手性晶系,有手性。 data_07102m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H8 Cl2 N6 Zn' _chemical_formula_weight 300.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 9.631(3) _cell_length_b 9.631(3) _cell_length_c 12.325(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1143.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 926 _cell_measurement_theta_min 2.69 _cell_measurement_theta_max 26.39 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.746 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 600 _exptl_absorpt_coefficient_mu 2.592 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.3693 _exptl_absorpt_correction_T_max 0.4910 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6869 _diffrn_reflns_av_R_equivalents 0.0467 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 27.08 _reflns_number_total 1259 _reflns_number_gt 1115 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0912P)^2^+2.9726P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 1259 _refine_ls_number_parameters 79 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0571 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1685 _refine_ls_wR_factor_gt 0.1620 _refine_ls_goodness_of_fit_ref 1.125 _refine_ls_restrained_S_all 1.125 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Zn1 Zn 1.30866(8) 1.30866(8) 0.0000 0.0408(4) Uani 1 2 d S . . Cl1 Cl 1.3155(9) 1.4524(10) -0.1473(7) 0.0302(12) Uani 0.50 1 d P . . N2 N 0.9192(6) 1.2520(6) 0.1336(5) 0.0388(12) Uani 1 1 d . . . N1 N 1.1128(6) 1.3146(6) 0.0582(5) 0.0406(12) Uani 1 1 d . . . C3 C 0.8119(7) 1.1693(8) 0.1888(6) 0.0472(16) Uani 1 1 d . . . H3A H 0.8214 1.0721 0.1695 0.057 Uiso 1 1 calc R . . H3B H 0.7203 1.2005 0.1670 0.057 Uiso 1 1 calc R . . C1 C 1.0429(8) 1.2092(8) 0.1054(7) 0.0485(18) Uani 1 1 d . . . H1 H 1.0773 1.1200 0.1161 0.058 Uiso 1 1 calc R . . N3 N 0.8989(7) 1.3870(6) 0.1057(5) 0.0443(14) Uani 1 1 d . . . C2 C 1.0210(7) 1.4190(7) 0.0608(6) 0.0404(14) Uani 1 1 d . . . H2 H 1.0407 1.5069 0.0335 0.048 Uiso 1 1 calc R . . Cl1' Cl 1.3402(9) 1.4759(10) -0.1257(8) 0.0344(16) Uani 0.50 1 d P . . 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 Zn1 0.0327(4) 0.0327(4) 0.0571(7) -0.0068(4) 0.0068(4) -0.0043(4) Cl1 0.022(3) 0.028(3) 0.041(3) 0.005(2) -0.001(2) -0.013(2) N2 0.029(3) 0.041(3) 0.047(3) 0.006(3) 0.009(2) -0.008(2) N1 0.033(3) 0.034(3) 0.055(3) 0.001(3) 0.008(2) -0.004(2) C3 0.032(3) 0.052(4) 0.057(4) 0.010(3) 0.009(3) -0.005(3) C1 0.041(4) 0.035(4) 0.070(5) 0.008(3) 0.012(3) 0.003(3) N3 0.041(3) 0.039(3) 0.053(3) 0.007(3) 0.002(3) 0.004(2) C2 0.041(4) 0.038(3) 0.042(3) 0.006(3) 0.003(3) 0.000(3) Cl1' 0.024(3) 0.025(3) 0.055(4) 0.006(2) -0.003(2) -0.0149(18) _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_2 _geom_bond_publ_flag Zn1 N1 2.019(5) 7 ? Zn1 N1 2.019(5) . ? Zn1 Cl1' 2.256(11) 7 ? Zn1 Cl1' 2.256(11) . ? Zn1 Cl1 2.284(10) 7 ? Zn1 Cl1 2.284(10) . ? N2 C1 1.308(8) . ? N2 N3 1.359(8) . ? N2 C3 1.471(9) . ? N1 C2 1.340(9) . ? N1 C1 1.350(9) . ? C3 C3 1.531(15) 8_775 ? N3 C2 1.335(9) . ? 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_3 _geom_angle_publ_flag N1 Zn1 N1 100.3(3) 7 . ? N1 Zn1 Cl1' 110.5(3) 7 7 ? N1 Zn1 Cl1' 114.8(3) . 7 ? N1 Zn1 Cl1' 114.8(3) 7 . ? N1 Zn1 Cl1' 110.5(3) . . ? Cl1' Zn1 Cl1' 106.2(3) 7 . ? N1 Zn1 Cl1 107.0(3) 7 7 ? N1 Zn1 Cl1 106.4(3) . 7 ? Cl1' Zn1 Cl1 10.7(2) 7 7 ? Cl1' Zn1 Cl1 116.36(19) . 7 ? N1 Zn1 Cl1 106.4(3) 7 . ? N1 Zn1 Cl1 107.0(3) . . ? Cl1' Zn1 Cl1 116.36(19) 7 . ? Cl1' Zn1 Cl1 10.7(2) . . ? Cl1 Zn1 Cl1 126.7(3) 7 . ? C1 N2 N3 111.4(6) . . ? C1 N2 C3 126.3(6) . . ? N3 N2 C3 122.3(6) . . ? C2 N1 C1 103.0(5) . . ? C2 N1 Zn1 130.3(5) . . ? C1 N1 Zn1 126.7(5) . . ? N2 C3 C3 108.0(8) . 8_775 ? N2 C1 N1 109.3(6) . . ? C2 N3 N2 101.5(6) . . ? N3 C2 N1 114.7(6) . . ? 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 N1 Zn1 N1 C2 -144.7(7) 7 . . . ? Cl1' Zn1 N1 C2 96.9(7) 7 . . . ? Cl1' Zn1 N1 C2 -23.2(7) . . . . ? Cl1 Zn1 N1 C2 104.0(6) 7 . . . ? Cl1 Zn1 N1 C2 -33.9(7) . . . . ? N1 Zn1 N1 C1 35.4(6) 7 . . . ? Cl1' Zn1 N1 C1 -83.0(7) 7 . . . ? Cl1' Zn1 N1 C1 156.9(6) . . . . ? Cl1 Zn1 N1 C1 -75.9(7) 7 . . . ? Cl1 Zn1 N1 C1 146.3(6) . . . . ? C1 N2 C3 C3 90.7(7) . . . 8_775 ? N3 N2 C3 C3 -89.2(6) . . . 8_775 ? N3 N2 C1 N1 0.8(9) . . . . ? C3 N2 C1 N1 -179.0(7) . . . . ? C2 N1 C1 N2 -0.4(9) . . . . ? Zn1 N1 C1 N2 179.5(5) . . . . ? C1 N2 N3 C2 -0.9(8) . . . . ? C3 N2 N3 C2 179.0(6) . . . . ? N2 N3 C2 N1 0.6(8) . . . . ? C1 N1 C2 N3 -0.2(9) . . . . ? Zn1 N1 C2 N3 180.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.08 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.136 _refine_diff_density_min -0.511 _refine_diff_density_rms 0.141