# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1235 #------------------------------------------------------------------------------ data_global _publ_requested_journal 'Chemical Communications' _publ_contact_letter ; ; _publ_contact_author ; Prof. Dr. Yoshiro Yamashita Research Center for Molecular Materials Institute for Molecular Science Myodaiji, Okazaki, Aichi 444-8585, Japan ; _publ_contact_author_phone '+81-564-55-7486' _publ_contact_author_fax '+81-564-53-5728' _publ_contact_author_email yoshiro@ims.ac.jp loop_ _publ_author_name 'Zaman, Md. Badruz' #<--'Last name, first name' 'Tomura, Masaaki' 'Yamashita, Yoshiro' _journal_name_full 'Chemical Communications' _journal_volume '?' _journal_page_first '?' _journal_page_last '?' _journal_year '1999' _ccdc_journal_depnumber '?' #------------------------------------------------------------------------------ data_1 _chemical_name_systematic ; complex of 4,4'-bipyridine and 2,5-dichloro-3,6-dihydroxy-1,4-benzoquinone ; _chemical_name_common ? _chemical_formula_moiety 'C10 H10 N2, C6 Cl2 O4' _chemical_formula_sum 'C16 H10 Cl2 N2 O4' _chemical_formula_weight 365.16 _chemical_melting_point 228 _cell_length_a 8.2377(7) _cell_length_b 5.9650(6) _cell_length_c 15.0893(10) _cell_angle_alpha 90.00 _cell_angle_beta 94.986(8) _cell_angle_gamma 90.00 _cell_volume 738.65(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 20.96 _cell_measurement_theta_max 43.32 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.642 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 372 _exptl_absorpt_coefficient_mu 4.193 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method BISECT _diffrn_standards_number 3 _diffrn_standards_interval_count 120 _diffrn_standards_decay_% -0.18 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 3 1 6 -3 0 1 0 13 _diffrn_reflns_number 1566 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_sigmaI/netI 0.0280 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_max 74.23 _diffrn_reflns_theta_min 5.89 _diffrn_reflns_reduction_process 'Lp corrections applied' #------------------------------------------------------------------------------ _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _reflns_number_total 1509 _reflns_number_observed 1265 _reflns_observed_criterion 'I>2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0536P)^2^+0.3405P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1508 _refine_ls_number_parameters 129 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0506 _refine_ls_R_factor_obs 0.0366 _refine_ls_wR_factor_all 0.1112 _refine_ls_wR_factor_obs 0.0932 _refine_ls_goodness_of_fit_all 1.057 _refine_ls_goodness_of_fit_obs 1.067 _refine_ls_restrained_S_all 1.157 _refine_ls_restrained_S_obs 1.067 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.234 _refine_diff_density_min -0.259 _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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. ; #------------------------------------------------------------------------------ _ccdc_disorder 'none' _ccdc_comments '?' #------------------------------------------------------------------------------ _computing_data_collection 'Enraf-Nonius CAD4 Express' _computing_cell_refinement 'Enraf-Nonius CAD4 Express' _computing_data_reduction 'teXsan' _computing_structure_solution 'SHELXS-86' _computing_structure_refinement 'SHELXL-93' _publ_section_references ; SHELXS-86: G. M. Sheldrick, Acta Crystallogr., Sect. A, 46, 467 (1990). SHELXL-93: G. M. Sheldrick, SHELXL-93, Program for refinement of crystal structures, University of G?tingen, Germany, 1993. Molecular Structure Corporation, Rigaku Corporation. (1998). teXsan. Single Crystal Structure Analysis Software. Version 1.9. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #------------------------------------------------------------------------------ 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cl(1) Cl 0.30180(7) 0.09465(9) 0.90794(3) 0.0397(2) Uani 1 d . . O(1) O 0.3459(2) 0.2092(3) 1.10290(9) 0.0386(4) Uani 1 d . . O(2) O 0.5129(2) 0.5509(3) 1.17706(10) 0.0484(5) Uani 1 d . . N(1) N 0.4323(2) 0.1689(3) 0.27822(12) 0.0396(4) Uani 1 d . . H(1) H 0.4158(40) 0.2135(57) 0.2153(23) 0.073(10) Uiso 1 d . . C(1) C 0.5136(4) -0.0192(4) 0.2977(2) 0.0472(6) Uani 1 d . . H(1A) H 0.5508(36) -0.1061(48) 0.2500(21) 0.059(9) Uiso 1 d . . C(2) C 0.5406(3) -0.0890(4) 0.38424(15) 0.0438(6) Uani 1 d . . H(2) H 0.5979(38) -0.2286(60) 0.3964(21) 0.069(9) Uiso 1 d . . C(3) C 0.4842(2) 0.0357(3) 0.45275(12) 0.0296(4) Uani 1 d . . C(4) C 0.3985(3) 0.2307(4) 0.42938(14) 0.0382(5) Uani 1 d . . H(4) H 0.3586(34) 0.3280(50) 0.4714(20) 0.053(8) Uiso 1 d . . C(5) C 0.3756(3) 0.2947(4) 0.3419(2) 0.0428(5) Uani 1 d . . H(5) H 0.3193(38) 0.4387(53) 0.3248(20) 0.061(9) Uiso 1 d . . C(6) C 0.4091(3) 0.3167(3) 0.95957(13) 0.0311(4) Uani 1 d . . C(7) C 0.4141(2) 0.3369(3) 1.05135(13) 0.0300(4) Uani 1 d . . C(8) C 0.5117(3) 0.5349(3) 1.09539(13) 0.0321(4) Uani 1 d . . #------------------------------------------------------------------------------ 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 Cl(1) 0.0472(3) 0.0352(3) 0.0367(3) -0.0033(2) 0.0044(2) -0.0059(2) O(1) 0.0472(8) 0.0382(8) 0.0312(7) 0.0077(6) 0.0066(6) -0.0065(7) O(2) 0.0768(12) 0.0446(9) 0.0243(7) -0.0003(7) 0.0084(7) -0.0116(8) N(1) 0.0504(11) 0.0437(10) 0.0243(8) 0.0072(8) 0.0014(7) -0.0062(9) C(1) 0.076(2) 0.0395(12) 0.0270(10) -0.0032(10) 0.0105(11) 0.0023(13) C(2) 0.072(2) 0.0315(11) 0.0282(10) -0.0008(9) 0.0055(10) 0.0098(11) C(3) 0.0367(10) 0.0268(9) 0.0251(10) -0.0001(8) 0.0018(7) -0.0047(8) C(4) 0.0484(12) 0.0376(11) 0.0288(10) 0.0023(9) 0.0045(9) 0.0094(10) C(5) 0.0487(13) 0.0456(13) 0.0338(11) 0.0081(10) 0.0015(9) 0.0076(11) C(6) 0.0362(10) 0.0285(9) 0.0282(10) -0.0001(8) 0.0012(8) -0.0002(8) C(7) 0.0338(10) 0.0287(9) 0.0275(9) 0.0048(8) 0.0034(7) 0.0049(8) C(8) 0.0399(11) 0.0310(10) 0.0254(9) 0.0031(8) 0.0034(8) 0.0039(8) #------------------------------------------------------------------------------ _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; #------------------------------------------------------------------------------ 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 Cl(1) C(6) 1.739(2) 1_555 1_555 yes O(1) C(7) 1.256(2) 1_555 1_555 yes O(2) C(8) 1.235(2) 1_555 1_555 yes N(1) C(1) 1.327(3) 1_555 1_555 yes N(1) C(5) 1.336(3) 1_555 1_555 yes N(1) H(1) 0.98(3) 1_555 1_555 yes C(1) C(2) 1.370(3) 1_555 1_555 yes C(1) H(1A) 0.96(3) 1_555 1_555 yes C(2) C(3) 1.386(3) 1_555 1_555 yes C(2) H(2) 0.97(3) 1_555 1_555 yes C(3) C(4) 1.390(3) 1_555 1_555 yes C(3) C(3) 1.489(4) 1_555 3_656 yes C(4) C(5) 1.371(3) 1_555 1_555 yes C(4) H(4) 0.94(3) 1_555 1_555 yes C(5) H(5) 1.00(3) 1_555 1_555 yes C(6) C(7) 1.387(3) 1_555 1_555 yes C(6) C(8) 1.411(3) 1_555 3_667 yes C(7) C(8) 1.546(3) 1_555 1_555 yes C(8) C(6) 1.411(3) 1_555 3_667 yes #------------------------------------------------------------------------------ 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 C(1) N(1) C(5) 121.1(2) 1_555 1_555 1_555 yes C(1) N(1) H(1) 117.9(20) 1_555 1_555 1_555 yes C(5) N(1) H(1) 121.0(20) 1_555 1_555 1_555 yes N(1) C(1) C(2) 120.3(2) 1_555 1_555 1_555 yes N(1) C(1) H(1A) 118.6(18) 1_555 1_555 1_555 yes C(2) C(1) H(1A) 121.0(18) 1_555 1_555 1_555 yes C(1) C(2) C(3) 120.7(2) 1_555 1_555 1_555 yes C(1) C(2) H(2) 118.6(19) 1_555 1_555 1_555 yes C(3) C(2) H(2) 120.7(19) 1_555 1_555 1_555 yes C(2) C(3) C(4) 117.1(2) 1_555 1_555 1_555 yes C(2) C(3) C(3) 121.2(2) 1_555 1_555 3_656 yes C(4) C(3) C(3) 121.6(2) 1_555 1_555 3_656 yes C(5) C(4) C(3) 120.1(2) 1_555 1_555 1_555 yes C(5) C(4) H(4) 116.8(18) 1_555 1_555 1_555 yes C(3) C(4) H(4) 123.0(18) 1_555 1_555 1_555 yes N(1) C(5) C(4) 120.6(2) 1_555 1_555 1_555 yes N(1) C(5) H(5) 118.7(18) 1_555 1_555 1_555 yes C(4) C(5) H(5) 120.7(18) 1_555 1_555 1_555 yes C(7) C(6) C(8) 123.9(2) 1_555 1_555 3_667 yes C(7) C(6) Cl(1) 118.9(2) 1_555 1_555 1_555 yes C(8) C(6) Cl(1) 117.2(2) 3_667 1_555 1_555 yes O(1) C(7) C(6) 126.1(2) 1_555 1_555 1_555 yes O(1) C(7) C(8) 116.2(2) 1_555 1_555 1_555 yes C(6) C(7) C(8) 117.7(2) 1_555 1_555 1_555 yes O(2) C(8) C(6) 125.0(2) 1_555 1_555 3_667 yes O(2) C(8) C(7) 116.5(2) 1_555 1_555 1_555 yes C(6) C(8) C(7) 118.4(2) 3_667 1_555 1_555 yes #------------------------------------------------------------------------------ #===END #------------------------------------------------------------------------------ data_2 _chemical_name_systematic ; complex of trans-1,2-bis(2-pyridyl)ethylene and 2,5-dichloro-3,6-dihydroxy-1,4-benzoquinone ; _chemical_name_common ? _chemical_formula_moiety 'C12 H12 N2, C6 Cl2 O4' _chemical_formula_sum 'C18 H12 Cl2 N2 O4 ' _chemical_formula_weight 391.21 _chemical_melting_point 215 _cell_length_a 9.855(1) _cell_length_b 11.245(1) _cell_length_c 3.9057(6) _cell_angle_alpha 91.34(1) _cell_angle_beta 99.69(1) _cell_angle_gamma 111.702(8) _cell_volume 394.68(10) _cell_formula_units_Z 1 _cell_measurement_temperature 293 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.5 _cell_measurement_theta_max 15.0 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.050 _exptl_crystal_density_diffrn 1.646 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 200.00 _exptl_absorpt_coefficient_mu 0.440 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 1.52 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -2 4 1 -4 4 0 -2 3 0 _diffrn_reflns_number 1906 _diffrn_reflns_av_R_equivalents 0.015 _diffrn_reflns_av_sigmaI/netI 0.053 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_reduction_process 'Lp corrections applied' #------------------------------------------------------------------------------ _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _reflns_number_total 1804 _reflns_number_gt 1258 _reflns_observed_expression 'I>3\s(I)' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme unit _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1258 _refine_ls_number_parameters 142 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0332 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0336 _refine_ls_wR_factor_gt 0.0336 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.242 _refine_ls_shift/su_max 0.1140 _refine_ls_shift/su_mean 0.0060 _refine_diff_density_max 0.21 _refine_diff_density_min -0.18 _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; #------------------------------------------------------------------------------ _ccdc_disorder 'none' _ccdc_comments '?' #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SHELXS-86 _computing_structure_refinement 'teXsan' _publ_section_references ; SHELXS-86: G. M. Sheldrick, Acta Crystallogr., Sect. A, 46, 467 (1990). Molecular Structure Corporation, Rigaku Corporation. (1998). teXsan. Single Crystal Structure Analysis Software. Version 1.9. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ 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_calc_flags _atom_site_refinement_flags _atom_site_disorder_group Cl(1) Cl 0.22789(7) 0.27042(6) 0.3776(2) 0.0370(2) Uani 1.00 d . . O(1) O -0.0600(2) 0.2130(2) -0.1045(5) 0.0355(5) Uani 1.00 d . . O(2) O 0.2515(2) 0.0115(2) 0.4220(5) 0.0420(5) Uani 1.00 d . . N(1) N 0.2538(2) 0.7558(2) 0.6184(5) 0.0284(5) Uani 1.00 d . . C(1) C 0.3945(3) 0.8295(2) 0.7628(7) 0.0342(6) Uani 1.00 d . . C(2) C 0.4827(3) 0.7798(3) 0.9733(7) 0.0368(7) Uani 1.00 d . . C(3) C 0.4216(3) 0.6508(3) 1.0304(7) 0.0379(7) Uani 1.00 d . . C(4) C 0.2767(3) 0.5760(2) 0.8822(7) 0.0323(6) Uani 1.00 d . . C(5) C 0.1906(2) 0.6306(2) 0.6731(6) 0.0268(6) Uani 1.00 d . . C(6) C 0.0349(3) 0.5626(2) 0.5072(7) 0.0312(6) Uani 1.00 d . . C(7) C -0.0260(3) 0.1176(2) -0.0456(6) 0.0268(6) Uani 1.00 d . . C(8) C 0.1024(2) 0.1214(2) 0.1727(6) 0.0275(6) Uani 1.00 d . . C(9) C 0.1382(3) 0.0130(2) 0.2319(6) 0.0273(6) Uani 1.00 d . . H(1) H 0.433(3) 0.924(3) 0.703(8) 0.054(9) Uiso 1.00 d . . H(2) H 0.583(3) 0.831(3) 1.078(7) 0.040(7) Uiso 1.00 d . . H(3) H 0.483(3) 0.614(3) 1.170(7) 0.041(8) Uiso 1.00 d . . H(4) H 0.235(3) 0.491(3) 0.922(7) 0.032(7) Uiso 1.00 d . . H(5) H -0.018(3) 0.615(3) 0.412(7) 0.041(7) Uiso 1.00 d . . H(6) H 0.197(4) 0.792(3) 0.453(9) 0.066(10) Uiso 1.00 d . . #------------------------------------------------------------------------------ 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 Cl(1) 0.0339(3) 0.0275(3) 0.0407(4) 0.0071(2) -0.0049(2) -0.0040(2) O(1) 0.0372(10) 0.0278(9) 0.040(1) 0.0149(7) -0.0037(8) 0.0013(7) O(2) 0.0333(10) 0.0376(10) 0.048(1) 0.0145(8) -0.0118(8) 0.0004(8) N(1) 0.027(1) 0.0257(10) 0.031(1) 0.0100(8) 0.0012(8) 0.0029(8) C(1) 0.029(1) 0.031(1) 0.036(1) 0.0056(10) 0.003(1) -0.001(1) C(2) 0.025(1) 0.040(1) 0.036(1) 0.007(1) -0.003(1) -0.006(1) C(3) 0.034(1) 0.045(1) 0.034(1) 0.018(1) -0.005(1) 0.000(1) C(4) 0.034(1) 0.027(1) 0.033(1) 0.011(1) 0.000(1) 0.0038(10) C(5) 0.026(1) 0.025(1) 0.028(1) 0.0088(9) 0.0044(9) 0.0006(9) C(6) 0.026(1) 0.028(1) 0.037(1) 0.0101(9) -0.0015(10) 0.004(1) C(7) 0.027(1) 0.025(1) 0.026(1) 0.0092(9) 0.0029(9) 0.0042(9) C(8) 0.026(1) 0.024(1) 0.028(1) 0.0055(9) 0.0013(9) 0.0003(9) C(9) 0.025(1) 0.029(1) 0.027(1) 0.0100(9) 0.0014(9) 0.0037(9) #------------------------------------------------------------------------------ _geom_special_details ; ? ; #------------------------------------------------------------------------------ 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 Cl(1) C(8) 1.746(2) 1_555 1_555 yes O(1) C(7) 1.252(3) 1_555 1_555 yes O(2) C(9) 1.238(3) 1_555 1_555 yes N(1) C(1) 1.339(3) 1_555 1_555 yes N(1) C(5) 1.351(3) 1_555 1_555 yes N(1) H(6) 0.98(3) 1_555 1_555 yes C(1) C(2) 1.372(4) 1_555 1_555 yes C(1) H(1) 1.03(3) 1_555 1_555 yes C(2) C(3) 1.389(4) 1_555 1_555 yes C(2) H(2) 0.95(3) 1_555 1_555 yes C(3) C(4) 1.376(3) 1_555 1_555 yes C(3) H(3) 0.96(3) 1_555 1_555 yes C(4) C(5) 1.393(3) 1_555 1_555 yes C(4) H(4) 0.92(3) 1_555 1_555 yes C(5) C(6) 1.461(3) 1_555 1_555 yes C(6) C(6) 1.313(5) 1_555 2_566 yes C(6) H(5) 0.96(3) 1_555 1_555 yes C(7) C(8) 1.387(3) 1_555 1_555 yes C(7) C(9) 1.545(3) 1_555 2_555 yes C(8) C(9) 1.403(3) 1_555 1_555 yes #------------------------------------------------------------------------------ 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 C(1) N(1) C(5) 122.5(2) 1_555 1_555 1_555 yes C(1) N(1) H(6) 118(1) 1_555 1_555 1_555 yes C(5) N(1) H(6) 118(1) 1_555 1_555 1_555 yes N(1) C(1) C(2) 120.9(2) 1_555 1_555 1_555 yes N(1) C(1) H(1) 116(1) 1_555 1_555 1_555 yes C(2) C(1) H(1) 122(1) 1_555 1_555 1_555 yes C(1) C(2) C(3) 117.9(2) 1_555 1_555 1_555 yes C(1) C(2) H(2) 121(1) 1_555 1_555 1_555 yes C(3) C(2) H(2) 120(1) 1_555 1_555 1_555 yes C(2) C(3) C(4) 120.8(2) 1_555 1_555 1_555 yes C(2) C(3) H(3) 118(1) 1_555 1_555 1_555 yes C(4) C(3) H(3) 120(1) 1_555 1_555 1_555 yes C(3) C(4) C(5) 119.4(2) 1_555 1_555 1_555 yes C(3) C(4) H(4) 121(1) 1_555 1_555 1_555 yes C(5) C(4) H(4) 119(1) 1_555 1_555 1_555 yes N(1) C(5) C(4) 118.5(2) 1_555 1_555 1_555 yes N(1) C(5) C(6) 116.8(2) 1_555 1_555 1_555 yes C(4) C(5) C(6) 124.8(2) 1_555 1_555 1_555 yes C(5) C(6) C(6) 123.7(3) 1_555 1_555 2_566 yes C(5) C(6) H(5) 116(1) 1_555 1_555 1_555 yes C(6) C(6) H(5) 119(1) 2_566 1_555 1_555 yes O(1) C(7) C(8) 125.0(2) 1_555 1_555 1_555 yes O(1) C(7) C(9) 116.2(2) 1_555 1_555 2_555 yes C(8) C(7) C(9) 118.8(2) 1_555 1_555 2_555 yes Cl(1) C(8) C(7) 117.9(2) 1_555 1_555 1_555 yes Cl(1) C(8) C(9) 118.4(2) 1_555 1_555 1_555 yes C(7) C(8) C(9) 123.7(2) 1_555 1_555 1_555 yes O(2) C(9) C(7) 116.4(2) 1_555 1_555 2_555 yes O(2) C(9) C(8) 126.1(2) 1_555 1_555 1_555 yes C(7) C(9) C(8) 117.5(2) 2_555 1_555 1_555 yes #------------------------------------------------------------------------------ #===END