555_3 . 555_3 555_3 N(2) Cu(1) O(2) Cl(1) -176.3(3) ? 555_3 . 555_3 555_3 O(3) Cl(1) O(2) Cu(1) -143.6(3) ? . . . . O(4) Cl(1) O(2) Cu(1) 96.9(3) ? . . . . O(5) Cl(1) O(2) Cu(1) -23.9(4) ? . . . . Cu(1) O(1) N(1) C(1) -25.9(5) ? . . . . Cu(1) O(1) N(1) C(6) 144.1(3) ? . . . . Cu(1) N(2) C(1) N(1) -6.3(5) ? . . . . Cu(1) N(2) C(1) C(2) 171.9(4) ? . . . . Cu(1) N(2) C(5) C(4) -173.2(4) ? . . . . C(1) N(2) C(5) C(4) -0.1(6) ? . . . . C(5) N(2) C(1) N(1) 179.7(4) ? . . . . C(5) N(2) C(1) C(2) -2.2(8) ? . . . . O(1) N(1) C(1) N(2) 21.7(6) ? . . . . O(1) N(1) C(1) C(2) -156.5(5) ? . . . . O(1) N(1) C(6) C(9) -126.2(5) ? . . . . O(1) N(1) C(6) C(8) 110.2(5) ? . . . . O(1) N(1) C(6) C(7) -8.8(7) ? . . . . C(1) N(1) C(6) C(9) 42.6(7) ? . . . . C(1) N(1) C(6) C(8) -81.0(6) ? . . . . C(1) N(1) C(6) C(7) 160.0(5) ? . . . . C(6) N(1) C(1) N(2) -147.5(5) ? . . . . C(6) N(1) C(1) C(2) 34.4(8) ? . . . . N(2) C(1) C(2) C(3) 2.2(8) ? . . . . N(1) C(1) C(2) C(3) -179.8(5) ? . . . . C(1) C(2) C(3) C(4) 0.0(8) ? . . . . C(2) C(3) C(4) C(5) -2.2(9) ? . . . . C(3) C(4) C(5) N(2) 2.3(8) ? . . . . Cu(1) N(2) C(5) H(4) 6.7 ? . . . . C(1) N(2) C(5) H(4) 179.7 ? . . . . N(2) C(1) C(2) H(1) -178.0 ? . . . . N(1) C(1) C(2) H(1) -0.0 ? . . . . C(1) C(2) C(3) H(2) -179.8 ? . . . . H(1) C(2) C(3) C(4) -179.7 ? . . . . H(1) C(2) C(3) H(2) 0.4 ? . . . . C(2) C(3) C(4) H(3) 177.7 ? . . . . H(2) C(3) C(4) C(5) 177.7 ? . . . . H(2) C(3) C(4) H(3) -2.4 ? . . . . C(3) C(4) C(5) H(4) -177.6 ? . . . . H(3) C(4) C(5) N(2) -177.6 ? . . . . H(3) C(4) C(5) H(4) 2.6 ? . . . . N(1) C(6) C(9) H(11) -59.4 ? . . . . N(1) C(6) C(9) H(12) 60.5 ? . . . . N(1) C(6) C(9) H(13) -179.5 ? . . . . N(1) C(6) C(8) H(8) 62.1 ? . . . . N(1) C(6) C(8) H(9) -177.9 ? . . . . N(1) C(6) C(8) H(10) -57.9 ? . . . . N(1) C(6) C(7) H(7) 179.5 ? . . . . N(1) C(6) C(7) H(6) -60.4 ? . . . . N(1) C(6) C(7) H(5) 59.6 ? . . . . C(9) C(6) C(8) H(8) -59.1 ? . . . . C(9) C(6) C(8) H(9) 60.9 ? . . . . C(9) C(6) C(8) H(10) -179.1 ? . . . . C(8) C(6) C(9) H(11) 62.8 ? . . . . C(8) C(6) C(9) H(12) -177.2 ? . . . . C(8) C(6) C(9) H(13) -57.3 ? . . . . C(9) C(6) C(7) H(7) -63.4 ? . . . . C(9) C(6) C(7) H(6) 56.7 ? . . . . C(9) C(6) C(7) H(5) 176.7 ? . . . . C(7) C(6) C(9) H(11) -175.7 ? . . . . C(7) C(6) C(9) H(12) -55.7 ? . . . . C(7) C(6) C(9) H(13) 64.2 ? . . . . C(8) C(6) C(7) H(7) 60.0 ? . . . . C(8) C(6) C(7) H(6) -179.9 ? . . . . C(8) C(6) C(7) H(5) -59.9 ? . . . . C(7) C(6) C(8) H(8) 179.8 ? . . . . C(7) C(6) C(8) H(9) -60.2 ? . . . . C(7) C(6) C(8) H(10) 59.7 ? . . . . 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 O(1) C(4) 3.552(7) ? . 455_1 O(1) C(5) 3.385(7) ? . 455_1 O(3) C(2) 3.162(7) ? . 554_1 O(3) C(3) 3.299(7) ? . 554_1 O(3) C(5) 3.479(7) ? . 655_3 O(3) C(9) 3.561(8) ? . 554_4 O(3) C(8) 3.589(8) ? . 554_4 O(3) C(7) 3.594(7) ? . 655_1 O(4) C(3) 3.598(6) ? . 454_1 O(4) C(9) 3.218(7) ? . 454_4 O(5) O(5) 3.421(6) ? . 554_3 O(5) C(3) 3.288(5) ? . 454_1 O(5) C(4) 3.256(5) ? . 454_1 O(5) C(4) 3.334(6) ? . 655_3 C(2) O(3) 3.162(7) ? . 556_1 C(3) O(3) 3.299(7) ? . 556_1 C(3) O(4) 3.598(6) ? . 656_1 C(3) O(5) 3.288(5) ? . 656_1 C(3) C(4) 3.274(8) ? . 656_3 C(3) C(8) 3.434(9) ? . 655_1 C(4) O(1) 3.552(7) ? . 655_1 C(4) O(5) 3.256(5) ? . 656_1 C(4) O(5) 3.334(6) ? . 655_3 C(4) C(3) 3.274(8) ? . 656_3 C(4) C(4) 3.349(8) ? . 656_3 C(5) O(1) 3.385(7) ? . 655_1 C(5) O(3) 3.479(7) ? . 655_3 C(9) O(3) 3.561(8) ? . 455_4 C(9) O(4) 3.218(7) ? . 555_4 C(8) O(3) 3.589(8) ? . 455_4 C(8) C(3) 3.434(9) ? . 455_1 C(7) O(3) 3.594(7) ? . 455_1 Cl(1) H(1) 3.457 ? . 554_1 Cl(1) H(2) 3.236 ? . 454_1 Cl(1) H(3) 3.244 ? . 655_3 Cl(1) H(4) 3.217 ? . 655_3 Cl(1) H(9) 3.243 ? . 554_4 O(1) H(3) 3.513 ? . 455_1 O(1) H(4) 3.252 ? . 455_1 O(2) H(4) 2.908 ? . 655_3 O(2) H(5) 2.937 ? . 655_1 O(3) H(1) 2.638 ? . 554_1 O(3) H(2) 2.895 ? . 554_1 O(3) H(3) 3.170 ? . 655_3 O(3) H(4) 2.810 ? . 655_3 O(3) H(13) 2.688 ? . 554_4 O(3) H(8) 3.504 ? . 554_1 O(3) H(9) 2.738 ? . 554_4 O(3) H(7) 3.334 ? . 554_4 O(3) H(6) 3.204 ? . 655_1 O(3) H(5) 3.284 ? . 655_1 O(4) H(2) 2.688 ? . 454_1 O(4) H(11) 2.889 ? . 454_4 O(4) H(12) 3.448 ? . 454_4 O(4) H(13) 2.833 ? . 454_4 O(4) H(8) 3.286 ? . 554_1 O(4) H(9) 2.850 ? . 554_4 O(4) H(7) 3.400 ? . 554_4 O(5) H(1) 3.453 ? . 554_1 O(5) H(2) 2.681 ? . 454_1 O(5) H(3) 2.619 ? . 454_1 O(5) H(3) 2.476 ? . 655_3 O(5) H(4) 3.433 ? . 655_3 N(1) H(3) 3.555 ? . 455_1 C(1) H(10) 3.531 ? . 655_1 C(2) H(3) 3.484 ? . 656_3 C(2) H(13) 3.574 ? . 555_4 C(2) H(10) 2.912 ? . 655_1 C(3) H(3) 3.096 ? . 656_3 C(3) H(13) 3.599 ? . 555_4 C(3) H(8) 3.588 ? . 655_1 C(3) H(10) 2.548 ? . 655_1 C(4) H(2) 3.215 ? . 656_3 C(4) H(3) 3.377 ? . 656_3 C(4) H(10) 2.931 ? . 655_1 C(5) H(2) 3.352 ? . 656_3 C(5) H(10) 3.586 ? . 655_1 C(9) H(6) 3.585 ? . 555_4 C(8) H(2) 3.431 ? . 455_1 C(8) H(12) 3.560 ? . 455_4 C(8) H(7) 3.003 ? . 555_4 C(7) H(8) 3.166 ? . 454_4 C(7) H(9) 3.449 ? . 454_4 H(1) Cl(1) 3.457 ? . 556_1 H(1) O(3) 2.638 ? . 556_1 H(1) O(5) 3.453 ? . 556_1 H(1) H(13) 2.958 ? . 555_4 H(1) H(10) 3.253 ? . 655_1 H(1) H(7) 2.918 ? . 555_4 H(2) Cl(1) 3.236 ? . 656_1 H(2) O(3) 2.895 ? . 556_1 H(2) O(4) 2.688 ? . 656_1 H(2) O(5) 2.681 ? . 656_1 H(2) C(4) 3.215 ? . 656_3 H(2) C(5) 3.352 ? . 656_3 H(2) C(8) 3.431 ? . 655_1 H(2) H(3) 3.176 ? . 656_3 H(2) H(4) 3.367 ? . 656_3 H(2) H(13) 2.997 ? . 555_4 H(2) H(8) 3.359 ? . 655_1 H(2) H(10) 2.686 ? . 655_1 H(3) Cl(1) 3.244 ? . 655_3 H(3) O(1) 3.513 ? . 655_1 H(3) O(3) 3.170 ? . 655_3 H(3) O(5) 2.619 ? . 656_1 H(3) O(5) 2.476 ? . 655_3 H(3) N(1) 3.555 ? . 655_1 H(3) C(2) 3.484 ? . 656_3 H(3) C(3) 3.096 ? . 656_3 H(3) C(4) 3.377 ? . 656_3 H(3) H(2) 3.176 ? . 656_3 H(3) H(10) 3.257 ? . 655_1 H(4) Cl(1) 3.217 ? . 655_3 H(4) O(1) 3.252 ? . 655_1 H(4) O(2) 2.908 ? . 655_3 H(4) O(3) 2.810 ? . 655_3 H(4) O(5) 3.433 ? . 655_3 H(4) H(2) 3.367 ? . 656_3 H(11) O(4) 2.889 ? . 555_4 H(11) H(9) 3.353 ? . 655_1 H(11) H(10) 3.114 ? . 655_1 H(11) H(7) 3.258 ? . 555_4 H(11) H(6) 3.140 ? . 555_4 H(11) H(5) 3.394 ? . 655_1 H(12) O(4) 3.448 ? . 555_4 H(12) C(8) 3.560 ? . 554_4 H(12) H(8) 3.519 ? . 554_4 H(12) H(9) 3.044 ? . 554_4 H(12) H(10) 3.568 ? . 554_4 H(12) H(7) 3.327 ? . 655_1 H(12) H(5) 3.094 ? . 655_1 H(13) O(3) 2.688 ? . 455_4 H(13) O(4) 2.833 ? . 555_4 H(13) C(2) 3.574 ? . 454_4 H(13) C(3) 3.599 ? . 454_4 H(13) H(1) 2.958 ? . 454_4 H(13) H(2) 2.997 ? . 454_4 H(13) H(7) 3.588 ? . 555_4 H(13) H(6) 3.186 ? . 555_4 H(8) O(3) 3.504 ? . 556_1 H(8) O(4) 3.286 ? . 556_1 H(8) C(3) 3.588 ? . 455_1 H(8) C(7) 3.166 ? . 555_4 H(8) H(2) 3.359 ? . 455_1 H(8) H(12) 3.519 ? . 455_4 H(8) H(7) 2.314 ? . 555_4 H(8) H(6) 3.334 ? . 555_4 H(8) H(5) 3.529 ? . 555_4 H(9) Cl(1) 3.243 ? . 455_4 H(9) O(3) 2.738 ? . 455_4 H(9) O(4) 2.850 ? . 455_4 H(9) C(7) 3.449 ? . 555_4 H(9) H(11) 3.353 ? . 455_1 H(9) H(12) 3.044 ? . 455_4 H(9) H(7) 2.877 ? . 555_4 H(9) H(6) 3.476 ? . 555_4 H(9) H(5) 3.472 ? . 555_4 H(10) C(1) 3.531 ? . 455_1 H(10) C(2) 2.912 ? . 455_1 H(10) C(3) 2.548 ? . 455_1 H(10) C(4) 2.931 ? . 455_1 H(10) C(5) 3.586 ? . 455_1 H(10) H(1) 3.253 ? . 455_1 H(10) H(2) 2.686 ? . 455_1 H(10) H(3) 3.257 ? . 455_1 H(10) H(11) 3.114 ? . 455_1 H(10) H(12) 3.568 ? . 455_4 H(7) O(3) 3.334 ? . 455_4 H(7) O(4) 3.400 ? . 455_4 H(7) C(8) 3.003 ? . 454_4 H(7) H(1) 2.918 ? . 454_4 H(7) H(11) 3.258 ? . 454_4 H(7) H(12) 3.327 ? . 455_1 H(7) H(13) 3.588 ? . 454_4 H(7) H(8) 2.314 ? . 454_4 H(7) H(9) 2.877 ? . 454_4 H(6) O(3) 3.204 ? . 455_1 H(6) C(9) 3.585 ? . 454_4 H(6) H(11) 3.140 ? . 454_4 H(6) H(13) 3.186 ? . 454_4 H(6) H(8) 3.334 ? . 454_4 H(6) H(9) 3.476 ? . 454_4 H(5) O(2) 2.937 ? . 455_1 H(5) O(3) 3.284 ? . 455_1 H(5) H(11) 3.394 ? . 455_1 H(5) H(12) 3.094 ? . 455_1 H(5) H(8) 3.529 ? . 454_4 H(5) H(9) 3.472 ? . 454_4 #============================================================================== # End of CIF #==============================================================================